Both ricin and R. communis agglutinin (RCA120), belonging to the type II ribosome-inactivating proteins (RIPs-Ⅱ), are derived from the seeds of castor bean plant. They share very similar amino acid sequences, but ricin is much more toxic than RCA120. It is urgently necessary to distinguish ricin and RCA120 in response to public safety. Currently, mass spectrometric assays are well established for unambiguous identification of ricin by accurate analysis of differentiated amino acid residues after trypsin digestion. However, diagnostic peptides are relatively limited for unambiguous identification of trace ricin, especially in complex matrices. Here, we demonstrate a digestion strategy of multiple proteinases to produce novel peptide markers for unambiguous identification of ricin. LC-HRMS was used to verified the resulting peptides, among which only the peptides with uniqueness and good MS response were selected as peptide markers. Seven novel peptide markers were obtained from tandem digestion of trypsin and endoproteinase Glu-C in PBS buffer. From the chymotrypsin digestion under reduction and non-reduction conditions, eight and seven novel peptides were selected respectively. Using pepsin under pH 1~2 and proteinase K digestion, 6 and 5 peptides were selected as novel peptide markers. In conclusion, the obtained novel peptides from the established digestion methods can be recommended for the unambiguous identification of ricin during the investigation of illegal use of the toxin.

A new sulbatamol sulphate SBS membrane electrode was prepared that utilizing for its determination ; depend on the forming of the association complex ion of sulbatamol sulphate by the phosphotungstate counter anion deposed in poly vinyl chloride PVC polymer, by use a (Di-n- Octyl Phenyl Phthalate)(Dopp) as the plastizier substance, in membrane.The features properties as well as the behavior of it .The new electrode have been elaborated. The concentrations of medicine by utillizing This sensor show a fast, stable, near-Nernstian response in the range (1x10^-1-1x10^-6) mol/ L were determined with correlation coefficient of about (r = 0.9991) and with of a relative standard about 0.416 additionally deviation relative standard error of 1.710  %.^pot The nernast linearity slop was founded and it is equal to 28.9 mV/decade and the detection limit was 4.1 x 10^-6 mol/ L.The electrode selectivity coefficient K_i,j was calculated, in the existence of several interferences cations with confirmed medicine solutions. It was found the pH range response is in the range of (3 -7), with the response time of (30 – 116) sec. for various  concentrations at room temperture , the lifetime for  electrode was found to be more than 21 days. The electrode was successfully used for potentiometric limitation of sulbatamol sulphate in several pharmaceutical drugs by using direct potentiometry.

The Privilegium maius is one of the most famous and spectacular forgeries in medieval Europe. It is a set of charters made in 14th century upon commitment by duke Rudolf IV, a member of the Habsburg family, to elevate the rank and the prestige of his family. These five charters, now kept at the Österreichisches Staatsarchiv in Vienna, have been subjected to a thorough interdisciplinary study in order to shed light on its controversial story. The charters are composed by pergamenaceous documents bound to wax seals with coloured textile threads. The present contribution concerns the characterisation of the inks used for writing and of the dyes used to colour to the threads: are they compatible with the presumed age of the charters? Though showing only a part of the whole story of the charters, dyes analysis could contribute in assessing their complex history from manufacturing to nowadays. The dyes were characterised with non-invasive in situ measurements by means of FORS and with micro-invasive measurements by means of SERS and HPLC-MS analysis. The results showed that the threads of four of the charters (three dyed with madder, one with orchil) were apparently coloured at different dyeing stages, then re-dyed in the 19th-20th century.

The reliable online analysis of volatile compounds in exhaled breath remains a challenge as a plethora of molecules occur in different concentration ranges (i.e. ppt to %), and need to be detected against an extremely complex background matrix. While this complexity is commonly addressed by hyphenating a specific analytical technique with appropriate preconcentration and/or preseparation strategies prior to detection, we herein propose the combination of three analytical tools based on truly orthogonal measurement principles as an alternative solution: field-asymmetric ion mobility spectrometry (FAIMS), Fourier-transform infrared (FTIR) spectroscopy-based sensors utilizing substrate-integrated hollow waveguides (iHWG), and luminescence sensing (LS). These three tools have been integrated into a single compact analytical platform suitable for online exhaled breath analysis. The analytical performance of this prototype system was tested via artificial breath samples containing nitrogen (N2), oxygen (O2), carbon dioxide (CO2) and acetone as a model volatile organic compound (VOC) commonly present and detected in breath. Functionality of the combined system was demonstrated by detecting these analytes in their respectively breath-relevant concentration range and mutually independent of each other generating orthogonal yet correlated analytical signals. Finally, adaptation of the system towards the analysis of real breath samples during future studies is discussed.

BiVO4 powder was synthesized by a simple hydrothermal method. The nanobelts with well dispersed and uniform morphology were synthesized by controlling the temperature. The structure of BiVO4 powder was studied by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The diameter of the nanobelts was about 50 nm. The structure and composition of the nanobelts were studied by X-ray diffraction (XRD), photoluminescence (PL) and X-ray photoelectron spectroscopy (XPS). The absorption intensity of BiVO4 powder in UV-Vis region was compared by UV–vis diffuse reflectance spectroscopy. As a photocatalyst, BiVO4 nanobelts have good photocatalytic ability under visible light irradiation, which is very useful for the treatment of environmental wastewater. The synthesized nanobelts photocatalyst can be reused without destroying its structure. The reusability and chemical stability of photocatalysts are of great significance for practical application.

Stable-isotope dimethyl labeling is a highly reactive and cost-effective derivatization procedure that could be utilized in proteomics analysis. In this study, a liquid chromatography-tandem mass spectrometry in multiple reaction monitoring mode (LC-MS-MRM) platform for the quantification of kiwi allergens was first developed using this strategy. Three signature peptides for target allergens Act d 1, Act d 5, and Act d 11 were determined and were derivatized with normal and deuterated formaldehyde as external calibrants and internal standards, respectively. The results showed that sample preparation with the phenol method provided comprehensive protein populations. Recoveries at four different levels ranging from 72.5–109.3% were achieved for the H-labeled signature peptides of Act d 1 (SPA1-H) and Act d 5 (SPA5-H) with precision ranging from 1.86–9.92%. The limit of quantification (LOQ) was set at 8 pg mL–1 for SPA1-H and at 4 ng mL–1 for SPA5-H. The developed procedure was utilized to analyze seven kinds of hand-made kiwi foods containing 0.0175–0.0515 mg g–1 of Act d 1 and 0.0252–0.0556 mg g–1 of Act d 5. This study extended the applicability of stable-isotope dimethyl labeling to the economical and precise determination of food allergens and peptides.

Experimental optimization of analytical methods based on solid-phase microextraction (SPME) is a complex and labor-intensive process associated with uncertainties. Using the theoretical basics of SPME and finite element analysis software for the optimization proved to be an efficient alternative. In this study, an improved finite element analysis-based model for SPME of volatile organic compounds (VOCs) by porous coatings was developed mainly focussing on the mass transport in coatings. Benzene and the Carboxen/polydimethylsiloxane (Car/PDMS) coating were used as the model VOC and a porous SPME coating, respectively. It has been established that in the coating, volumetric fractions of Carboxen, PDMS, and air are 33, 42 and 24%, respectively. Knudsen diffusion in micropores can slow down a mass transport of analytes in the coating. When PDMS was considered as the solid part of the coating, lower root-mean-square deviation of the modeling results from experimental data was observed. It has been shown that the developed model can be used to model the extraction of VOCs from air and water samples encountered in a typical SPME development method procedure. It was possible to determine system equilibration times and use them to optimize sample volume and Henry’s law constant. The developed model is relatively simple, fast, and can be recommended for optimization of extraction parameters for other analytes and SPME coatings. The diffusivity of analytes in a coating is an important property needed for improved characterization of existing and new SPME polymers and analytical method optimization.

The authors determined mass concentrations of 12 elements (As, Cd, Cr, Cu, Mn, Ni, Pb, Se, Sr, Tl, V, Zn) in blood and urine taken from 100 rural children living in unremarkable condition in the West Ural region of the Russian Federation. We applied inductively coupled plasma mass spectrometry in conformity with Methodical Guidelines 4.1. 3230-14 (FR.1.31.2014.17064) designed by us and detailed in the paper. The article contains setting parameters for Agilent 7500cx quadrupole inductively coupled plasma mass spectrometer . The authors present grounds for an optimal scheme of samples preparation which helps to eliminate "matrix" effect and explain why it is advisable to use reaction/collision functioning mode as it enables interference overlaps suppression.To prepare whole blood samples for analysis, we used acid dissolution in concentrated nitric acid followed by centrifugation. The arithmetic mean (AM) of element content in blood amounted to 0.34 µg/l (As); 0.39 µg/l (Cd); 6.41 µg/l (Cr); 866.11 µg/l (Сu); 13.73 µg/l (Mn); 5.86 µg/l (Ni); 23.65 µg/l (Pb); 87.43 µg/l (Se); 33.54 µg/l (Sr); 0.04 µg/l (Tl); 0.16 µg/l (V); 4713.48 µg/l (Zn). The validity of the results was confirmed by means of  SERONORM ^TM Whole Blood L2 standard samples (Norway). Urine samples were directly analyzed after 1/10 (V/V) dilution with 1% nitric acid solution. The arithmetic mean of element  content of urine corresponded to 18.99 µg/l (As); 0.12 µg/l (Cd); 1.91 µg/l (Cr); 13.28 µg/l (Сu);  0.96 µg/l (Mn); 1.84 µg/l (Ni); 0.83 µg/l  (Pb); 22.55 µg/l (Se); 239.09 µg/l (Sr); 0.16 µg/l  (Tl); 0.68 µg/l (V); 270.56 µg/l (Zn).  The validity of the results was confirmed by analyzing the SERONORM ^TM standard urine samples (Norway). Regional differences from levels found in other countries included  higher concentrations of Cr, Mn and Ni in blood and  lower levels of Se and Zn levels in West Ural children. Urine concentrations of West Ural children showed  higher levels of As and Sr.

Fructus Amomi (FA) is usually regarded as the dried ripe fruits of Amomum villosum Lour. (FAL) or Amomum villosum Lour. var. xanthioides T. L.Wu et Senjenis (FALX) However, FAL, which always has a much higher price because of its better quality, is confused with FALX in the market. As volatile oil is the main constituent of FA, a strategy of chromatography-mass spectrometry (GC-MS) and chemometric approches was applied to compare the chemical composition of FAL and FALX. The results showed that the oil yield of FAL was significantly higher than that of FALX. Total ion chromatograph (TIC) showed that cis-nerolidol existed only in FALX. Bornyl acetate and camphor, could be considered as the most important ones in FAL and FALX respectively. Moreover, hierarchical cluster analysis (HCA) and principal component analysis (PCA) successfully distinguished the chemical constitutes of the volatile oils in FAL and FALX. Additionally, bornyl acetate, α-cadinol, linalool, β-myrcene, camphor, d-limonene, terpinolene and endo-borneol were selected as the potential markers for discriminating FAL and FALX by partial least squares discrimination analysis (PLS-DA). In conclusion, this present study first developed a scientific approach to separate FAL and FALX based on volatile oils by GC-MS combined with chemometric techniques.

Environmental isolates, genetically manipulated organisms, plants, animals and their products and economical methods are being expertly explored to biosynthesize poly-3-hydroxybutyrate plastics of comparable properties to petroplastics. This study assessed a hypothesized feasibility of utilizing a proliferative pleustophytic greenery, water hyacinth (Eichhornia crassipes (Mart.) Solms-Laubach) in Lake Victoria, Uganda as a potential carbon source for poly-3-hydroxybutyrate biosynthesis. The  poly-3-hydroxybutyrate biosynthesizing bacteria (Bacillus megaterium) was isolated from municipal sewage sludge and harnessed for batch fermentation of acid-catalysed water hyacinth biomass. Poly-3-hydroxybutyrate  formed in the cytoplasm of the bacterial cells was extracted by chloroform extraction method, and thereof confirmed and quantified by UV spectroscopy. Batch fermentation was carried out in 100ml of the culture media in a 250ml fermenter for different times (48, 96, 144 and 192 hours) to determine the best incubation time for maximum yield. An all-out net yield of 61.3% was realized after 96 hours of fermentation. Utilization of this ecological plague for poly-3-hydroxybutyrate biosynthesis is a promising strategy for regulating the weed population along the length of Nile River and the Victorian basin.

The development of a stationary phase material for high performance liquid chromatography based on a surface of silica hydride as opposed to silanols on ordinary silica is discussed including synthetic approaches, characterization and applications.  There are several synthetic approaches available to create a silica hydride surface.  Modification of the Si-H moiety on the silica surface can be accomplished through use of a hydrosilation reaction.  Both the intermediate silica hydride and the material modified with an organic moiety can be characterized by a number of spectroscopic as well as a variety of other methods.  Further insights into the retention mechanism are provide through chromatographic measurements.  The ultimate utility of any chromatographic stationary phase material is determined by its success for solving challenging analytical problems.  A broad range of applications are reviewed to illustrate the versatility and usefulness of silica hydride-based stationary phases. 

Deep fat frying is not novel, but a classical antiquity culinary technique preferred chiefly for its swiftness, amenity, conferment of a crisp texture, attractive sensorial and organoleptic qualities and thus delectableness of the fries. Regrettably, repeated use of oils for deep frying impacts the storage life and nutritional suitability of fries. This concerted study investigated the effects of continuous deep fat frying on the physicochemical properties of ten brands of edible cooking oils: Fortune Butto, Roki, Tamu, Best Fry, Golden Fry, Mukwano, Sunny, Sunvita, Sunlite and Sunseed used in deep frying of potato chips in Kampala, Uganda. Three oil samples from local Irish chip fryers were also collected. The color value (CV) and the acidification of the oils as free fatty acid (FFA), peroxide value (POV), paraanisidine value (AnV) and iodine adsorption value (IV) before and between ten successive deep-fryings using potato chips were determined. The possible reuse of the oils was estimated from the frying round when a quality criterion surpassed national or CODEX specifications for the respective edible cooking oils. For fresh oils, the statistical parameter ranges were: CV (0.4R 3.4Y-7.7R 70Y), % FFA (0.0430-0.1508), POV (0.5951-6.6134 meqO₂/Kg), AnV (0.90-4.30) and IV (57.62-128.35gI₂/100g). By the tenth fry, the values were respectively 3.0R 23Y-20.4R 70Y, 0.2286-0.4817, 11.1138-15.7525 meqO₂/Kg, 10.31-22.16 and 53.66-126.03 gI₂/100g. Reuse of the oils for continuous frying of potatoes on the same day can be done only up to 7 times on average for hard oils and 6 times for soft oils.

The present work describes the optimization and validation of a highly selective and sensitive analytical method using solid phase extraction and liquid chromatography tandem mass spectrometry (SPE LC-MS/MS) for the determination of some frequently prescribed pharmaceuticals in urban wastewater received and treated by Sharjah sewage treatment plant (STP). The extraction efficiency of different SPE cartridges was tested and the simultaneous extraction of pharmaceuticals was successfully accomplished using hydrophilic-lipophilic-balanced reversed phase Waters^® Oasis HLB cartridge (200 mg/ 6 mL) at pH 3. The analytes were separated on an Aquity BEH C₁₈ column (1.7 µm, 2.1 mm x 150 mm) using gradient elution and the mass spectrometric analysis were performed in multiple reactions monitoring (MRM) selecting two precursor ions to produce ion transition for each pharmaceutical using positive electrospray ionization (+ESI) mode. The correlation coefficient values in the linear calibration plot for each target compound exceeded 0.99 and the recovery percentages of the investigated pharmaceuticals were more than 84%. Limit of detection (LOD) varied between 0.1-1.5 ng/L and limit of quantification (LOQ) was 0.3-5 ng/L for all analytes. The precision of the method was calculated as the relative standard deviation (RSD%) of replicate measurements and was found to be in the ranges of 2.2% to 7.7% and 2.2% to 8.6% for inter and intra-day analysis, respectively. All of the obtained validation parameters satisfied the requirements and guidelines of analytical method validation.

Deep fat frying is not novel, but a classical antiquity culinary technique preferred chiefly for its swiftness, amenity, conferment of a crisp texture, attractive sensorial and organoleptic qualities and thus delectableness of the fries. Regrettably, repeated use of oils for frying impacts the storage life and nutritional suitability of fries. This concerted study investigated the effects of continuous deep frying on physicochemical properties of ten brands of edible cooking oils: Fortune Butto, Roki, Tamu, Best Fry, Golden Fry, Mukwano, Sunny, Sunvita, Sunlite and Sunseed used in Kampala, Uganda. The color value (CV) and the acidification of the oils as free fatty acid (FFA), peroxide value (POV), paraanisidine value (AnV) and iodine adsorption value (IV) before and between ten successive deep-frying using potato chips were determined. The possible reuse of the oils was estimated from the frying round when a quality criterion surpassed the specifications for edible oils. For fresh oils, the mean statistical parameter readings were: CV (0.4R 3.4Y-7.7R 70Y), % FFA (0.0430-0.1508), POV (0.5951-6.6134 meqO₂/Kg), AnV (0.90-4.30) and IV (57.62-128.35gI₂/100g). By the tenth fry, the values were respectively 3.0R 23Y-20.4R 70Y, 0.2286-0.4817, 11.1138-15.7525 meqO₂/Kg, 10.31-22.16 and 53.66-126.03 gI₂/100g. Reuse of the oils for continuous frying of potatoes on the same day can be done only up to 7 times on average for hard oils and 6 times for soft oils.

Experimental optimization of analytical methods based on solid-phase microextraction (SPME) is a complex and labor-intensive process associated with uncertainties. Using theoretical basics of SPME and finite element analysis software for the optimization proved to be an efficient alternative. In this study, an improved finite element analysis-based model for SPME of volatile organic compounds (VOCs) by porous coatings was developed mainly focussing on the mass transport in coatings. Benzene and the Carboxen/polydimethylsiloxane (Car/PDMS) coating were used as the model VOC and a porous SPME coating, respectively. It has been established that in the coating, volumetric fractions of Carboxen, PDMS, and air are 33, 42 and 25%, respectively. It has been proven that Knudsen diffusion in micropores can slow down a mass transport of analytes in the coating. For Car/PDMS coating, mass transport of benzene is mostly characterized by a molecular diffusion, which can be explained by a large fraction of macro- and mesopores. It has been shown that the developed model can be used to model the extraction of VOCs from air and water samples encountered in a typical SPME development method procedure. It was possible to determine system equilibration times and use them to optimize sample volume and Henry’s law constant. The developed model is relatively simple, fast, and can be recommended for optimization of extraction parameters for other analytes and SPME coatings. The diffusivity of analytes in a coating is an important property needed for improved characterization of existing and new SPME polymers and analytical method optimization.

This contribution is aimed to measure for the first time the amount of biogenic amines (BAs) in one of the most ancient and traditional sheep cheese produced in Sardinia, Italy: the Protected Designation of Origin (PDO) Fiore Sardo. For doing this, an original RP-HPLC-DAD-UV method has been developed, completely validated in terms of LoD, LoQ, linearity, precision and trueness, and tested on 36 real Fiore Sardo PDO cheese samples produced by four different cheesemakers and marketed by four stores. The average total concentration of the eight BAs (i.e. tyramine, tryptamine, histidine, putrescine, cadaverine, 2-phenylethylamine, spermine and spermidine) measured in Fiore Sardo cheese was 700 mg/kg, with a range between 170 mg/kg and 1100 mg/kg. A great variability in the total amount of BAs has been evidenced among the Fiore Sardo marketed in the four stores as well as for the cheeses purchased in different times in the same store. Tyramine (350 mg/kg), putrescine (150 mg/kg), histamine (80 mg/kg) and cadaverine (30 mg/kg) are the most abundant BAs found in this matrix. Among many factors concurring, the dominant microflora of Fiore Sardo PDO is likely the principal cause of the qualitative and quantitative distribution of BAs in this matrix. Finally, the total amount of BAs found in Fiore Sardo PDO is not able to cause any situation of health alert for consumers.

The water-rich liquid layer immobilized on the surface of the polar stationary phases is critical to the retention of polar compounds in hydrophilic interaction chromatography (HILIC). Although the presence of the adsorbed water layer has been investigated and confirmed by multiple techniques, there is a lack of quantitative measure that can be easily determined and linked to chromatographic parameters. This study proposes a simple measure termed volume ratio (the ratio of the adsorbed water layer volume and the mobile phase volume) that provides a relative, but quantitative information on the adsorbed water layer and may be linked to the phase ratio. The volume ratio can be easily determined using toluene elution volume. The volume ratio values are measured in 25 polar stationary phases in various mobile phase conditions. In addition to the acetonitrile content in the mobile phase, ammonium acetate concentration in the mobile phase and column temperature also have significant influences on the volume ratio and the adsorbed water layer.

Fabric phase sorptive extraction, an innovative integration of solid phase extraction and solid phase microextraction principles, has been combined with gas chromatography-mass spectrometry for the rapid extraction and determination of nineteen organochlorine pesticides in various fruit juices and water samples. FPSE consolidates the advanced features of sol-gel derived extraction sorbents with the rich surface chemistry of cellulose fabric substrate, which could directly extract target analytes from complex sample matrices and substantially simplifies the sample preparation operation. Important FPSE parameters including sorbent chemistry, extraction time, stirring speed, type and volume of back-extraction solvent and back-extraction time have been optimized. Calibration curves were obtained in the concentration range 0.1-500 ng/mL. Under the optimum conditions, the limits of detection were obtained in the range 0.007-0.032 ng/mL with satisfactory precision (RSD<6%). The relative recoveries obtained by spiking organochlorine pesticides in water and selected juice samples were in the range of 91.56–99.83%. The sorbent sol-gel poly(ethylene glycol)-poly(propylene glycol)-poly(ethylene glycol) was applied for the extraction and preconcentration of organochlorine pesticides in aqueous and fruit juice samples prior to analysis with gas chromatography-mass spectrometry. The results demonstrated that the present method is simple, rapid, and precise for the determination of organochlorine pesticides in aqueous samples.

Potato is a starchy, tuberous crop from the perennial Solanum tuberosum having high nutritional values. This paper is the first analytical approach to quantify Pt and Rh in vegetal food. In this study a total of 38 different potatoes samples produced in Europe and one in Australia were investigated. Determinations of Pt and Rh in potatoes samples were carried out by Differential Pulse Voltammetry (DPV/a) for platinum and by Adsorptive Stripping Voltammetry (AdSV) for Rh using standard addition procedure. Because no certified reference potatoes containing platinum and rhodium are available, we used addition standard method. The quantification limits for Pt and Rh are 0.007 and 0.0008 μg Kg−1 respectively. Considering all the potatoes samples, concentrations of Pt and Rh vary in the ranges from 0.007 to 109 μg Kg−1 (sample n° 6 potatoes grown in Sicily) and from 0.0008 to 0.030 μg Kg−1 (sample n°23 of potatoes grown in Emilia Romagna) respectively. For both metals, in many cases the concentrations fall near the quantification limit. In all the samples, platinum is always more abundant than rhodium and their ratio meanly is 14500, which is much greater than that of the earth's crust (about 100).

A combination of physical-chemical analysis has been used to monitor the aging of red wines from D.O. Toro (Spain). The changes in the chemical composition of wines that occur along aging time can be permitted to discriminate wine samples collected after one, four, seven and ten months of aging. Different computational models were used to develop a good authenticity tool to certificate wines. In this research different models have developed: Artificial Neural Network models (ANNs), Support Vector Machine (SVM) and Random Forest (RF) models. The results obtained for the ANN model developed with sigmoidal function in the output neuron and the RF model permit to determine the aging time, with an average absolute percentage deviation below 1% and it can conclude that these two models have demonstrated its capacity as a valid tool to predict the wine age.

Techniques of stripping voltammetry (SV) determination of silver and gold in pyrites and carbonaceous matter were developed. The problem of quantitative transfer of the sample into the solution was solved. For this purpose, the ore matrix of carbonaceous shales was decomposed by mineral acids in autoclaves at high pressures. The element to be determined from the sample matrix was separated by extraction. Ag(I) ions from the solutions were extracted in the form of dithizonate complex in CCl₄. Au(III) ions were extracted by diethyl ether. The extracts were decomposed thermally. The dry residue was dissolved in the background electrolyte, and the element was determined by the SV method. The graphite electrode (GE) impregnated with polyethylene was used as a working electrode in SV–determination of silver. SV–determination of gold was carried out using GE modified by bismuth. The limits of detection (LOD) of Ag(I) and Au(III) contents were equal to 0.016 mg L^-1 and 0.0086 mg L^-1, respectively. The results of SV-determination of gold and silver in standard samples, pyrites and carbonaceous shales were presented. The silver content in the pyrite was 13.6 g t^-1, in carbon shale—0.34 g t^-1. The concentration of gold in the pyrite ore zone "Kirovsko–Kryklinskaya" was 1.15 g t^-1; in carbonaceous shales—2.66 g t^-1. The obtained data were consistent with the data of atomic emission spectroscopy (AES) and inductively coupled plasma mass spectrometry (ICP—MS). The error of determination of elements by stripping voltammetry was calculated when determining the silver content of 10...6 g t^-1 in pyrite and carbonaceous material, which was less than 12%, and when determining the gold content of 1...3 g t^{- 1} in pyrite and carbonaceous matter, which was less than 23%.

Potato is a starchy, tuberous crop from the perennial Solanum tuberosum having high nutritional values. This paper is the first analytical approach to quantify Pt and Rh in vegetal food. In this study a total of 38 different potatoes samples produced in Europe and one in Australia were investigated. Determinations of Pt and Rh in potatoes samples were carried out by Differential Pulse Voltammetry (DPV/a) for platinum and by Adsorptive Stripping Voltammetry (AdSV) for Rh using standard addition procedure. Because no certified reference potatoes containing platinum and rhodium are available, we used addition standard method. The quantification limits for Pt and Rh are 0.007 and 0.0008 μg Kg−1 respectively. Considering all the potatoes samples, concentrations of Pt and Rh vary in the ranges from 0.007 to 109 μg Kg−1 (sample n° 6 potatoes grown in Sicily) and from 0.0008 to 0.030 μg Kg−1 (sample n°23 of potatoes grown in Emilia Romagna) respectively. For both metals, in many cases the concentrations fall near the quantification limit. In all the samples, platinum is always more abundant than rhodium and their ratio meanly is 14500, which is much greater than that of the earth's crust (about 100).

Seeds represent the major source of food protein, impacting on both human nutrition and animal feeding. Therefore, seed quality needs to be appropriately addressed in the context of viability and food safety. Indeed, long-term and inappropriate storage of seeds might result in enhancement of protein glycation, which might affect their quality and longevity. Glycation of seed proteins can be probed by exhaustive acid hydrolysis and quantification of the glycation adduct N^ɛ-(carboxymethyl)lysine (CML) by liquid chromatography-mass spectrometry (LC-MS). This approach, however, does not allow analysis of thermally and chemically labile glycation adducts, like glyoxal-, methylglyoxal- and 3-deoxyglucosone-derived hydroimidazolones. Although enzymatic hydrolysis might be a good solution in this context, it requires aqueous conditions, which cannot ensure reconstitution of seed protein isolates. Because of this, the complete profiles of seed AGEs are not characterized so far. Therefore, here we propose the approach, giving access to quantitative solubilization of seed proteins in presence of sodium dodecyl sulfate (SDS) and their quantitative enzymatic hydrolysis prior to removal of SDS by reversed phase solid phase extraction (RP-SPE). Using MG-H1 as a case example, we demonstrate the applicability of this method for reliable and sensitive LC-MS-based quantification of chemically labile AGEs and its compatibility with bioassays.

We describe a selective and sensitive fluorescence platform for the detection of trinitrophenol (TNP) based on competitive host–guest recognition between pyridine-functionalized pillar[6]arene (PCP6) and probe (acridine orange, AO) that used PCP6-functionalized reduced graphene (PCP6-rGO) as the receptor. TNP is an electron-deficient and negative molecule which is captured by PCP6 via electrostatic interactions and π-π interactions. Therefore, a selective and sensitive fluorescence sensor for TNP detection is developed. It has a low detection limit of 0.0035 μM (S/N=3) and a wider linear response of 0.01−5.0 and 5.0−125.0 for TNP. The sensing platform is also used to test TNP in two water and soil samples with satisfying results. This suggests that this approach has potential applications for the determination of TNP.

This study aimed to investigate the airborne release of N-nitrosodimethylamine (NDMA) as a result of the dry heat cooking of some meats using charcoal grilling and pan broiling methods. Three types of meat, beef sirloin, pork belly, and duck, were chosen and cooked in a temporary building using the above methods. Air samples were collected in Thermosorb-N cartridges, which were qualitatively and quantitatively analyzed for NDMA using ultra-high performance liquid chromatography–mass spectrometry and high-performance liquid chromatography–fluorescence detection, respectively. Overall, the charcoal grilling method showed higher average NDMA concentrations than the pan broiling method for all types of meat. The highest average concentration was observed for charcoal-grilled beef sirloin (410 ng/m3) followed by pork belly, suggesting that meat protein content and cooking duration are important determinants of NDMA formation. Cancer risk assessment showed that the charcoal grilling of such meats can pose an additional cancer risk for restaurant customers.

Simultaneous measurement of different substances from a single sample is an emerging issue to achieve efficient and high-throughput detection in several fields of application. Although immunoanalytical techniques have well-established and prevailing advantages over alternative screening analytical platforms, one of the incoming challenges for immunoassay is exactly multiplexing. The Lateral Flow Immunoassay (LFIA) is a leading immunoanalytical technique for onsite analysis thanks to its simplicity, rapidity and cost-effectiveness. Moreover, LFIA architecture is adaptable to multiplexing and therefore candidates as a possible answer to the pressing demand of multiplexing point-of-need analysis. The review present an overview of diverse approaches for multiplex LFIA, with a special focus on strategies based on new types of magnetic, fluorescent and colored labels

Food analysis demands fast methods for routine control and high throughput of samples. Chromatographic separation enables simultaneous determination of numerous compounds in complex matrices, several approaches increasing separation efficiency and speed of analysis were involved. In this work, modern types of column with monolithic rod or superficially porous particles were employed and compared for determination of eight synthetic food dyes, their chromatographic performance was evaluated. During method optimization, cyano stationary phase Chromolith Performance CN 100 × 4.6 mm and Ascentis Express ES-CN 100 × 4.6 mm, 5 µm were selected for the separation of polar colorants. The separation was performed by gradient elution of acetonitrile/methanol and 2% water solution of ammonium acetate at flow rate 2.0 ml min-1. Mobile phase composition and the gradients were optimized in order to enable efficient separation on both columns. The method using fused-core particle column provided higher separation efficiency, narrow peaks of analytes resulted in increased peak capacity and shortening of analysis time. After the validation, the method was applied for analysis of colored beers, soft drinks and candies.

A common task in the immunodetection of structurally close compounds is to analyze the selectivity of immune recognition: it is required to understand the regularities of immune recognition and to elucidate the basic structural elements which provide it. Triazines are compounds of particular interest for such a research due to their high variability and the necessity of their monitoring to provide safety of agricultural products and foodstuffs. We evaluated the binding of 20 triazines with polyclonal (pAb) and monoclonal (mAb) antibodies obtained using atrazine as the immunogenic hapten. A total of >3000 descriptors was used in QSAR analysis of binding activities (pIC50). Comparison of the two enzyme immunoassay systems showed that the system with pAb is much easier to describe using 2D QSAR methodology, while the system with mAb can be described using the 3D QSAR COMFA. Thus, for the 3D QSAR model of the polyclonal antibodies, the main statistical parameter q² (‘leave-many-out’) is equal 0.498, and for monoclonal antibodies q² is equal 0.566. Obviously, in the case of pAb, we deal with several targets, while in the case of mAb the target is one, and therefore it is easier to describe it using specific fields of molecular interactions distributed in space.

Drinking water contamination of lead from various environmental sources, leaching consumer products and intrinsic water-pipe infrastructure is still today a matter of great concern. Therefore, new highly sensitive and convenient Pb²⁺ measurement schemes are necessary, especially for in-situ measurements at a low-cost. Within this work dye/ionophore/Pb²⁺ co-extraction and effective water phase de-colorization was utilized for highly sensitive lead measurements and sub-ppb naked-eye detection. A low-cost ionophore Benzo-18-Crown-6-ether was used, and a simple test-tube mix and separate procedure was developed. Instrumental detection limits were in the low ppt region (LOD=3, LOQ=10), and naked-eye detection was 500 ppt. Note, however, that this sensing scheme still has improvement potential as concentrations of fluorophore and ionophore were not optimized. Artificial tap-water samples, leached by a standardized method, demonstrated drinking water application. Implications for this method are convenient in-situ lead ion measurements.

Almost 50 papers on surface plasmon resonance biosensors, published between 2016 and mid-2018, are reviewed. Papers concerning the determination of large particles such as vesicles, exosomes, cancer cells, living cells, stem cells and microRNA are excluded, as these are covered by a very recent review. The reviewed papers are categorized into five groups, depending on the degree of maturity of the reported solution: ranging from simple marker detection to clinical application of a previously developed biosensor. Instrumental solutions and details of biosensor construction are analyzed, including the chips, receptors and linkers used, as well as calibration strategies. Biosensors with a sandwich structure containing different nanoparticles are considered separately, as are SPR applications for investigating the interactions of biomolecules. An analysis is also made of the markers determined using the biosensors. Concluding, there is shown to be a growing number of SPR applications in the solution of real clinical problems.

NiFe alloy nanoparticles/graphene oxide hybrid (NiFe/GO) was prepared for electrochemical glucose sensing. The as-prepared NiFe/GO hybrid was characterized by transmission electron microscopy (TEM) and X-ray diffraction (XRD). The results indicated that NiFe alloy nanoparticles can be successfully deposited on GO. The electrochemical glucose sensing performance of the as-prepared NiFe/GO was studied by cyclic voltammetry and amperometric measurement. Results showed that NiFe/GO modified glassy carbon electrode had sensitivity of 173 μA mM⁻¹cm⁻² for glucose sensing with a linear range up to 5 mM, which was superior to commonly used Ni nanoparticles. Furthermore, high selectivity for glucose detection can be achieved by NiFe/GO. All the results demonstrated that NiFe/GO hybrid was promising for using in electrochemical glucose sensing.

A supramolecular host-guest interaction and sensing between cationic pillar[5]arenes (CP5) and L-carnitine were developed by the competitive host-guest recognition for the first time. The fluorescence sensing platform was constructed by CP5 functionalized Au nanoparticles ([email protected]) as receptor and probe (rhodamine 123, R123), which shown a high sensitivity and selectivity to L-carnitine detection. Due to the property of the negative charge and molecular size of L-carnitine, it can be highly captured by the CP5 via electrostatic interactions and hydrophobic interactions. The mechanism of host-guest between PP5 and L-carnitine was studied by ¹H NMR and molecular docking, which indicated more affinity binding force of PP5 with L-carnitine. Therefore, a selective and sensitive fluorescent method was developed. It has a linear response of 0.1–2.0 and 2.0–25.0 μM and a detection limit of 0.067 μM (S/N = 3) for L-carnitine. The fluorescent sensing platform was also used to detect L-carnitine in human serum and milk samples, which provided potential applications of detection drugs of abuse, and had path for guarding a serious food safety issues.   

Membrane Inlet Mass Spectrometry (MIMS) was used to analyze monochloramine solutions (NH₂Cl) and ammonia solutions in a compact FTICR. Chemical ionization enables identification and quantification of the products present in the permeate. The responses of protonated monochloramine and ammonium increase linearly with the solution concentration. The enrichments were respectively 1.2 and 5.5. Pervaporation is dependent on pH and only the basic form of ammonia NH₃ pervaporates through the membrane. Unexpectedly, the small ammonia molecule permeated very slowly. It could be due to interactions with water molecules inside the membrane that create clusters. Moreover, NH₂Cl solutions, in addition to the NH₃Cl⁺ signal, presented a strong NH₄⁺ signal at m/z 18.034 . Ammonia presence in the low-pressure zone before ionization is probable as NH₄⁺ was detected with all the precursors used, particularly CF₃⁺ and trimethylbenzene that presents a proton affinity higher than monochloramine. Ammonia may be formed inside the membrane due to the fact that NH₂Cl is unstable and may react with the water present in the membrane. Those results highlight the need for caution when dealing with chloramines in MIMS and more generally with unstable molecules.

The use of fluoride (F^-) for decreasing the prevalence and incidence of tooth decay was the greatest worldwide preventive public health measure of the 20th century. There have been controversial reports about the benefits of the use of F^-, because in small amounts it helps prevent dental caries, but in high concentrations it can be potentially toxic and harmful to dental and systemic health. Since the mid-20th century, F^- has been studied by toxicologists, looking at its deleterious effects in human populations. During the last decade, the interest on the undesirable effects has resurfaced because of the knowledge that it interacts with the cellular system, even in low doses, with a very small safety margin. Acute ingestion of toxic amounts of fluoride can cause corrosive gastric mucosa injury. Also respiratory effects such as bleeding, pulmonary edema, tracheostomy and shortness of breath, have been observed in individuals who inhale hydrogen fluoride. Some researchers had shown that F^- is an oxidizing agent and a well-known reversible enzymatic inhibitor that interferes with the enzyme activity of at least 80 proteins, can altered the intracellular redox equilibrium, lipid peroxidation, as well as, alteration in the gene expression and apoptosis induction. The primary purpose of this review is to examine findings of the action of inorganic F^-, and an overview of hard and soft tissue disturbances, known as fluorosis. The goal of this review is to enhance understanding of the mechanisms by which F^- affects cells with an emphasis on human tissue-specific events.

Vitamin B2, also known as riboflavin (RF) is an essential micronutrient for human health and must be obtained from dietary sources. Plants biosynthesize riboflavin and are important dietary sources of vitamin B2 for humans. Our present study reports sensitive detection of Vitamin B2 in widely consumed for tea infusions, namely black, green, sage and rosemary tea infusions, by a capillary electrophoresis method combined with laser induced fluorescence detection. Moreover, the correlation between Vitamin B2 contents of tea plants with their total phenolics (TPs) and antioxidant capacity are evaluated in this study. Whereas green teas have the highest TPs and antioxidant capacity, the highest RF contents are in sage infusions. The RF contents range between 0.34 and 10.36 µg/g for all tea samples studied. Comparing RF contents of tea samples found in this study to the RF contents of known RF sources, tea infusions are proposed as important dietary sources of Vitamin B2.

Platinum(II) complexes have been found to be effective against cancer cells. Cisplatin curbs cell replication by interacting with the deoxyribonucleic acid (DNA), eventually leading to cell death and reducing cell proliferation. In order to investigate the ability of platinum complexes to affect cancer cells, two examples from the class of polyflurophenylorganoamidoplatinum(II) complexes were synthesised and tested on isolated DNA. The two compounds trans-[N,N’-bis(1,2,3,5,6-pentafluorophenyl)ethane-1,2-diaminato(1-)](2,3,4,5,6-pentafluorobenzoato)(pyridine)platinum(II) (PFB), and trans-[N,N’-bis(1,2,3,5,6-pentafluorophenyl)ethane-1,2-diaminato(1-)](2,4,6-trimethylbenzoato)(pyridine)platinum(II) (TMB) were compared with cisplatin through their reaction with DNA. Attenuated Total Reflection Fourier Transform Infrared (ATR-FTIR) spectroscopy was applied to analyse the interaction of the Pt^(II) complexes with DNA in the hydrated, dehydrated and rehydrated state. These were compared with control DNA in acetone/water (PFB, TMB) and isotonic saline (cisplatin) under the same conditions. Principle Component Analysis (PCA) was applied to compare the ATR-FTIR spectra of the untreated control DNA with spectra of PFB and TMB treated DNA samples. Disruptions in the conformation of DNA treated with the Pt^(II) complexes upon rehydration were mainly observed by monitoring the position of the IR-band around 1711 cm^-1 assigned to the DNA base-stacking vibration. Furthermore, other intensity changes in the phosphodiester bands of DNA at ~1234 cm^-1 and 1225 cm^-1 and shifts in the dianionic phosphodiester vibration at 966 cm^-1 were observed. The isolated double stranded DNA (dsDNA) or single stranded DNA (ssDNA) showed different structural changes when incubated with the studied compounds. PCA confirmed PFB had the most dramatic effect by denaturing both dsDNA and ssDNA. Both compounds, along with cisplatin, induced changes in DNA bands at 1711, 1088, 1051 and 966 cm^-1 indicative of DNA conformation changes. The ability to monitor conformational change with infrared spectroscopy paves the way for a sensor to screen for new anticancer therapeutic agents.

In the last decade, the tremendous improvement in the sensitivity and also affordability of Liquid Chromatography-tandem Mass Spectrometry (LC-MS/MS) have revolutionized its application in pharmaceutical analysis, resulting in wide-spread of employing LC-MS/MS for determining pharmaceutical compounds including anticancer drugs in pharmaceutical research and also industries. Currently, LC-MS/MS has been widely used to quantify small molecule oncology drugs in various biological matrices to support preclinical and clinical Pharmacokinetic studies in R & D of oncology drugs. This mini-review article will describe the state-of-the art LC-MS/MS and its application in rapid quantification of small molecule anticancer drugs. In addition, efforts have also been made in this review to address several key aspects in the development of rapid LC-MS/MS methods, including sample preparation, chromatographic separation and matrix effect evaluation.

The exploitation of lipid membranes in biosensors has provided the ability to reconstitute a considerable part of their functionality to detect trace of food toxicants and environmental pollutants. Nanotechnology enabled sensor miniaturization and extended the range of biological moieties that could be immobilized within a lipid bilayer device. This chapter reviews recent progress in biosensor technologies based on lipid membranes suitable for environmental applications and food quality monitoring. Numerous biosensing applications are presented, putting emphasis on novel systems, new sensing techniques and nanotechnology-based transduction schemes. The range of analytes that can be currently detected include, insecticides, pesticides, herbicides, metals, toxins, antibiotics, microorganisms, hormones, dioxins, etc. Technology limitations and future prospects are discussed, focused on the evaluation/ validation and eventually commercialization of the proposed sensors.

In this study, the use of recycled diatomaceous earth as the extraction phase in a the solid phase microextraction (SPME) technique for the determination of polycyclic aromatic hydrocarbons (PAHs) in river water samples, with separation/detection performed by gas chromatography-mass spectrometry (GC-MS), is proposed. The optimized extraction conditions are extraction time 70 min at 80 ºC with no addition of salt. The limits of quantification were close to 0.5 μg L-1 with RSD values lower than 25% (n = 3). The linear working range was 0.5 μg L-1 to 25 μg L-1 for all analytes. The method was applied to samples collected from the Itajaí River (Santa Catarina, Brazil) and the RSD values for repeatability and reproducibility were lower than 15% and 17%, respectively. The efficiency of the recycled diatomaceous earth fiber was compared with that of commercial fibers and good results were obtained, confirming that this is a promising option for use as the extraction phase in SPME.

The high sensitivity of chiroptical responses to conformational changes and supramolecular interactions has prompted an increasing interest in the development of chiroptical applications. However, prediction and understanding the chiroptical responses of the necessary large systems may not be affordable for calculations at high levels of theory. In order to facilitate the development of chiroptical applications, methodologies capable of evaluating the chiroptical responses of large systems are necessary. Exciton chirality method has been extensively used for the interaction between two independent chromophores through the Davydov model. For systems presenting C2 or D2 symmetry one can get to the same results by applying the selection rules. In the present article, analysis of the selection rules for systems with symmetries Cn and Dn with n = 3 and 4 is used to uncover the origin of their chiroptical responses. We hope that the use of the chiroptical symmetry analysis (CSA) for systems presenting the symmetries explored herein as well as for systems presenting higher symmetries will serve as a useful tool for the development of chiroptical applications.

Drinking water contamination of lead from various environmental sources, leaching consumer products and intrinsic water-pipe infrastructure is still today a matter of great concern. Therefore, new highly sensitive and convenient Pb²⁺ measurement schemes are necessary, especially for in-situ measurements at a low-cost. Within this work dye/ionophore/Pb²⁺ co-extraction and effective water phase de-colorization was utilized for highly sensitive lead measurements and sub-ppb naked-eye detection. Low-cost ionophore Benzo-18-Crown-6-ether was used, and a simple test-tube mix, shake and separate procedure was developed. Instrumental detection limits were in the low ppt region (LOD=3, LOQ=10), and naked-eye detection was 500 ppt. Note, however, that this sensing scheme still has improvement potential as concentrations of fluorophore and ionophore were not optimized. Artificial tap-water samples, leached by a standardized method, demonstrated drinking water application. Implications for this method are convenient in-situ lead ion measurements.

In this work, unmodified screen-printed electrode (bare SPE) and Sb-film modified SPE (SbFSPE) sensors were employed for the analysis of trace amounts of Pb(II) in non-deaerated water solutions. The modified electrode was performed in situ in 0.5 mg/L Sb(III) and 0.01 M HCl. The methodology was validated for an accumulation potential of –1.1 V vs. Ag/AgCl and an accumulation time of 60 s. A comparative analysis of bare SPE and SbFSPE showed that the detection and quantification limits decrease for the bare SPE. The method with the bare SPE showed a linear response in the 69.8–368.4 µg/L concentration range, whereas linearity for the SbFSPE was in the 24.0–319.1 µg/L concentration range. This work also reports the reason why the multiple standard addition method instead of a linear calibration curve for Pb(II) analysis should be employed. Furthermore, the analytical method employing SbFSPE was found to be more accurate and precise compared to the use of bare SPE when sensors were employed for the first time, however this performance changed significantly when these sensors were reused in the same manner. Furthermore, electrochemical impedance spectroscopy was used for the first time to analyse the electrochemical response of sensors after being used for multiple successive analyses. Surface characterisation before and after multiple successive uses of bare SPE and SbFSPE sensors, with atomic force microscopy and field emission scanning electron microscopy, showed sensor degradation. The interference effect of Cd(II), Zn(II), As(III), Fe(II), Na(I), K(I), Ca(II), Mg(II), NO₃^– Bi(III), Cu(II), Sn(II), and Hg(II) on the Pb(II) stripping signal was also studied. Finally, the application of SbFSPE was tested on a real water sample (from a local river), which showed high precision (RSD = 8.1%, n = 5) and accurate results.

Determination of time-weighted average (TWA) concentrations of volatile organic compounds (VOCs) in air using solid-phase microextraction (SPME) is advantageous over other sampling techniques, but is often characterized by insufficient accuracies, particularly at longer sampling times. Experimental investigation of this issue and disclosing the origin of the problem is problematic and often not practically feasible due to high uncertainties. This research is aimed at developing the model of TWA extraction process and optimization of TWA air sampling by SPME using finite element analysis software (COMSOL Multiphysics). It was established that sampling by porous SPME coatings with high affinity to analytes is affected by slow diffusion of analytes inside the coating, an increase of analytes concentrations in the air near the fiber tip due to equilibration, and eventual lower sampling rate. The increase of a fiber retraction depth (Z) resulted in better recoveries. Sampling of studied VOCs using 23-ga Car/PDMS assembly at maximum possible Z (40 mm) was proven to provide more accurate results. Alternative sampling configuration based on 78.5 x 0.75 mm i.d. SPME liner was proven to provide similar accuracy at improved detection limits. Its modification with the decreased internal diameter from the sampling side should provide even better recoveries. The developed model offers new insight into optimization of air and gas sampling using SPME.

The present study was carried out at the north-eastern part of Bangladesh to investigate organochlorine pesticide (OCP) residues and microbiological quality of dried barb (Puntius sophore). Samples were collected from both producers and retailers from December 2016 to April 2017. A control sample was also prepared with the same raw fish used by the producers in the laboratory to compare the result. Gas Chromatography with Electron Capture Detector (GC-ECD) was used to detect and quantify OCP residues. Around 22 % (6) samples out of 27 were found contaminated with OCP residues. Among these six adulterated samples, four were from retailers and two from producers. Only Aldrin was detected in four samples and rest two samples were detected with both Aldrin + Dieldrin and Aldrin + Endrin. Aldrin was found between 0.332 to 0.967 ppm, Dieldrin 0.762 ppm, and Endrin 0.828 ppm. All these values were much higher than the Maximum Residual Limit (MRL) 0.1 ppm. Aerobic Plate Count (APC) of producer samples were ranged between log5.3 ± 0.02 to log5.4 ± 0.03, log6.2 ± 0.02 to log6.4 ± 0.02 for retailer samples and log5.0 ± 0.03 to log5.2 ± 0.04 for control samples. While fungal count was ranged between log3.2 ± 0.04 to log3.5 ± 0.04, log3.4 ± 0.04 to log3.6 ± 0.03 and log2.2 ± 0.05 to log2.5 ± 0.03 for producer, retailer and control samples respectively. All the producer and retailer samples and one-third of the control samples were found contaminated with Escherichia coli. Whereas, Salmonella sp. was detected as 13.3% in producer samples, 20% in retailer samples except for the control. In case of Vibrio sp., maximum count was found for retailer samples (13.3%), whereas, producer and control samples showed no detection. The finding of the present study revealed the presence of pesticides and poor microbiological quality of dried barb are alarming for the consumers of Bangladesh and which may cause chronic disease and potential long-term risk for human health.

In this study, an improved UPLC-MS method for simultaneously quantifying twelve major components belonging to two chemical types was developed and validated, and was applied to quantitatively compare the quality of Astragali Radix sulfur-fumigated with different durations and the fresh reference sample. The results showed that the contents of triterpenes Astragaloside III and Astragaloside IV decreased moderately, while the flavonoids calycosin, formononetin, and 7,2'-dihydroxy-3',4'-dimethoxyisoflavane decreased significantly, and its corresponding flavonoid glycosides increased accordingly, which indicatied that the happening of chemical transformation of flavonoids and glycosides in the sulfur-fumigated process. These transformations were further confirmed by the the synthesis of flavonoid glycosides under the simulated sulphur-fumigation circumstances. Furthermore, the sulfur-fumigated duration had a proportional relationship with the contents of compounds 7, 11, and 12. All these results suggested that the established method was precise, accurate and sensitive enough for the global quality evaluation of sulfur-fumigated Astragali Radix, and sulfur-fumigation can not only change the proportions of bioactive components, but also cause the chemical transformation in the Astragali Radix.

Given the rise in the number of cases and their recurrences, Urinary Tract Infections (UTI) are one of the major burdens on public healthcare worldwide. Rapid, inexpensive and selective detection of Uropathogenic E. coli (UPEC), a major contributor to UTIs, is the need of the hour for effective treatment, given the rise of antibiotic-resistant bacteria due to improper diagnosis. Here we present a rapid, real-time, selective and label-free detection of UPEC using an integrated sensing platform based on Crossed Surface Relief Gratings (CSRGs) as nanoplasmonic sensors. Detection is achieved due to the unique Surface Plasmon Resonance (SPR)-based light energy exchange attributed to the CSRGs, allowing real-time sensing in a very narrow bandwidth of the incident light to pass where the SPR energy conversion occurs. The sensing ability of the platform is experimentally demonstrated by the detection of bulk Refractive Index (RI) changes, with a bulk sensitivity of 382.2 nm/RIU and a resolution in the order of 10-6 RIU. We demonstrate selective capture and detection of clinical concentration of UPEC, as opposed to other gram-negative bacteria, in real-time, a first for CSRGs. This work is particularly important for effective treatment of UTIs, allowing point-of-care diagnosis for economically disadvantaged regions around the world.

Headspace solid phase microextraction (HS-SPME) coupled to gas chromatography-mass spectrometry is widely employed for volatile analyses of plants, including mapping populations used in plant breeding research. Studies often employ a single internal surrogate standard, even when multiple analytes are measured, with the assumption that any relative changes in matrix effects among individuals would be similar for all compounds, i.e. matrix effects do not show Compound × Individual interactions. We tested this assumption using individuals from two plant populations, an interspecific grape (Vitis spp.) mapping population (n = 140) and a tomato (Solanum spp.) recombinant inbred line (RIL) population (n = 148). Individual plants from the two populations were spiked with a cocktail of internal standards (n = 6, 9, respectively) prior to HS-SPME-GC-MS. Variation in the relative responses of internal standards indicated that Compound × Individual interactions exist but were different between the two populations. For the grape population, relative responses among pairs of internal standards varied considerably among individuals, with a maximum of 249% relative standard deviation (RSD) for the pair of [U13C]hexanal and [U13C]hexanol. However, in the tomato population, relative responses of internal standard pairs varied much less, with pairwise RSDs ranged from 8% to 56%. The approach described in this paper could be used to evaluate the suitability of using surrogate standards for HS-SPME-GC-MS studies in other plant populations.

1) Background: Recently, illegal abuse of γ-hydroxybutyric acid (GHB) has increased in drug-facilitated crimes, but determination of GHB exposure and intoxication is difficult due to rapid metabolism of GHB. Its biochemical mechanism has not been completely investigated. And metabolomic study by polyamine profile and pattern analyses was not performed in rat urinefollowing intraperitoneal injection with GHB. 2) Methods: Polyamine profiling analysis by gas chromatography-mass spectrometry combined with star pattern recognition analysis was performed in this study. Multivariate statistical analysis was used to evaluate discrimination between control and GHB administration groups. 3) Results: Six polyamines were determined in control, single and multiple GHB administration groups. Star pattern showed distorted hexagonal shapes with characteristic and readily distinguishable patterns for each group. N¹-Acetylspermine (p < 0.001), putrescine (p <0.006), N¹-acetylspermidine (p <0.009), and spermine (p < 0.027) were significantly increased in single administration group but were significantly lower in the multiple administration group than in the control group. N¹-Acetylspermine was the main polyamine for discrimination between control, single and multiple administration groups. Spermine showed similar levels in single and multiple administration groups. 4) Conclusions: The polyamine metabolic pattern was monitored in GHB administration groups. N¹-Acetylspermine and spermine were evaluated as potential biomarkers of GHB exposure and addiction.

In this study, four kinds of animal bone marrow powders were extracted with n-hexane using the Soxhlet extraction method. Polyunsaturated fatty acids were enriched by urea inclusion and low temperature crystallization method, then were further evaluated antioxidant and antibacterial activities. These results showed that the oil composition of the n-hexane extracts of four kinds of animal bone marrow primarily consisted of palmitic acid (18.57–31.01%), stearic acid (3.6–20.95%), and oleic acid (40.22–58.69%). The ratios of saturated fatty acids (SFA)/unsaturated fatty acids (UFA) were 1/1.417, 1/1.327, 1/2.140, and 1.285/1 for sheep, bovine, horse, and camel bone marrow oil, respectively. The SFA/UFA ratios determined by the urea inclusion method were 1/1.518, 1/1.390, 1/2.037, and 1.216/1, respectively. The SFA/UFA ratios according to the low temperature crystallization method with acetone were 1/1.920, 1/2.141, 1/2.360, and 1/1.157 for sheep, bovine, horse, and camel bone marrow oil, respectively. These enrichment methods effected the concentrations of UFAs from the camel bone marrow oil. Among the methods, the low temperature crystallization method effectively enriched the UFAs. All four bone marrow oils exhibited strong antioxidant and antimicrobial activities. The horse bone marrow oil showed the strongest antioxidant activity. Both antioxidant and antimicrobial activity improved after enrichment of the UFAs. These results lay a theoretical basis for application bone marrow oil resources in food and medicine.

Direct mass spectrometry-based metabolomics has been widely employed in the last years to characterize metabolic alterations underlying to Alzheimer’s disease development and progression. This high-throughput approach presents a great potential for fast and simultaneous fingerprinting of a vast number of metabolites, which can be applied to multiple biological samples such as serum/plasma, urine, cerebrospinal fluid and tissues. In this review article we present the main advantages and drawbacks of metabolomics based on direct mass spectrometry compared with conventional analytical techniques, and provide a comprehensive revision of the literature on the application of these tools in Alzheimer’s disease research.

Concentrations of six polycyclic aromatic hydrocarbons (benzanthrone, benz[a]anthracene, chrysene, fluoranthene, pyrene, and triphenylene) of soil samples from Diboll, an East Texas city (USA), were analyzed with gas chromatography-mass spectrometry (GC-MS). Samples were collected from five sites; Old Orchard Park, two heavy traffic intersections (Judd Street and Lumberjack Drive), an industrial site (West Borden Drive), and a truck stop. Acetone and dichloromethane extracts in all samples showed the presence of fluoranthene and pyrene. The sum of fluoranthene and pyrene concentrations in sites followed the order West Borden Drive > Judd Street > Lumberjack Drive > Old Orchard Park > truck stop. Concentrations of fluoranthene and pyrene were in the range 12.3 – 396.5 μg kg^-1 (ppb) and 13.6 – 209.8 μg kg^-1 ₍in dry soil₎, respectively. Benzanthrone, benz[a]anthracene, chrysene, and triphenylene concentrations were < 2 ppb levels. The higher concentrations in soils were associated with sites close to heavy traffic and vehicular emissions.

A new type of gold nanoparticles was synthesized by using benzoyl pyrazolone as a capping agent. The synthesized AuNPs exhibited a spherical shape and a monodisperse and fluorescence emission characteristic peak at 650 nm. The AuNPs –BMPBP was demonstrated as sensitive and selective fluorescent chemosensor for detection of Al ³⁺ ion. In the presence of Al ³⁺ ion, the fluorescent emission of BMPBP-AuNPs at 650 nm, increased with an increasing concentration of  Al ³⁺ ion with a low detection limit (2 µM), the proposed method provided to apply determination of Al ³⁺ ion of tap water with satisfactory results.

The exploitation of lipid membranes in biosensors has provided the ability to reconstitute a considerable part of their functionality to detect trace of food toxicants and environmental pollutants. Nanotechnology enabled sensor miniaturization and extended the range of biological moieties that could be immobilized within a lipid bilayer device. This chapter reviews recent progress in biosensor technologies based on lipid membranes suitable for environmental applications and food quality monitoring. Numerous biosensing applications are presented, putting emphasis on novel systems, new sensing techniques and nanotechnology-based transduction schemes. The range of analytes that can be currently detected include, insecticides, pesticides, herbicides, metals, toxins, antibiotics, microorganisms, hormones, dioxins, etc. Technology limitations and future prospects are discussed, focused on the evaluation/ validation and eventually commercialization of the proposed sensors.

Gas chromatography-olfactometry/mass spectrometry coupled with headspace-solid phase microextraction (HS-SPME/GC-O/MS) was applied for the characterization of volatile compounds in Tom Yum soup and its individual ingredients. Using HS-SPME with a 50/30 µm DVB/CAR/PDMS fiber and an extraction temperature of 40 °C for 50 min along with an HP-5MS capillary column, 101 peaks in the HS-SPME/GC-MS chromatogram of Tom Yum soup were detected, and 96 compounds were identified including alcohols, aldehydes, esters, ethers, and terpenes. These findings are based on the comparison of MS spectra with the NIST library as well as experimental and literature retention index data. In comparison with the compound profiles of each individual ingredient of Tom Yum soup (both before and after cooking), five extra volatile compounds in Tom Yum soup were found after the cooking process. Furthermore, odor descriptions of the eighteen aroma compounds in Tom Yum soup, along with the odor ingredient sources, were also obtained.

Forensic detection of non-volatile nitro explosives poses a tough analytical challenge. A colorimetric sensor comprising ultrasonically prepared silica-dye microspheres was developed for sensitive gas detection of cyclohexanone, a volatile marker of explosives 1,3,5-trinitro-1,3,5-triazinane (RDX) and 1,3,5,7-tetranitro-1,3,5,7-tetrazocane (HMX). The silica-dye composites were synthesized from the hydrolysis of ultrasonically sprayed organosiloxanes under mildly heating conditions (150 ^oC), which yields microspherical, nanoporous structures with high surface area (~300 m²/g) for gas exposure. The sensor inks were deposited on cellulose paper and gave sensitive colorimetric responses to trace amount of cyclohexanone vapors even at sub-ppm levels, with the detection limit down to ~150 ppb. The sensor showed high chemical specificity towards cyclohexanone against humidity and other classes of common solvents, including ethanol, acetonitrile, ether, ethyl acetate, and ammonia. Paper-based colorimetric sensors with hierarchical nanostructures could represent an alternative sensing materials for practical applications in the detection of explosives.

Elephant dung coffee (Black Ivory Coffee) is a special Thai coffee produced from Arabica coffee cherries consumed by Asian elephants and collected from their feces. In this work, elephant dung coffee and controls were analyzed using static headspace gas chromatography hyphenated with mass spectrometry (SHS GC–MS), and chemometric approaches were applied for multivariate analysis and the selection of marker compounds that are characteristic of the coffee. Seventy-eight volatile compounds belonging to 13 chemical classes were tentatively identified, including 6 alcohols, 5 aldehydes, one carboxylic acid, 3 esters, 17 furans, one furanone, 13 ketones, 2 oxazoles, 4 phenolic compounds, 14 pyrazines, one pyridine, 8 pyrroles and 3 sulfur-containing compounds. Moreover, four potential discriminant markers of elephant dung coffee, including 3-methyl-1-butanol, 2-methyl-1-butanol, 2-furfurylfuran and 3-penten-2-one were established. The proposed method may be useful for elephant dung coffee authentication and quality control.

In this work, we firstly explored a mild, clean, and highly efficient approach for the synthesis of graphene quantum dots (GQDs). GQDs with carboxyl groups or amino groups, were prepared from one-pot environmentally friendly method assisted by hydrogen peroxide, respectively. It was proved that carboxyl groups played an important role in the fluorescence quenching. Based on these findings, we developed a novel fluorescent nanosensor by combining molecularly imprinted polymers (MIPs) with carboxyl functionalized GQDs for the determination of tetracycline (TC) in aqueous samples. The nanocomposite was prepared using a sol-gel process. GQDs-MIPs showed strong fluorescent emission at 410 nm when excited at 360 nm, which was subsequently quenched in the presence of TC. Under optimum conditions, the fluorescence intensity of GQDs-MIPs decreased in response to the increase of TC concentration with good linearity rage of 1.0-104 µg L-1. The limit of detection was determined to be 1 µg L-1. The fluorescence intensity of GQDs-MIPs was more strongly quenched by TC compared to the corresponding non-imprinted polymers, GQDs-NIPs. With the high sensitivity, the material was also successfully worked for the detection of TC in real spiked milk samples.

The problem of limited water supply in the Vhembe District (Limpopo Province, South Africa) is exacerbated by a preponderance of dissolved salts, which cause disagreeable taste and odour in the water as reported by the communities using this water for drinking. The water treatment plant that supplies the treated water to the communities in the District sources this raw water from the Nandoni Dam at the Livhuvu river catchment. However, there are no scientific studies that have been reported in the literature which focused on determining the levels of water salinity from various water sources in the municipalities of the District. Water samples from various sites across the Nandoni Dam, a primary source of domestic water supply in the region, were collected during all the seasons basis over a period of twelve months in order to ascertain the concentrations of dissolved salts in the dam. Onsite analyses of the water samples were conducted using the YSI ProDSS multimeter, while the laboratory water analyses were conducted using the spectroquant and atomic absorption spectrometers. Although salinity tests seem to indicate that the water sampled across most of the Nandoni Dam is brackish during all seasons of the year with the highest being 750 mg/L, water samples from the dam mid-outlet and the treatment plant are slightly below the WHO brackish water bracket of 500 mg/L with unfavourable taste for drinking. Results from this study indicate that the water sourced from the Nandoni Dam is not suitable for human consumption and therefore requires integrated water resource management, as well as robust and cost-effective water desalination treatment.

Different kinds of freshwater fish soups show a diverse range of health functions, due to their different nutritional substances and corresponding bioactivities. Crucian carp soup and snakehead soup have different dietotherapy functions, crucian carp soup is suitable for lactating women and snakehead soup is suitable for postoperative patients. In the current study, the changes of nutrient profiles in the different fish soups, such as chemical composition, free amino acids, mineral and fatty acid contents, were investigated. The antioxidant activities of the fish soups were evaluated by using the DPPH radical scavenging activity, the ferrous ion chelating activity, the hydroxyl radical-scavenging activity and the reducing power effect. In order to learn the theoretical basis of the potential role fish soup plays in diet therapy functions after being digested by the human body, the nutrient profiling and bioactivities of the fish soup samples after simulated gastrointestinal digestion were also explored. The intensive profiles of nutritional composition and antioxidant activities of these two kinds of fish soups were expected to partly provide the theoretical basis of therapeutic effects.

High-throughput screening of samples is the strategy of choice to detect occupational exposure biomarkers, yet it requires user-friendly apparatus that gives relatively prompt results while ensuring high degrees of selectivity, precision, accuracy and automation, particularly in preparation processes. In the last 10 years, miniaturization has attracted much attention in analytical chemistry and has driven solvent and sample savings and easier automation, the latter thanks to the introduction on the market of three axis autosampler. In light of the above, this contribution describes a novel user-friendly solid-phase microextraction (SPME) off- and on-line platform coupled with gas chromatography triple quadrupole-mass spectrometry to determine urinary 1- and 2-hydroxy-napthalene, 9-hydroxy-phenantrene, 1-hydroxy-pyrene, 3- and 9-hydroxy-benzoantracene and 3-hydroxy-benzo[a]pyrene, metabolites of the related polycyclic aromatic hydrocarbons. In this new procedure chromatography’s sensitivity is combined with the user-friendliness of N-tert-butyldimethylsilyl-N-methyltrifluoroacetamide on-fiber SPME derivatization previous direct immersion sampling, to which is added the quantitative accuracy afforded using specific isotope-labelled internal standards. The detection limits for the seven OH-PAHs were ranged from 0.28 to 1.87 ng/L. Intra-(from 2.5 to 3.0%) and inter-session (from 2.4 to 3.9%) repeatability was also evaluated. This method serves to identify suitable risk-control strategies for occupational hygiene conservation programs

The high sensitivity of chiroptical responses to conformational changes and supramolecular interactions has prompted an increasing interest in the development of chiroptical applications. However, prediction and understanding the chiroptical responses of the necessary large systems may not be affordable for calculations at high levels of theory. In order to facilitate the development of chiroptical applications, methodologies capable of evaluating the chiroptical responses of large systems are necessary. Exciton chirality method has been extensively used for the interaction between two independent chromophores through the Davydov model. For systems presenting C2 or D2 symmetry one can get to the same results by applying the selection rules. In the present article, analysis of the selection rules for systems with symmetries Cn and Dn with n = 3 and 4 is used to uncover the origin of their chiroptical responses. We hope that the use of the chiroptical symmetry analysis (CSA) for systems presenting the symmetries explored herein as well as for systems presenting higher symmetries will serve as a useful tool for the development of chiroptical applications.

Graph theory plays a crucial role in modeling and designing of chemical structure or chemical network. Chemical Graph theory helps to understand the molecular structure of molecular graph. The molecular graph consists of atoms as vertices and bonds as edges. Topological indices capture symmetry of molecular structures and give it a mathematical language to predict properties such as boiling points, viscosity, the radius of gyrations etc. In this article, we study the chemical graph of carbon Crystal structure of graphite and cubic carbon and compute several degree-based topological indices. Firstly we compute M-Polynomials of these structures and then from these M-polynomials we recover nine degree-based topological indices.

The aim of this study (first analytical approach) was to obtain data on the fatty acid composition of gluten-free foods (bakery products) for celiac people. The study included 35 different products (snacks, biscuits, bakery products, pasta, flours, etc.) from several manufacturers. After extraction and esterification, the fatty acid content was determined by GC-MS. The monounsaturated fatty acids (MUFAs) are the major constitutes (57%) of the fatty acids pool followed by saturated fatty acids (SFAs) (30%) and polyunsaturated fatty acid (13%). Only fifteen, of the thirty-five gluten free samples analyzed, provide adequate energy intake, while in eleven samples, saturated fatty acids take more energy than that recommended by EFSA. It has emerged that local producers generally use the finest raw materials (olive oil, etc.) compared to the industries which, as has been pointed out, in many cases use palm and palm kernel oils although gluten free commercial products are high added value foods, expensive and intended for a particularly sensitive public.

The application of graph theory in chemical and molecular structure research far exceeds people's expectations, and it has recently grown exponentially. In the molecular graph, atoms are represented by vertices and bonded by edges. In this report, we study the silicon-carbon Si₂C₃-I[p,q] and Si₂C₃-II[p,q]. We compute several Zagreb polynomials and Redefined Zagreb indices of these silicon-carbons.

Quantitative structure-activity relationship (QSAR) model is adopted to study the relationship between the chemical and physical properties of various substances and the structure. Through QSAR studies, the internal relationship between the invisible structure and the activity can be obtained. In this paper, a novel chaos-enhanced accelerate particle swarm algorithm (CAPSO) is proposed, which is used to molecular descriptors screening and optimization of the weights of back propagation artificial neural network (BP ANN). Then, the QSAR model based on CAPSO and BP ANN is put forward, hereinafter referred to as CAPSO BP ANN model. The prediction experiment showed that the CAPSO algorithm is a reliable method for screening molecular descriptors and the five molecular descriptors obtained by CAPSO algorithm could well characterize the molecular structure of each compound in pKa prediction. The experimental results also showed the CAPSO BP ANN model has a good performance in predicting the pKa values of various compounds, the absolute mean relative error, root mean square error, and square correlation coefficient are respectively 0.5364, 0.0632, and 0.9438, indicating the higher prediction accuracy and correlation. The proposed hybrid intelligent model can be applied in all kinds of engineering design, prediction of physical and chemical properties and intelligent calculation.

Three new secoiridoid constituents Gonocarin A-C (1-3) and a new derivative Gonocarin A monoacetate (4), along with two known lignins pinoresinol (5) and paulownin (6) were isolated from the seed of Gonocaryum calleryanum (Baill.) Becc. The structures of the new metabolites were determined on the basis of extensive spectroscopic analysis, particularly mass spectroscopy and 2D NMR (1H–1H COSY, HMQC, HMBC, and NOESY) spectroscopy. When mouse macrophages RAW264.7 were treated with compounds 1-6 together with LPS -stimulated, a concentration-dependent inhibition of nitric oxide (NO) and tumor necrosis factor (TNF-α) productions were detected. The results confirmed that the Gonocaryum calleryanumrrg could be a potential anti-inflammatory agent.

This review provides informations and details for the fabrication of biosensors that are composed from lipid membranes and have been utilized and applied to rapidly detect food toxic compounds, environmental pollutants and analytes of clinical interest. Biosensors based on polymeric lipid membranes have been used to rapidly detect a wide range of these analytes and offer several advantages such as fast response, high sensitivity and selectivity, can be portable for in the field applications, and small size. A description of the construction of these devices and their applications for the rapid detection of food toxic substance, environmental pollutants and analytes of clinical interest is provided in this review.

In the study of QSAR/QSPR, due to high degree of predictability of pharmaceutical properties, the eccentric-connectivity index has very important place among the other topological descriptors, In this paper, we compute the exact formulas of eccentric-connectivity index and its corresponding polynomial, total eccentric-connectivity index and its corresponding polynomial, first Zagreb eccentricity index, augmented eccentric-connectivity index, modified eccentric-connectivity index and its corresponding polynomial for a class of phosphorus containing dendrimers.

NaoMaiTong (NMT: Radix et Rhi-zoma Rhei, Radix Ginseng, Radix Puerariae, and Rhizoma Ligustici Chuanxiong as 9: 9: 6: 6) is a traditional Chinese medicine prescription for treating ischemia cerebral apoplexy. In this work, four cell injury models of ischemic stroke were establish, namely hypoxic injury, glutamate damage, injury of potassium chloride and hydrogen peroxide damage model. The protective effects of NMT and its single herbs-containing sera of different time points on PC12 cell damage were evaluated respectively, and the corresponding efficacy-time curves were drawn. Cell viability was measured by MTT (3-(4,5)-Dimethylthiahiazo(-z-y1)-3,5-di-phenytetrazoliumromide) assay. Furthermore, an statistical methods of support vector machine (SVM) were used to establish the correlation between concentration-time-efficacy for the first time. These results revealed that NMT-containing serum has obvious protective effect on the four injury models and can significantly improve cell viability. The PK-PD correlation between fifteen ingredients in the NMT compound with four model efficacy indexes indicated that rhein, puerarin, and 3'-methoxy puerarin might be the most important constituents controlling the pharmacological effects of NMT. The study suggested that these fifteen components are likely to be the material basis of NMT and recommended to increase the amounts of Pueraria in the NMT compound. That provided the scientific basis and demonstration for the research of efficacy material base of Traditional Chinese Medicine (TCM).

Pomegranate juice (PJ) has total antioxidant capacity (TAC) which is reportedly higher compared to other common beverages. This short study aimed to evaluate the TAC of commercial PJ and pomegranate fruit in terms of a newly described iron (III) reducing antioxidant capacity (iRAC) and to compare with ABTS free radical quenching activity. Commercial PJ, freeze-dried pomegranate, and oven dried-pomegranate were analyzed. The total phenols content (TPC) was also assessed by the Folin-Ciocalteu method. The calibration results for iRAC were comparable to ABTS and Folin-Ciocalteu methods in terms of linearity (R2 > 0.99), sensitivity and precision. The TAC for PJ expressed as trolox equivalent antioxidant capacity (TEAC) was 33.4 ± 0.5 mM with the iRAC method and 36.3 ± 2.1 mM using the ABTS method. For dried pomegranates, TAC was 89–110 mmol/100 g or 76.0 ± 4.3 mmol/100 g using iRAC and ABTS methods, respectively. Freeze-dried pomegranate had 15% higher TAC compared with oven-dried pomegranate. In conclusion, pomegranate has high TAC as evaluated by the iRAC and ABTS methods, though variations occur due to the type of cultivar, geographic origin, processing and other factors. The study is relevant for attempts to refine food composition data for pomegranate and other functional foods.

Re-investigation of the chemical composition of the annual plant Mitracarpus scaber Zucc. led to the identification of clarinoside, a new pentalogin derivative containing a rare quinovose moiety, and the known compound harounoside. While the planar structure was fully determined using tandem MS and quantum mechanics calculations (QM), the tridimensional structure was unravelled after isolation and NMR analysis. The absolute configuration was assigned by comparison of experimental and theoretical SRCD spectra. Both compounds were tested for anti-inflammatory activity and compound 1 showed the ability to inhibit the production of interleukin-8 (Il-8) with an IC₅₀ of 9.17 µM.

Antibiotic resistance and accordingly their pollution because of uncontrolled usage has emerged as a serious problem in recent years. Hence, there is an increased demand to develope robust, easy, and sensitive methods for rapid evaluation of antibiotic and their residues. Among different analytical methods, the aptamer-based biosensors (aptasensors) have attracted considerable attention because of good selectivity, specificity, and sensitivity. This review gives an overview about recent developed aptasensors for antibiotic detection. The use of various aptamer assays to determine different groups of antibiotics like β-lactams, Aminoglycosides, Anthracyclines, Chloramphenicol, (Fluoro)Quinolones, Lincosamide, Tetracyclines and Sulfonamides are presented in this paper.

Antibiotic resistance and accordingly their pollution because of uncontrolled usage has emerged as a serious problem in recent years. Hence, there is an increased demand to develope robust, easy, and sensitive methods for rapid evaluation of antibiotic and their residues. Among different analytical methods, the aptamer-based biosensors (aptasensors) have attracted considerable attention because of good selectivity, specificity, and sensitivity. This review gives an overview about recent developed aptasensors for antibiotic detection. The use of various aptamer assays to determine different groups of antibiotics like β-lactams, Aminoglycosides, Anthracyclines, Chloramphenicol, (Fluoro)Quinolones, Lincosamide, Tetracyclines and Sulfonamides are presented in this paper.

This paper reports a novel fabric phase sorptive extraction-high performance liquid chromatography-ultra violet detection (FPSE-HPLC-UV) method for the simultaneous extraction and analysis of four phenyltin derivatives that include triphenyltin hydroxide, triphenyltin acetate, triphenyltin chloride and tetraphenyltin in environmental water (agricultural waste water and municipal waste water) and canned food samples. The selected analytes were well resolved by Waters Nova pack C18 column (3.9 x 150 mm, 4 µm particle size) in isocratic elution mode within 15 minutes. The new microextraction media has been analytically evaluated using phenyltin derivatives as model compounds. The factors affecting the extraction efficiency of FPSE have been evaluated and the optimum extraction conditions were determined. Under these optimum conditions, the limits of detection (LODs) for sol-gel C18 coated fabric phase sorptive extraction (FPSE) media in combination with HPLC-UV for the analysis of the phenyltin derivatives were in the range of 10-100 ng/mL with high precision (low relative standard deviation) at 10 ng/mL concentration with good absolute recoveries. To the best of our knowledge, this is the first FPSE extraction procedure applied to environmental water and canned food samples for the simultaneous determination of phenyltin derivatives and could be readily adopted as a rapid and robust green analytical tool for routine environmental and food analytical laboratories.

Since the systematic evolution of ligands by exponential enrichment (SELEX) method was developed, aptamers have made significant contributions as bio-recognition sensors. Microdevice systems allow for low reagent consumption, high-throughput of samples, and disposability. Due to these advantages, there has been an increasing demand to develop microfluidic-based aptasensors for analytical technique applications. This review introduces the principal concepts of aptasensors and then presents some advanced applications of microdevice-based aptasensors on several platforms. Highly sensitive detection techniques such as electrochemical and optical detection have been integrated into lab-on-a-chip devices and researchers have moved towards the goal of establishing point-of-care diagnoses for target analyses.

A novel plasma source of pulsed electrolyte cathode atmospheric pressure discharge (pulsed-ECAD) driven by an alternating current (AC) power supply coupled with a high voltage diode was generated, and the discharge was generated in the open-to-air atmosphere between a metal electrode and a small-sized flowing liquid cathode. The spatial distribution of plasma temperatures (excitation, vibrational and rotational) of the pulsed-ECAD were investigated. The electron excitation temperature of H T_exc(H), vibrational temperature of N₂ T_vib(N₂), and rotational temperature of OH T_rot(OH) were measured as 4900±36-6800±108 K, 4600±86-5800±100 K and 1050±20-1140±10 K, respectively. Meanwhile, the temperature characteristics of dc solution cathode glow discharge (dc-SCGD) were also studied for comparison with pulsed-ECAD. The effects of operating parameters, including discharge voltage and discharge frequency, on the plasma temperatures were investigated. The electron number density determined in the discharge system and dc-SCGD were within the range (3.8–18.9) ×10¹⁴ cm^-3 and 2.6×10¹⁴-17.2×10¹⁴ cm^-3, respectively.

4-(thiazol-2-yldiazenyl)phenol (L₁) and 2-((4-hydroxyphenyl) diazenyl)-5-nitrophenol (L₂) based on azo phenol were synthesised and used as selective colorimetric sensor for CN^- and AcO⁻ ion in DMSO/H₂O-HEPES (v/v; 1:1, pH–7.3 ± 0.2) and showed good sensitivity with large red shifts and nanomolar detection limit for CN^- and AcO^- ion. The stoichiometry of L₁ with CN⁻/AcO⁻ ion was found to be 1:1 and L₂ with CN⁻/AcO⁻ ion was found to be 1:2. Binding constant for L₁+ CN⁻, L₁ + AcO⁻, L₂ + CN⁻ and L₂ + AcO⁻ were calculated by B-H plot as 1.6 × 10³, 8.0 × 10², 8.4 × 10³ and 1.7 × 10² respectively. L₂ showed high selectivity towards CN⁻ ion with low detection limit of 81 nM and large binding constant. In addition, ¹H NMR titration and DFT studies also supported the deprotonation mechanism of receptors in the presence of selective anions.

Re-investigation of the chemical composition of the annual plant Mitracarpus scaber Zucc. led to the identification of a new pentalogin derivative containing a rare quinovose moiety. While the planar structure has been fully determined using tandem MS and quantum mechanics calculations (QM), the tridimensional structure was unraveled after isolation and NMR analysis. The absolute configuration was assigned by comparison of experimental and theoretical SRCD spectra. Both compounds were tested for anti-inflammatory activity and compound 1 showed the ability to inhibit the production of interleukin-8 (Il-8) with an IC₅₀ of 9.17 µM.

Pollution caused by copper is one of the key factors of environment contamination. As one of heavy metals, copper is hard to decompose in nature, the biological enrichment of which may lead to severe damage to health. Cu²⁺ detection, thus, possesses a bright application prospect both in environment protection and in human health. In this paper, a dual-functional fluorescence-magnetic composite nano-platform has been designed to sensitively detect, meanwhile capture and remove Cu²⁺ in the solution of water and ethanol (1:1, v/v). The core-shell structure nanoparticle synthesized by using Fe₃O₄ as core and SiO₂ as shell, is covalently bonded with rhodamine derivatives on the silica layer to construct the nano-platform. The emission is increased upon the addition of Cu²⁺, showing fluorescence turn on effect for the detection, and the limit of detection which was as low as 1.68 nM. Meanwhile, Cu²⁺ ions are captured by the coordination with rhodamine derivatives, and can be removable with the help of magnetic field.

Guayule (Parthenium argentatum Gray) is a shrub native of the arid regions of Mexico. In the last decades, significant attention for its cultivation has risen because it is the raw material for the production of hypoallergenic natural rubber. Guayule biomass contains also high amounts of resin, which is not normally exploited in any way. Among other sesquiterpenic esters, guayulins (i.e. the parteniol esters of cinnamic acid, guayulin A, or of anisic acid, guayulin B) are contained in resin. In addition, minor amounts of guayulin C and guayulin D are formed by degradation/oxidation of guayulins A and B, respectively. Guayulins likely act as cinnamate and p-anisate reservoirs for Guayule shrub, in addition, it has been postulated that they might have a key role in the chemical defense system of Guayule. Furthermore, it seems reasonable that guayulins may possess significant biological properties (e.g. antibacterial and anticancer activities), in close analogy with those shown by sesquiterpene lactones contained in many other species of Parthenum genus. As a matter of fact, guayulins A and B play an important role in the synthesis of antineoplastics used in breast cancer treatment. In this contribution we propose an original and validated RP-HPLC approach to the simultaneous quantification of guayulins A, B, C and D. The procedure of resin extraction from Guayule biomass has been optimized in terms of both extraction method and solvent. RP-HPLC separation has been accomplished by an Ascentis^® C18 column under isocratic elution with a 80:20 (v:v) acetonitrile:water mixture. Validation was carried out in terms of limits of detection and quantification, linearity, precision, and trueness. Finally, the method was tested with a number of fresh and seasoned samples of spontaneous Guayule shrub from Mexico.

Guayule (Parthenium argentatum Gray) is a shrub native of the arid regions of Mexico. In the last decades, significant attention for its cultivation has risen because it is the raw material for the production of hypoallergenic natural rubber. Guayule biomass contains also high amounts of resin, which is not normally exploited in any way. Among other sesquiterpenic esters, guayulins (i.e. the parteniol esters of cinnamic acid, guayulin A, or of anisic acid, guayulin B) are contained in resin. In addition, minor amounts of guayulin C and guayulin D are formed by degradation/oxidation of guayulins A and B, respectively. Guayulins likely act as cinnamate and p-anisate reservoirs for Guayule shrub, in addition, it has been postulated that they might have a key role in the chemical defense system of Guayule. Furthermore, it seems reasonable that guayulins can possess significant biological properties (e.g, antibacterial and anticancer activities), in close analogy with those shown by sesquiterpene lactones in many other species of Parthenum genus. As a matter of fact, guayulins A and B play an important role in the synthesis of antineoplastics used in breast cancer treatment. In this contribution we propose an original and validated RP-HPLC approach to the simultaneously quantification of guayulins A, B, C and D. The procedure of resin extraction from Guayule biomass has been optimized in terms of both nature of extraction method and solvent of extraction. RP-HPLC separation has been accomplished on an Ascentis^® C18 column under isocratic elution with a 80:20 (v:v) acetonitrile:water mixture. Validation was carried out in terms of both the limit of detection, limit of quantification, linearity, precision, and trueness. Finally, the method was tested with a number of fresh and seasoned samples of spontaneous Guayule shrub from Mexico.

Tributyltin (TBT) is one of the most toxic anthropogenic compounds introduced into the marine environment. Despite its global ban in 2008, TBT is still a problem of great concern due to its high affinity for particulate matter, providing a direct and potentially persistent route of entry into benthic sediments. Bioremediation strategies may constitute an alternative approach to conventional physicochemical methods, benefiting from the microorganism’s potential to metabolize anthropogenic compounds. In this work, a simple, precise and accurate static headspace gas chromatography method was developed to investigate the ability of TBT degrading microbes in sedimentary microcosms over a period of 120 days. The proposed method was validated for linearity, repeatability, accuracy, specificity, limit of detection and limit of quantification. The method was subsequently successfully applied for the detection and quantification of TBT and degrading compounds in sediment samples on day 0, 30, 60, 90 and 120 of the experiment employing the principles of green chemistry. On day 120 the concentration of TBT remaining in the microcosms ranged between 91.91 ng/g wet wt for the least effective microbial inoculant to 52.73 ng/g wet wt for the most effective microbial inoculant from a stating concentration of 100 ng/g wet wt.

After screening nearly 1000 synthetic peptides, a synthetic peptide termed JAL-AK22 (KYEGHWYPEKPYKGSGFRCIHI) derived from the BoxA domain in Tob1 protein was found to activate both unfolded and folded proMMP-7. In addition, JAL-AK22 showed auto-proteolytic activity. Interestingly, the smaller derivative of JAL-AK22 termed JAL-TA9 (YKGSGFRMI) also possessed auto-proteolytic activity and cleaved 2 fragment peptides (MMP18-33 and MMP18-40) derived from the prodomain of proMMP-7 under physiological conditions. These proteolytic activities were inhibited by AEBSF, a serine protease inhibitor. Our results demonstrate that a small synthetic peptide consisting of only 9 amino acids has serine protease-like activity and activates proMMP-7 by cleaving the prodomain region. We thus propose calling small peptides possessing with protease-like activity Catalytides (catalytic peptides). We expect that our findings will stimulate the development of novel Catalytides and related applications.

Polydiacetylene (PDA) inserted in films or in vesicles have received increasing attention due to PDA property to undergo a blue-to-red colorimetric transition along with a change from non-fluorescent to fluorescent upon application of various stimuli. In this review paper, the principle of the detection of various microorganisms (bacteria: directly detected or detected through the emitted toxins or through their DNA, and viruses) and of antibacterial and antiviral peptides based on these responsive PDA vesicles are detailed. The obtained analytical performances, when vesicles are in suspension or immobilized, are given and compared to those of the responsive vesicles mainly based on the vesicle encapsulation method. Many future challenges are then discussed.

After screening nearly 1000 synthetic peptides, a synthetic peptide termed JAL-AK22 (KYEGHWYPEKPYKGSGFRCIHI) derived from the BoxA domain in Tob1 protein was found to activate both unfolded and folded proMMP-7. In addition, JAL-AK22 showed auto-proteolytic activity. Interestingly, the smaller derivative of JAL-AK22 termed JAL-TA9 (YKGSGFRMI) also possessed auto-proteolytic activity and cleaved 2 fragment peptides (MMP18-33 and MMP18-40) derived from the prodomain of proMMP-7 under physiological conditions. These proteolytic activities were inhibited by AEBSF, a serine protease inhibitor. Our results demonstrate that a small synthetic peptide consisting of only 9 amino acids has serine protease-like activity and activates proMMP-7 by cleaving the prodomain region. We thus propose calling small peptides possessing with protease-like activity Catalytides (catalytic peptides). We expect that our findings will stimulate the development of novel Catalytides and related applications.

In this study, the optimal condition for the extraction of antioxidants from the fruit Buah Mahkota Dewa (Phaleria macrocarpa) was determined by using Response Surface Methodology (RSM). The optimization was applied using central composite design (CCD) to investigate the three independent variables, namely extraction temperature (^oC), extraction time (minutes) and extraction solvent to-feed ratio (%v/v) on the responses of free radical scavenging activity (DPPH), ferric ion reducing power assay (FRAP), total phenolic content (TPC) and total flavonoid content (TFC).The optimal conditions for the antioxidants extraction were found to be extraction temperature (64^oC), extraction time (66 minutes) and solvent to-feed ratio (75 %v/v) with the highest percentage yield of DPPH, FRAP, TPC and TFC were 86.85%, 7.47%, 292.86 mg/g and 3.22 mg/g respectively. Moreover, the data were subjected to response surface methodology (RSM) and the results showed that the polynomial equations for all models were significant, did not show lack of fit, and presented adjusted determination coefficients (R²) above 99%, proving the yield of phenolic, flavonoid and antioxidants activities obtained experimentally were close to the predicted values and the suitability of the model employed in RSM to optimize the extraction conditions. Hence, in this study, the fruit from P.macrocarpa could be considered to have the strong antioxidant ability and can be used in various cosmeceutical or medicinal applications.

A multi-tool analytical practice was used for characterization of 16^th century carpet manufactured in Cairo. Mild extraction method with hydrofluoric acid enabled isolation of intact flavonoids and their glycosides, anthraquinones, tannins and indigoids from fibre samples. High-performance liquid chromatography coupled to spectroscopic and mass spectrometric detectors was used for identification of natural dyes present in the historical samples. Weld, young fustic and brazilwood were identified as the dye sources in yellow thread samples. Red fibres have been colored with lac dye, whereas green fibre shades were obtained with indigo and weld. Tannin-containing plant material in combination with indigo and weld were used to obtain brown hue of thread. Four uncommon and thus-far unknown dye components were also found in the historical samples. These compounds probably represent unique fingerprint of dyed threads from this region. Scanning electron microscopy with energy-dispersive X-ray detector (SEM-EDS) and Fourier transformation infrared spectroscopy (FT-IR) were used for identification and characterization of substrates and mordants present in the historical carpet. Carbon and oxygen were detected in large quantities as a part of the wool protein. The presence of aluminum, iron and calcium indicated their usage as mordants. FT-IR analysis showed bands characteristic to woolen fibres and SEM micrographs definite structure of wool.

Food pathogens contaminate food products that allow their growth on the shelf and also under refrigerated conditions. Therefore, it is of utmost importance to lower the limit of detection (LOD) of the method used and to obtain the results within hours to few days. Biosensor methods exploit the available technologies to individuate and provide an approximate quantification of the bacteria present in a sample. The main bottleneck of these methods depend on the aspecific binding to the surfaces and on a change in sensitivity when bacteria are in a complex food matrix in respect to bacteria in a liquid food sample. In this review we introduce Surface Plasmon Resonance (SPR), new advancements in SPR techniques, and Electrochemical Impedance Spectroscopy (EIS), as label-free biosensing technologies for the detection of L. monocytogenes in foods. The application of the two methods has made possible the detection of L. monocytogenes with LOD of 1 log CFU/mL. Further advancement are envisaged through the combination of biosensor methods with immunoseparation of bacteria from larger volumes.

A simple method for the determination of caffeine in coffee grains by GC-FID is presented in the current work. The method was fully validated according to ISO 17025 requirements and European Commission regulation. The accuracy, as provided by recovery experiments was higher than 93%, and the precision, as provided by the (%)Relative standard deviation under reproducibility conditions, was lower than 5%. All independent parameters that lead in the increase of methods uncertainty were investigated. In the present work all special precautions were taken into account in order to avoid the use of an internal standard. The method was applied in real samples and possible health claims were investigated.

Carbon nanotubes (CNTs) possess unique mechanical, physical, electrical and absorbability properties coupled with their nanometer dimensional scale that renders them extremely valuable for applications in many fields including nanotechnology and chromatographic separation. The aim of this review is to provide an updated overview about the applications of CNTs in chiral and achiral separations of pharmaceuticals, biologics and chemicals. Chiral SWCNTs and MWCNTs have been directly applied for the enantioseparation of pharmaceuticals and biologicals by using them as stationary or pseudostationary phases in chromatographic separation techniques such as high-performance liquid chromatography (HPLC), capillary electrophoresis (CE) and gas chromatography (GC). Achiral MWCNTs have been used for achiral separations as efficient sorbent objects in solid-phase extraction techniques of biochemicals and drugs. Achiral SWCNTs have been applied in achiral separation of biological samples. Achiral SWCNTs and MWCNTs have been also successfully used to separate achiral mixtures of pharmaceuticals and chemicals. Collectively, functionalized CNTs have been indirectly applied in separation science by enhancing the enantioseparation of different chiral selectors whereas, non-functionalized CNTs have shown efficient capabilities for chiral separations by using techniques such as encapsulation or immobilization in polymer monolithic columns.

The theory and working principle of fabric phase sorptive extraction (FPSE) is presented that eloquently explains the mystery behind this new and powerful sample preparation technique. FPSE innovatively integrates the benefits of sol-gel coating technology and the rich surface chemistry of cellulose/polyester/fiberglass fabric, resulting in a microextraction device with very high sorbent loading in the form of an ultra-thin coating. This porous sorbent coating and the permeable substrate synergistically facilitate very fast extraction equilibrium. The flexibility of the FPSE device allows for direct insertion into original, unmodified samples of different origin. Strong chemical bonding between the sol-gel sorbent and the fabric substrate permits the exposure of FPSE devices to any organic solvent for analyte back-extraction/elution and to highly acidic or basic environments (pH 1-12) if required. A sol-gel derived sorbent, highly polar sol-gel poly(ethylene glycol) coating, was generated on cellulose substrates. Five cm2 segments of these coated fabrics were used as the FPSE devices for sample preparation using direct immersion. An important class of environmental pollutants, substituted phenols, was used as model compounds to evaluate the extraction performance of FPSE. The high primary contact surface area (PCSA) of the FPSE device and porous structure of the sol-gel coatings resulted in very high sample capacities and incredible extraction sensitivities for both the compound classes in a relatively short period of time. Different extraction parameters were evaluated and optimized. The new extraction devices demonstrated part per trillion level detection limits for substituted phenols, a wide range of detection linearity, and good performance reproducibility.

A novel catechol (CA) biosensor was developed by the immobilization of tyrosinase (Tyr) onto in situ electrochemical reduction graphene (EGR) on choline functionalized gold nanoparticals (AuNPs–Ch) film. The results of UV–visible spectra indicated that Tyr retained its original structure in the film. And electrochemical investigation of the biosensor showed a pair of well–defined, quasi–reversible redox peaks with E_pa= –0.0744V and E_pc= –0.114 V (vs. SCE) in 0.1 M, pH 7.0 sodium phosphate buffered saline at the scan rate of 100 mV/s. The transfer rate constant k_s was 0.66 s^–1. The Tyr–EGR/AuNPs–Ch showed a good electrochemical catalytic response for the reduction of CA, with the linear range from 0.2 to 270 μM and a detection limit of 0.1 μM (S/N= 3). The apparent Michaelis–Menten constant was estimated to be 109 μM.

Fabric phase sorptive extraction (FPSE) combines the advanced material properties of sol–gel derived microextraction sorbents and the flexible and permeable fabric support to create a robust, simple and green sample preparation device. It simultaneously improves the extraction sensitivity, and the speed of the extraction by incorporating high volume of sponge-like porous sol–gel hybrid inorganic–organic sorbents into permeable fabric substrates that is capable of extracting target analytes directly from simple to complex aqueous sample matrices. For the first time, this technique was applied to the trace level determination of selected polycyclic aromatic hydrocarbons (PAHs) in environmental water samples using a non-polar sol–gel C18 coated FPSE media. Several extraction parameters were optimized to improve extraction efficiency and to achieve high detection sensitivity. Validation tests of spiked samples showed good linearity for four selected PAHs (R² = 0.9983–0.9997) over a wide range of concentrations (0.010-10 ng/mL). Limits of detection (LODs) and quantification (LOQs) were measured at pg/mL levels, 0.1–1 pg/mL and 0.3–3 pg/mL, respectively. Inter- and intra-day precision tests showed variations of 1.1–4.1% for four selected PAHs. Average absolute recovery values were in the range of 88.1–90.5% surpassed the recovery prediction model, with relative standard deviations below 5%. The developed FPSE-HPLC-FLD protocol was finally applied to analyze 8 environmental water samples. Out of four selected PAHs, fluoranthene (Flu) and phenanthrene (Phen) were the most frequently detected in four samples, at concentration levels of 5.6–7.7 ng/mL and 4.1-11 ng/mL, respectively followed by anthracene (Anth) and pyrene (Pyr) in two samples. The newly developed FPSE-HPLC-FLD protocol is simple, green, fast and economical, with adequate sensitivity for trace levels of four selected PAHs and seems to be promising in routine monitoring of water quality and safety.

Metabolomic analysis of biological fluids and tissues has become an increasingly routine tool in the biological toolbox. However, challenges remain to be overcome, including developing strategies to maximise coverage of the metabolome without requiring large sample volumes. Here we describe a multimodal strategy that combines data using both LC-MS and GC-MS from a unique vial with a sample of plasma (20µl) or a sample of brain tissue (3mg). Using a split phase extraction the non-aqueous phase was analyzed by reversed phase (RP) LC-MS, whilst the aqueous phase was analyzed using hydrophilic liquid interaction chromatography (HILIC)LC-MS, with both phases also analysed using GC-MS after derivatization of the extract. Analytical performance was assessed in 7 rat cerebellum samples and a pilot study of 40 plasma samples (20 vs. 20: AD vs. healthy controls). The method, which uses four hours of instrument time, measured 20,707 metabolite features in brain samples and 17,266 in plasma samples, from those 44.1% features displayed CV’s below 15% and 75.2% below 30%. The method has potential to resolve subtle biological differences and to correlate metabolite composition directly to clinical outcomes including MMSE, age and ADCS-ADL. This method can acquire in the order of 20K metabolic features when low volumes are available.

Fabric phase sorptive extraction (FPSE) combines the advanced material properties of sol–gel derived microextraction sorbents and the flexible and permeable fabric support to create a robust, simple and green sample preparation device. It simultaneously improves the extraction sensitivity, and the speed of the extraction by incorporating high volume of sponge-like porous sol–gel hybrid inorganic–organic sorbents into permeable fabric substrates that is capable of extracting target analytes directly from simple to complex aqueous sample matrices. For the first time, this technique was applied to the trace level determination of selected polycyclic aromatic hydrocarbons (PAHs) in environmental water samples using a non-polar sol–gel C18 coated FPSE media. Several extraction parameters were optimized to improve extraction efficiency and to achieve high detection sensitivity. Validation tests of spiked samples showed good linearity for four selected PAHs (R² = 0.9983–0.9997) over a wide range of concentrations (0.010-10 ng/mL). Limits of detection (LODs) and quantification (LOQs) were measured at pg/mL levels, 0.1–1 pg/mL and 0.3–3 pg/mL, respectively. Inter- and intra-day precision tests showed variations of 1.1–4.1% for four selected PAHs. Average absolute recovery values were in the range of 88.1–90.5% surpassed the recovery prediction model, with relative standard deviations below 5%. The developed FPSE-HPLC-FLD protocol was finally applied to analyze 8 environmental water samples. Out of four selected PAHs, fluoranthene (Flu) and phenanthrene (Phen) were the most frequently detected in four samples, at concentration levels of 5.6–7.7 ng/mL and 4.1-11 ng/mL, respectively followed by anthracene (Anth) and pyrene (Pyr) in two samples. The newly developed FPSE-HPLC-FLD protocol is simple, green, fast and economical, with adequate sensitivity for trace levels of four selected PAHs and seems to be promising in routine monitoring of water quality and safety.

The theory and working principle of fabric phase sorptive extraction (FPSE) is presented that eloquently explains the mystery behind this new and powerful sample preparation technique. FPSE innovatively integrates the benefits of sol-gel coating technology and the rich surface chemistry of cellulose/polyester/fiberglass fabric, resulting in a microextraction device with very high sorbent loading in the form of an ultra-thin coating. This porous sorbent coating and the permeable substrate synergistically facilitate very fast extraction equilibrium. The flexibility of the FPSE device allows for direct insertion into original, unmodified samples of different origin. Strong chemical bonding between the sol-gel sorbent and the fabric substrate permits the exposure of FPSE devices to any organic solvent for analyte back-extraction/elution and to highly acidic or basic environments (pH 1-12) if required. A sol-gel derived sorbent, highly polar sol-gel poly(ethylene glycol) coating, was generated on cellulose substrates. Five cm2 segments of these coated fabrics were used as the FPSE devices for sample preparation using direct immersion. An important class of environmental pollutants, substituted phenols, was used as model compounds to evaluate the extraction performance of FPSE. The high primary contact surface area (PCSA) of the FPSE device and porous structure of the sol-gel coatings resulted in very high sample capacities and incredible extraction sensitivities for both the compound classes in a relatively short period of time. Different extraction parameters were evaluated and optimized. The new extraction devices demonstrated part per trillion level detection limits for substitute phenols, a wide range of detection linearity, and good performance reproducibility.

A simple, isocratic and robust RP-HPLC method for the analysis of azithromycin was developed, validated and applied for the analysis of bulk samples, tablets and suspensions. The optimum chromatographic conditions for separation were established as mobile phase comprising of acetonitrile-0.1M KH₂PO₄ pH 6.5-0.1M tetrabutyl ammonium hydroxide pH 6.5-water (25:15:1:59% v/v/v/v) delivered at a flow rate of 1.0 ml/min. The stationary phase consisted of reverse-phase XTerra^® (250 mm× 4.6 mm i.d., 5 µm particle size) maintained at a temperature of 43 °C with a UV detection at 215 nm. The method was found to be linear in the range 50-150% (r²=0.997). The limits of detection and quantification were found to be 0.02% (20 µg) and 0.078% (78 µg) respectively with a 100.7% recovery of azithromycin. Degradation products of azithromycin in acidic and oxidative environments at 37 °C were resolved from the active pharmaceutical ingredient and thus the method is fit for the purpose of drug stability confirmation.

A simple, isocratic and robust RP-HPLC method for the analysis of azithromycin was developed, validated and applied for the analysis of bulk samples, tablets and suspensions. The optimum chromatographic conditions for separation were established as mobile phase comprising of acetonitrile-0.1M KH₂PO₄ pH 6.5-0.1M tetrabutyl ammonium hydroxide pH 6.5-water (25:15:1:59% v/v/v/v) delivered at a flow rate of 1.0 ml/min. The stationary phase consisted of reverse-phase XTerra^® (250 mm× 4.6 mm i.d., 5 µm particle size) maintained at a temperature of 43 °C with a UV detection at 215 nm. The method was found to be linear in the range 50-150% (r²=0.997). The limits of detection and quantification were found to be 0.02% (20 µg) and 0.078% (78 µg) respectively with a 100.7% recovery of azithromycin. Degradation products of azithromycin in acidic and oxidative environments at 37 °C were resolved from the active pharmaceutical ingredient and thus the method is fit for the purpose.

A method based on ultra performance liquid chromatography with diode array detector (UPLC-DAD) was developed for quantitative analysis of five active compounds and chemical fingerprint analysis of Rosa rugosa. Ten batches of Rosa rugosa collected from different plantations in the Xinjiang region of China were used to establish the fingerprint. The feasibility and advantages of the used UPLC fingerprint were verified for its similarity evaluation by systematically comparing chromatograms with professional analytical software recommended by State Food and Drug Administration (SFDA) of China. In quantitative analysis, the five compounds showed good regression (R²=0.999 5) within the test ranges and the recovery of the method was in the range of 94.2–103.8%. The similarities of the fingerprints of 10 batches of the samples were more than 0.981. The developed UPLC fingerprint method is simple, reliable and validated for the quality control and identification of Rosa rugosa. Additionally, simultaneous quantification of five major bioactive ingredients in the Rosa rugosa samples was conducted to interpret the consistency of the quality test. The results indicated that the UPLC fingerprint as a characteristic distinguishing method combining similarity evaluation and quantification analysis, can be successfully used to assess the quality and to identify the authenticity of Rosa rugosa.

A novel determination method using flow-through cartridge purification and ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) was developed for the identification and quantification of 30 mycotoxins (aflatoxin B1, B2, G1, G2, sterigmatocysin, T-2 toxin, diacetoxyscirpenol, roquefortine C, methylergonovine, ergocornine, lysergol, enniatin A, enniatin A1, enniatin B, enniatin B1, beauvericin, deoxynivalenol, 3-acetylDeoxynivalenol, 15-acetylDeoxynivalenol, patulin, verruculogen, neosolaniol, gliotoxin, HT-2 toxin, wortmannin, zearalenone, α-zearalenol, β-zearalenol, α-zearalanol, and β-zearalanol) in feedstuffs. Mycotoxins were extracted from sample by 0.1% formic acid aqueous solution/acetonitrile (16/84 v/v), then purified by a Cleanert® MC clean-up column. As a result, the pigments and other matrices were efficient removed from the sample extract solution. The purified eluate was collected, then evaporated and redissolved by 0.1% formic acid aqueous solution/acetonitrile (70:30 v/v) for UPLC-MS/MS detection. A BEH Shield RP18 chromatographic column was employed for separation of 30 mycotoxins in a total of 14 min. Multiple-reaction monitoring (MRM) mode was applied for qualitative and quantitative analysis, and matrix calibration curves obtained with the external-standard method was used for quantitation of target analytes. Under optimized conditions, the linearity range was from 2 to 1000 ng/g, and the limit of quantification of the developed method was from 2 to 50 ng/g. The recoveries of 30 mycotoxins spiked in urine samples were from 72.0% to 118.5%, and the relative standard deviation was below 20%. The method was also well approved by certified reference sample, and applied on the real feedstuff samples testing successfully.