Unrecorded alcohol comprises all types of alcohol that is not registered in the jurisdiction where it is consumed. In some countries in Central and Eastern parts of Europe as well as the Balkan, the major amount of unrecorded alcohol consumption may derive from homeproduction of fruit spirits. Some studies found a high prevalence of lead and cadmium in such spirits. This article provides a quantitative comparative risk assessment using the margin of exposure (MOE) methodology for lead and cadmium, compared to ethanol, for unrecorded fruit spirits. For average concentration levels, the lowest MOE (0.8) was calculated for ethanol (alcohol itself). For lead, the MOE was 13 for moderate daily drinking and 0.9 for the worst case. For cadmium, the MOE was 1982 for moderate daily drinking and 113 for the worst case. The results of this study are consistent with previous comparative risk assessments that ethanol itself comprises by far the highest risk of all compounds in alcoholic beverages. Regarding the metal contaminants, the risk of cadmium appears negligible, however, lead may pose an additional health risk in heavy drinking circumstances. Strategies to avoid metal contamination in settings of artisanal homeproduction of spirits need to be developed.

The study reports about a case of a lung cancer patient with increasing difficulties in falling asleep and frequent periods of wakefulness. Severe dyspnea related to pneumonitis caused as a side effect of immunotherapy worsened the situation. Eventually, fear of falling asleep developed, including panic attacks and anxiety of choking, which was shown to lead to nights of complete wakefulness. The patient did not only sleep poorly; he did not sleep at all at night for several days, as evidenced by the notes he made during the night. Polygraphy showed no evidence of sleep-disordered breathing, but frequent periods of wakefulness and reduced basal saturation around 90% during sleep due to lung changes such as extensive functional failure of the left upper lobe with position-dependent shunts. The authors hypothesized that the symptoms described were causally related to a drop in oxygen saturation in the patient's blood. Therefore, they pursued the goal of finding a measurement technique that is as inexpensive as possible and that the patient can operate without outside assistance and great effort. So the patient started using a low-cost wearable device that allows simultaneous measurements of blood oxygen content, pulse rate and movement intensity. It consists of a finger ring with pulse oximetry sensor and a wristband with the control unit containing a vibration motor. The described device reliably warned of disturbances in oxygen concentration in the blood during the night with its vibration alarm. By use of that device during the whole night at home, the events of reduced oxygen saturation and the anxiety symptoms were reduced. Sleep disturbances with sudden awakenings did not occur when using the device. The patient benefited from the security gained in this way and slept much more peacefully, and he could spend nights without waking up again. In conclusion, wearable oximeters with vibration alarm can be recommended for patients’ home care in lung cancer patients.

Epidemiological studies indicate an increased risk of cancer from the consumption of very hot foods and beverages. The International Agency for Research on Cancer (IARC) has already recommended threshold values for the maximum drinking temperature of very hot beverages. The contact time and the contact temperature are decisive for the risk of injury when hot media come into contact with human skin. However, measuring the contact temperature is not easily possible in practice. In the present study, a numerical simulation based on the solution of the heat conduction equation was initially used to investigate whether and for what period of time a constant contact temperature is to be expected under oral conditions. For small circular 3-cm food samples (e.g., cooked potatoes) with 2.5 mm thickness in contact with the tongue, the simulation results in a constant contact temperature of 10 s before cooling. With a thickness of 0.5 mm, the contact temperature is only maintained 1 s. Hot beverages, which spread as a thin film and thereby increase their surface area, can therefore be consumed at higher temperatures than solid foods. Furthermore, a simple test technique with a "measuring spoon" was developed. A hot sample is placed on the tongue. Orientating measurements were used to determine which contact temperature was considered to be just comfortable for any period > 10 s and for which period of less than 10 s it was still just bearable. The contact temperature, which was still perceived as tolerable for periods > 10 s, was 46.5 °C. The time spans for the higher contact temperature 48 °C were between 2 and 4 s and for 49 °C between 1 and 2 s. The course of the contact temperatures determined in the experiment over time allows to calculate the corresponding threshold values of consumption temperatures for various foods. Consumption temperatures of about 56 °C for potatoes and 60 °C for cheese are still perceived as tolerable. In view of the fact that the contact temperature is obviously the determining factor for the risk of injury from burns in the oral cavity in addition to the contact time, it makes sense to reference threshold values to the contact temperature rather than to the surface or consumption temperature of a food product, which is current customary practice. If this contact temperature is defined as a threshold value, the surface or consumption temperature for any other food can be calculated.

The International Agency for Research on Cancer (IARC) evaluates “very hot (>65 °C) beverages” as probably carcinogenic to humans. However, there is a lack of research regarding what temperatures consumers actually perceive as “very hot” or as “too hot”. A methodology for organoleptical assessment of such threshold temperatures was developed. The participants were asked to mix a very hot coffee step by step into a cooler coffee. Because of that, the coffee to be tasted was incrementally getting hotter during the test. The participants took a sip at every addition, until they perceive the beverage as too hot for consumption. The protocol was evaluated using 87 participants. Interestingly, the average pain threshold of the test group (67 °C) and the preferred drinking temperature (63 °C) iterated around the IARC threshold for carcinogenicity. The developed methodology was found as fit for the purpose and may be applied in larger studies.

Very hot (> 65 °C) beverages such as espresso were evaluated by the International Agency for Research on Cancer (IARC) as probably carcinogenic to humans. For this reason, research into lowering beverage temperature without compromising its quality or taste is important. For espresso, one obvious possibility consists in lowering the brewing temperature. In two sensory trials using ISO 4120:2004 triangle test methodology, brewing temperatures of 80°C vs. 128°C and 80° vs. 93°C were compared. From the tested levels, espresso brewed at the lowest temperature had the highest acceptance. However, most tasters were unable to distinguish between 80°C and 93°C. The results of these pilot experiments proof the possibility to decrease the health hazard of very hot beverages by lower brewing temperatures.

In the European Union (EU), cannabidiol products require pre-marketing authorisation under the novel food regulation. Currently, 19 CBD applications are under assessment at the European Food Safety Authority (EFSA). During the initial assessment of the application files, the EFSA Panel on Nutrition, Novel Foods and Food Allergens (NDA) located several knowledge gaps in their 07 June 2022 statement on safety of cannabidiol as a novel food that need to be addressed before the evaluation of CBD can be concluded. Namely, the effect of CBD on the liver, gastrointestinal tract, endocrine system, nervous system, psychological function, and reproductive system needs to be clarified. Nevertheless, the available literature allows a benchmark dose (BMD)-response modelling of several bioassays, resulting in a BMD lower confidence limit (BMDL) of 20 mg/kg bw/day for liver toxicity in rats. Human data in healthy volunteers found increases in the liver enzymes alanine aminotransferase (ALT) and aspartate aminotransferase (AST) in a study at 4.3 mg/kg bw/day, which was defined by EFSA NDA panel as a lowest observed adverse effect level (LOAEL). The EFSA NDA panel currently concluded that the safety of CBD as a novel food cannot be evaluated, leading to a so-called clock stop of the applications until the applicants provide the required data. Meanwhile, the authors suggest that CBD products still available as food supplements on the EU market despite the lack of authorisation must be considered as “unsafe”. Products exceeding a health-based guidance value of 10 mg/day must be considered as being “unfit for consumption” (Article 14(1) and (2) (b) of Regulation No 178/2002), while the ones in exceedance of the human LOAEL must be considered “injurious to health” (Article 14(1) and (2) (a) of Regulation No 178/2002).

Cheap licit and artisanal illicit spirit drinks have been associated with numerous outbreaks of alcohol poisoning especially with methanol. This study aimed to evaluate the quality of cheap spirit drinks in Kibera slums in Nairobi County, Kenya. The samples consisted of cheap licit spirits (n=11) and the artisanal spirit drink, ‘chang’aa’, (n=28). The parameters of alcoholic strength and volatile composition were used as indicators of quality and were determined using GC-FID and GC-MS respectively. The pH of chang’aa was 3.3-4.2 and 4.4-8.8 for licit spirit drinks while ranges for alcoholic strength were 42.8-85.8 % vol. and 28.3-56.7% vol. for chang’aa and licit spirit drinks respectively. The majority of volatiles were found in artisanal spirits and they included higher alcohols, ethyl esters and carbonyl compounds. The alcoholic strength of all the artisanal spirits (100%) and 91% of the licit spirits was above the 40% vol. of standard spirits such as vodka. The high ethanol content of the alcohol products was the only element of public health significance in this study.

Toxicologically relevant levels of the psychoactive ∆9-tetrahydocannabinol (∆9-THC) as well as high levels of non-psychoactive cannabinoids potentially occur in CBD (cannabidiol) oils. For consumer protection in the fast-growing CBD oil market, facile and rapid quantitative methods to determine the cannabinoid content are crucial. However, the current standard method, i.e., liquid chromatography combined with tandem mass spectrometry (HPLC-MS/MS), requires a time-consuming multistep sample preparation. In this study, a quantitative nuclear magnetic resonance spectroscopy (qNMR) method for screening cannabinoids in CBD oils was developed. Contrary to the HPLC-MS/MS method, this qNMR features a facile sample preparation, i.e., only diluting the CBD oil in deuterochloroform. Pulse length-based concentration determination (PULCON) enables a direct quantification using an external standard. The signal intensities of the cannabinoids were enhanced during the NMR spectra acquisition by means of multiple suppression of the triglycerides which are a major component of the CBD oil matrix. The validation confirmed linearity for CBD, cannabinol (CBN), ∆9-THC and ∆8-THC in hemp seed oil with sufficient recoveries and precision for screening. Comparing the qNMR results to HPLC-MS/MS data for 46 commercial CBD oils verified the qNMR accuracy for ∆9-THC and CBD but with higher limits of detection. The developed qNMR method paves the way for increasing the sample throughput as a complementary screening before HPLC-MS/MS.

Cold brew coffee has emerged as a new trend during the last decade. However, “cold brew” is an extraction style of ground roasted coffee with water at less than body temperature (typically 8°C or room temperature) rather than a beverage per se. Cold brew extraction poses several challenges including the need of specific optimization depending on the multivariate influences of coffee variety and processing, roast degree, grinding, dosage, water composition, turbulence, brew system (drip, immersion etc.), time and temperature. While cold brew is typically characterized by a floral sweetness, over-extraction may lead to abundant acidity and bitterness. To avoid this, an extraction degree of 70% was suggested using rather shorter times (i.e. 2 h at 15°C with 80 g/L coffee with optimized medium roast profiles). Due to the lack of sterilizing temperatures during preparation, cold brew is special in the coffee sector because hygiene and food safety aspects pose specific challenges for food industry. To avoid microbiological contamination and spoilage, cold brew should be as freshly prepared as possible and shelf-life should be minimized.

Highly reactive decomposition products of (deuterated) chloroform can deteriorate samples dissolved in this commonly used NMR solvent. For sensitive samples (such as peptides, unsaturated fatty acids, vitamins), this can lead to abnormal NMR spectra (e.g. signal shifts depending on pH, attenuation of signals over time due to chemical changes of analytes, new signals from reaction products). Such irreproducibly influenced spectra are especially problematic for non-targeted analysis methods. To prevent these artefacts, chlorine, phosgene and hydrochloric acid need to be eliminated from deuterated chloroform prior to its use. Since the common stabilization methods have proven insufficient for sensitive NMR samples, another purging method has been tested: Mitigation is easily and reliably achieved by washing the deuterated chloroform with concentrated Na2CO3-solution and subsequent desiccation with oven-dried Na2CO3.

For decades, compounds present in foods and beverages have been implicated in the etiology of human cancers. The International Agency for Research on Cancer (IARC) continues to classify such agents regarding their potential carcinogenicity in humans based on new evidence from animal and human studies. Furfuryl alcohol and β-myrcene belong to these potential human carcinogens due to be evaluated. The major source of furfuryl alcohol in foods is thermal processing and ageing of alcoholic beverages while β-myrcene occurs naturally as a constituent of essential oils of plants such as hops, lemongrass and derived products. This study aimed to summarize the occurrence of furfuryl alcohol and β-myrcene in foods and beverages using data from own nuclear magnetic resonance (NMR) analysis and literature review. The highest content of furfuryl alcohol was found in coffee beans (>100 mg/kg) and in some fish products (about 10 mg/kg) while among beverages, wines contained between 1–10 mg/L with 8 mg/L in pineapple juice. The content of β-myrcene was highest in hops. In conclusion, the data about the occurrence of the two agents is either very old or based on single sample analysis, and currently judged as insufficient for exposure and risk assessment. The results of this study point out the food and beverage groups that may be considered for future monitoring of furfuryl alcohol and β-myrcene.

The three heat-induced coffee contaminants acrylamide, furfuryl alcohol (FA) and 5-hydroxymethylfurfural (HMF) were analyzed in a collective of commercial samples as well as in Coffea arabica seeds roasted under controlled conditions from very light Scandinavian style to very dark Neapolitan style profiles. Regarding acrylamide, average contents in commercial samples were lower than in a previous study in 2002 (196 compared to 303 µg/kg). The roasting experiment confirmed the inverse relationship between roasting degree and acrylamide content, i.e. the lighter the coffee the higher the acrylamide content. However, FA and HMF were inversely related to acrylamide and found in higher contents in darker roasts. Therefore, mitigation measures must consider all contaminants and not be focused isolatedly on acrylamide, specifically since FA and HMF are contained in much higher contents with lower margins of exposure compared to acrylamide.

The food additive sorbic acid is considered as an effective preservative for certain cereal products, and propionic acid is commonly added in bakery wares, e.g. bread and fine bakery wares. The aim of this study is to develop and validate a new nuclear magnetic resonance spectroscopy (¹H NMR) method for routine screening and quantification of sorbic and propionic acids in bread and several bakery products for quality control purposes. Results showed that none of the screened samples contained higher concentrations than regulatory maximum limits. However, for some samples, labelling of preservatives was lacking or they were used in food categories, for which the use is not approved. It can be concluded that the developed NMR method can be used for routine screening of bakery products.

Due to legal regulations, the rise of globalised (online) commerce and the need for public health protection, the analysis of spirits (alcoholic beverages > 15 % vol) is a task with growing importance for governmental and commercial laboratories. In this article a newly developed method using nuclear magnetic resonance (NMR) spectroscopy for the simultaneous determination of 15 substances relevant for the quality and authenticity assessment of spirits is described. The new method starts with a simple and rapid sample preparation and does not need an internal standard. For each sample a group of 1H-NMR spectra is recorded, among them a 2D spectrum for analyte identification and 1D spectra with suppression of solvent signals for quantification. Using the Pulse Length Based Concentration Determination (PULCON) method, concentrations are calculated from curve fits of the characteristic signals for each analyte. The optimisation of the spectra, their evaluation and the transfer of the results are done fully automatically. Glucose, fructose, sucrose, acetic acid, citric acid, formic acid, ethyl acetate, ethyl lactate, acetaldehyde, ethanol, methanol, n-propanol, isobutanol, isopentanol, 2-phenylethanol and 5-(hydroxymethyl)furfural (HMF) can be quantified with an overall accuracy better than 8 %. This new NMR-based targeted quantification method enables the simultaneous and efficient quantification of relevant spirits ingredients in their typical concentration ranges in one process with good accuracy. It has proven to be a reliable method for all kinds of spirits in routine food control.

Monitoring coffee quality as a means of detecting and preventing economically motivated fraud is an important aspect of international commerce today. Therefore, there is a compelling need for rapid high throughput validated analytical techniques such as quantitative proton NMR spectroscopy for screening and authenticity testing. For this reason, we sought to validate an NMR spectroscopic method for routine screening of coffee for quality and authenticity. A factorial experimental design was used to investigate the influence of NMR device, extraction time and nature of coffee on the content of caffeine, 16-O-methylcafestol (OMC), kahweol, furfuryl alcohol and 5-hydroxymethylfurfural (HMF) in coffee. The method was successfully validated for specificity, selectivity, sensitivity and linearity of detector response. The proposed method produced satisfactory precision for all analytes in roasted coffee, except for kahweol in canephora (robusta) coffee. The proposed validated method may be used for routine screening of roasted coffee for quality and authenticity control, as its applicability was demonstrated during the recent OPSON VIII Europol-Interpol operation on coffee fraud control.

This study aimed to investigate the occurrence of the artificial sweetener aspartame (E951) in a wide range of foods and beverages sampled by food control authorities in Germany between 2000 and 2022. The dataset was obtained through the Consumer Information Act. The results showed that aspartame was present in a wide range of product groups tested, most commonly in powdered drink bases (84%) and flavored milk drinks (78%). In the solid food groups, the highest mean aspartame content was found in chewing gum (1543 mg/kg, n=241), followed by sports foods (1453 mg/kg, n=125), fiber supplements (1248 mg/kg, n=11), powdered drink bases (1068 mg/kg, n=162), and candies (437 mg/kg, n=339). Liquid products generally had the highest aspartame content in diet soft drinks (91 mg/l, n=2021), followed by regular soft drinks (59 mg/l, n= 574), flavored milk drinks (48 mg/kg, n=207), and mixed beer drinks (24 mg/l, n=40). These results suggest that aspartame is widely used in foods and beverages in Germany and that certain product groups contain higher concentrations of the sweetener than others. However, the levels of aspartame found were generally within the legal limits set by the European Union. These findings provide the first comprehensive overview of aspartame in the German food market and may be particularly useful in informing the forthcoming working groups of the WHO International Agency for Research on Cancer (IARC) and the WHO/FAO Joint Expert Committee on Food Additives (JECFA), which are in the process of evaluating the human health hazards and risks associated with the consumption of aspartame.

Methanol is a natural ingredient with major occurrence in fruit spirits, such as apple, pear, plum or cherry spirits, but also in spirits made from coffee pulp. The compound is formed during fermentation and the following mash storage by enzymatic hydrolysis of naturally present pectins. Methanol is toxic above certain threshold levels and legal limits have been set in most jurisdictions. Therefore, the methanol content needs to be mitigated and its level must be controlled. This article will review the several factors that influence the methanol content including the pH value of the mash, the addition of various yeast and enzyme preparations, fermentation temperature, mash storage, and most importantly the raw material quality and hygiene. From all these mitigation possibilities, lowering the pH value and the use of cultured yeasts when mashing fruit substances is already common as best practice today. Also a controlled yeast fermentation at acidic pH facilitates not only reduced methanol formation, but ultimately also leads to quality benefits of the distillate. Special care has to be observed in the case of spirits made from coffee by-products which are prone to spoilage with very high methanol contents reported in past studies.

Coffee pulp, obtained from wet coffee processing, is the major by-product accumulating in the coffee producing countries. One of the many approaches valorising this underestimated agricultural residue is the production of distillates. This research project deals with the production of spirits from coffee pulp using three different Coffea arabica varieties as a substrate. Coffee pulp was fermented for 72 hours with a selected yeast strain (Saccharomyces cerevisiae L.), acid, pectin lyase, and water. Several parameters, such as temperature, pH, sugar concentration and alcoholic strength were measured to monitor the fermentation process. Subsequently, the alcoholic mashes were double distilled with stainless steel pot stills and a sensory evaluation of the products was conducted. Furthermore, the chemical composition of fermented mashes and produced distillates were evaluated. It showed that elevated methanol concentrations were present in mashes and products of all three varieties. The sensory evaluation found the major aroma descriptor for the coffee pulp spirits as being stone fruit. The fermentation and distillation experiments revealed that coffee pulp can be successfully used as a raw material for the production of fruit spirits. However, the spirit quality and its flavour characteristics can be improved with optimised process parameters and distillation equipment.

Acrylamide is probably carcinogenic to humans (International Agency for Research on Cancer, group 2A) with major occurrence in heated, mainly carbohydrate-rich foods. For roasted coffee, a European Union benchmark level of 400 µg/kg acrylamide is of importance. Regularly, the acrylamide contents are controlled using liquid chromatography combined with tandem mass spectrometry (LC-MS/MS). This reference method is reliable and precise but laborious because of the necessary sample clean-up procedure and instrument requirements. This research investigates the possibility of predicting the acrylamide content from proton nuclear magnetic resonance (NMR) spectra that are already recorded for other purposes of coffee control. In the NMR spectrum acrylamide is not directly quantifiable, so that the aim was to establish a correlation between the reference value and the corresponding NMR spectrum by means of a partial least squares (PLS) regression. Therefore, 40 commercially available coffee samples with already available LC-MS/MS data and NMR spectra were used as calibration data. To test the accuracy and robustness of the model and its limitations, 50 coffee samples with extreme roasting degrees and blends were additionally prepared as test set. The PLS model shows an applicability for the varieties C. arabica and C. canephora, which were medium to very dark roasted using drum or infrared roasters. The root mean square error of prediction (RMSEP) is 79 µg/kg acrylamide (n=32). The PLS model is judged as suitable to predict the acrylamide values of commercially available coffee samples. On the other hand, very light roasts containing more than 1000 µg/kg acrylamide are currently not suitable for PLS prediction.

The production of coffee leaf tea (Coffea arabica) in El Salvador and the influences of processing steps on non-volatile compounds and volatile aroma-active compounds were investigated. The tea was produced according to process steps of conventional tea (Camellia sinensis) with available possibilities on the farm. Influencing factors were the leaf type (old, young, yellow, shoots), processing (blending, cutting, rolling, freezing, steaming), drying (sun drying, oven drying, roasting) and fermentation (wild, yeast, Lactobacillus). Subsequently, the samples were analysed for the maximum levels of caffeine, chlorogenic acid, and epigallocatechin gallate permitted by the European Commission. The caffeine content varied between 0.37 g/100 g dry mass (DM) and 1.33 g/100 g DM, the chlorogenic acid between not detectable and 9.35 g /100 g DM and epigallocatechin gallate could not be detected at all. Furthermore, water content, essential oil, ash content, total polyphenols, total catechins, organic acids, and trigonelline were determined. Gas chromatography—mass spectrometry-olfactometry and calculating of the odour activity values (OAVs) were carried out to determine the main aroma-active compounds, which are β-ionone (honey-like, OAV 132-927), decanal (citrus-like, floral, OAV 14-301), α-ionone (floral, OAV 30-100), (E,Z)-2,6-nonadienal (cucumber-like, OAV 18-256), 2,4-nonadienal (melon-like, OAV 2-18), octanal (fruity, OAV 7-23), (E)-2 nonenal (citrus-like, OAV 1-11), hexanal (grassy, OAV 1-10), and 4-heptenal (green, OAV 1-9).

Cold brew coffee is a new trend in coffee industry. This paper presents pilot studies into several aspect of this beverage. Using an online survey, the current practices of cold brew coffee preparation were investigated identifying a rather large variability with a preference for extraction of medium roasted Arabica coffee using 50-100 g/l at 8°C for about 1 day. Sensory testing using ranking and triangle tests showed that cold brew may be preferred over iced coffee (cooled down hot extracted coffee). Extraction experiments at different conditions combined with nuclear magnetic resonance (NMR) analysis showed that the usual extraction time may be longer than necessary as most compounds are extracted within only a few hours, while increasing turbulence (e.g. using ultrasonication) and temperature may additional increase the speed of extraction. NMR analysis also revealed a possible chemical differentiation between cold brew and hot brew using multivariate data analysis. Decreased extraction time and reduced storage times could be beneficial for cold brew product quality as microbiological analysis of commercial samples detected samples with spoilage organisms and contamination with Bacillus cereus.

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.