Preprint Article Version 1 Preserved in Portico This version is not peer-reviewed

Simultaneous Determination of Pharmaceuticals by Solid-phase Extraction and Liquid Chromatography–tandem Mass Spectrometry: A Case Study from Sharjah Sewage Treatment Plant

Mohammad H. Semreen
* ORCID logo ,
Abdallah Shanableh
,
Lucy Semerjian
,
Hasan Alniss
ORCID logo ,
Muath Mousa
,
Xuelian Bai
,
Kumud Acharya
Version 1 : Received: 31 January 2019 / Approved: 2 February 2019 / Online: 2 February 2019 (03:21:04 CET)

A peer-reviewed article of this Preprint also exists.

Semreen, M.H.; Shanableh, A.; Semerjian, L.; Alniss, H.; Mousa, M.; Bai, X.; Acharya, K. Simultaneous Determination of Pharmaceuticals by Solid-phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry: A Case Study from Sharjah Sewage Treatment Plant. Molecules 2019, 24, 633. Semreen, M.H.; Shanableh, A.; Semerjian, L.; Alniss, H.; Mousa, M.; Bai, X.; Acharya, K. Simultaneous Determination of Pharmaceuticals by Solid-phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry: A Case Study from Sharjah Sewage Treatment Plant. Molecules 2019, 24, 633.

Abstract

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.

Keywords

liquid chromatography–tandem mass spectrometry; pharmaceuticals; wastewater analysis; solid phase extraction

Subject

Chemistry and Materials Science, Analytical Chemistry

Copyright: This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

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