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Molecules 2019, 24(3), 633; https://doi.org/10.3390/molecules24030633

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

1
College of Pharmacy, University of Sharjah, P.O. Box 27272, Sharjah, United Arab Emirates
2
Sharjah Institute for Medical Research, University of Sharjah, P.O. Box 27272, Sharjah, United Arab Emirates
3
Research Institute of Sciences and Engineering, University of Sharjah, P.O. Box 27272, Sharjah, United Arab Emirates
4
College of Health Sciences, University of Sharjah, P.O. Box 27272, Sharjah, United Arab Emirates
5
Desert Research Institute, 755 E Flamingo Rd, Las Vegas, NV 89119, United States
*
Author to whom correspondence should be addressed.
Academic Editor: Simone Morais
Received: 19 December 2018 / Revised: 31 January 2019 / Accepted: 7 February 2019 / Published: 11 February 2019
(This article belongs to the Section Analytical Chemistry)
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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 × 150 mm) using gradient elution and 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. View Full-Text
Keywords: liquid chromatography-tandem mass spectrometry; pharmaceuticals; wastewater analysis; solid phase extraction liquid chromatography-tandem mass spectrometry; pharmaceuticals; wastewater analysis; solid phase extraction
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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 (CC BY 4.0).
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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.

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