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. 2019 Feb 11;24(3):633.
doi: 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

Mohammad H Semreen  1   2 , Abdallah Shanableh  3 , Lucy Semerjian  4 , Hasan Alniss  5   6 , Mouath Mousa  7 , Xuelian Bai  8 , Kumud Acharya  9
Affiliations

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 et al. Molecules. .

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.

Keywords: liquid chromatography-tandem mass spectrometry; pharmaceuticals; solid phase extraction; wastewater analysis.

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Conflict of interest statement

There are no conflicts to declare.

Figures

Figure 1
Figure 1
Graph bars showing the effect of pH on the % recoveries of the selected pharmaceuticals at (A) pH 3 using Oasis HLB, ENVI-C18 and Oasis MAX cartridges. (B) pH 7 using Oasis HLB, ENVI-C18 and Oasis MAX cartridges (C) comparison of the recoveries at pH 3 and 7 using HLB oasis cartridge using Oasis HLB, ENVI-C18 and Oasis MAX at two pH values (n = 3).
Figure 2
Figure 2
Chromatogram showing the separation of the selected pharmaceuticals using the optimized chromatographic conditions. (a) Acetaminophen, (b) Sulfadiazine, (c) Sulfapyridine, (d) Sulfamethazine, (e) Ofloxacin, (f) (Sulfamethoxazole and ciprofloxacin), (g) Metoprolol, (h) Resperidone, and (i) Erythromycin.
Figure 3
Figure 3
MRM LC-MS/MS chromatograms of the target compounds analyzed by positive ionization mode.
See this image and copyright information in PMC

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