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Simultaneous determination of 44 pharmaceutically active compounds in water samples using solid-phase extraction coupled with ultra-performance liquid chromatography-tandem mass spectrometry

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Abstract

This study examines an improved and simplified method for solid-phase extraction (SPE), which offers rapid and accurate determination and identification of 44 pharmaceutically active compounds using ultra-performance liquid chromatography (UPLC) and tandem mass spectrometry (MS/MS). The common active compounds include four macrolides, seventeen sulfonamides, four quinolones, chloramphenicol, eight β-lactams, four tetracyclines, lincomycin, amantadine, 4-acetamidophenol, phenylbutazone, trimethoprim, clenbuterol, and hydrocortisone in water samples. We optimized crucial parameters of MS/MS, UPLC, and SPE and studied the matrix effect related to the modified analytical process from water samples. The matrix-matched calibration curves were accomplished at seven concentration levels and a satisfactory linear relationship (r2 > 0.994) was observed within the range of 0.1–500 ng/mL. Results show varying limits of detection (0.0111–0.966 ng/L for different analytes based on signal-to-noise (S/N) = 3) and limits of quantitation (0.0382–3.26 ng/L). Recoveries of the spiked samples ranged from 75.7 to 108% with relative standard deviation lower than 9.6%. The proposed method was successfully applied to the analysis of real samples.

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Acknowledgments

The authors would like to thank Fanxu Yang and Tao Xue for their kind help and useful scientific discussions.

Funding

This work has been supported by Zhejiang Medical and Health Technology Project (2017KY131) and Hangzhou Science and Technology Development Project (20170533B72).

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Correspondence to Ming Xue.

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Xue, M., Wu, H., Liu, S. et al. Simultaneous determination of 44 pharmaceutically active compounds in water samples using solid-phase extraction coupled with ultra-performance liquid chromatography-tandem mass spectrometry. Anal Bioanal Chem 412, 203–222 (2020). https://doi.org/10.1007/s00216-019-02229-8

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