期刊
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
卷 412, 期 1, 页码 203-222出版社
SPRINGER HEIDELBERG
DOI: 10.1007/s00216-019-02229-8
关键词
Pharmaceutically active compounds; Ultra-performance liquid chromatography-tandem mass spectrometry; Water; Solid-phase extraction
资金
- Zhejiang Medical and Health Technology Project [2017KY131]
- Hangzhou Science and Technology Development Project [20170533B72]
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 beta-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 (r(2) > 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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