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

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

Analytical and bioanalytical chemistry (2019-12-06)
Ming Xue, Haocheng Wu, Shaoying Liu, Xihui Huang, Quan Jin, Ren Ren
要旨

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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製品番号
ブランド
製品内容

Sigma-Aldrich
タイロシン 溶液, 8 mg/mL in 0.9% NaCl, 0.1 μm filtered, BioReagent, suitable for cell culture
Supelco
スルファジアジン-フェニル-13C6, VETRANAL®, analytical standard
システム適合性用ロキシスロマイシン, European Pharmacopoeia (EP) Reference Standard