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目的:运用液-质联用技术(LC-MS/MS),建立测定人体血浆中万古霉素浓度的方法,监测万古霉素血药浓度。方法:以替洛福韦为内标,乙腈沉淀蛋白后,经LC-MS/MS方法分析。采用色谱柱为安捷伦Poroshell 120 EC-C18柱(4.6 mm×100mm,2.7μm),流动相为混合有机相(乙腈∶甲醇-2∶1)-0.1%甲酸水溶液(10∶90);流速0.4 mL·min-1;采用质谱电喷雾电离源(ESI),正离子模式,多重反应监测方式(MRM)检测;待测物质万古霉素用于定量的母子离子对:m/z 725.6→m/z 144.2,内标替洛福韦用于定量的母子离子对:m/z288.0→m/z176.2。结果:万古霉素在0.2~100μg·mL~(-1)范围内线性关系良好,最低定量限为0.2μg·mL~(-1);日内RSD均在6%以下,日间RSD均在12%以下。提取回收率为58.01%~66.58%。结论:该分析方法快速、准确、灵敏度高、专属性强、重复性好,可用于医疗机构检测人体血浆中万古霉素的药物浓度。
OBJECTIVE: To establish a method for the determination of vancomycin in human plasma by liquid chromatography-mass spectrometry (LC-MS / MS) and monitor the plasma concentration of vancomycin. Methods: Tolufloxacin was used as an internal standard. Acetonitrile was used to precipitate proteins and analyzed by LC-MS / MS. The column was Agilent Poroshell 120 EC-C18 column (4.6 mm × 100 mm, 2.7 μm) with a mobile phase of mixed organic phase (acetonitrile: methanol-2: 1) Min -1; ESI, positive ion mode and multiple reaction monitoring (MRM) were used to detect the mass spectrometry; m / z 725.6 → m / z 144.2, internal standard tilofloxacin for quantitative mother-ion pair: m / z 288.0 → m / z 176.2. Results: The linear range of vancomycin was 0.2 ~ 100μg · mL ~ (-1), with the lowest limit of quantitation of 0.2μg · mL ~ (-1). The intraday RSD was less than 6% and the intraday RSD was 12 %the following. The extraction recovery was 58.01% ~ 66.58%. Conclusion: The method is rapid, accurate, sensitive, specific and reproducible. It can be used in medical institutions to detect vancomycin in human plasma.