高效液相色谱质谱法测定人血浆中索拉菲尼的浓度

发布时间：2018-01-26 21:52

  本文关键词： 索拉菲尼 液质联用法 血药浓度 药代动力学　出处：《中国临床药理学杂志》2016年20期 　论文类型：期刊论文

【摘要】：目的建立人血浆中索拉菲尼浓度测定的HPLC-MS/MS方法。方法人血浆样品用乙腈-沉淀蛋白后,色谱柱:Eclipse Plus C18(2.1 mm×100 mm,3.5μm),流动相:乙腈∶10 mmol·L~(-1)醋酸铵溶液(均含0.05%甲酸)=80∶20,流速:0.25 m L·min~(-1)。用电喷雾离子化源,正离子方式,多反应监测扫描方式进行监测。考察该方法的专属性、标准曲线和定量下限、精密度与回收率、基质效应以及稳定性。结果血浆中索拉菲尼的线性范围为0.02~10.00μg·m L~(-1)(r=0.997 1),定量下限为0.02μg·m L~(-1);质控样品的准确度在95.01%~104.86%;日内、日间RSD均小于15%;提取回收率为82.08%~89.72%,无明显基质效应。质控样品室温放置8 h、处理后自动进样器4℃放置12 h,反复冻融3次,于-80℃环境中放置20 d后准确度在91.78%~106.19%,RSD在4.31%~9.73%。结论本方法快速、灵敏、准确,专属性强,重复性好,适用于人血浆中索拉菲尼浓度的测定。
[Abstract]:Objective to establish a HPLC-MS/MS method for the determination of solafenil in human plasma. Methods Human plasma samples were treated with acetonitrile-precipitated protein. The chromatographic column was: eclipse Plus C182.1 mm 脳 100mm ~ (3. 5 渭 m). Mobile phase: acetonitrile: 10 mmol 路L ~ (-1) ammonium acetate solution (all containing 0.05% formic acid) 80: 20. The flow rate is 0.25 mL 路min ~ (-1). The electrospray ionization source, the positive ion mode and the multi-reaction monitoring and scanning method are monitored. The specificity, the standard curve and the quantitative limit of the method are investigated. Results the linear range of Solafenil in plasma was 0.02 渭 g 路mL ~ (-1) ~ (-1) 渭 g 路m ~ (-1). The lower limit of quantification is 0.02 渭 g 路mL ~ (-1); The accuracy of quality control samples was 95.01 and 104.86; During the day, RSD was less than 15. The recovery rate was 82.08% and 89.72%, and there was no obvious matrix effect. The quality control samples were stored at room temperature for 8 hours, and the automatic sampler was placed at 4 鈩，

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