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目的建立了测定大鼠血浆中forsklin的液相色谱-串联质谱法(LC-MS/MS)。方法血浆样品经叔丁基甲醚萃取后,以水(0.1%甲酸)-乙腈为流动相梯度洗脱,BetaBasic-C18柱分离。通过电喷雾离子化四极杆串联质谱,以多反应监测(MRM)方式进行正离子检测,用于定量分析的离子对分别为m/z 411→375.3(forsklin)和285→193(地西泮)。结果在本实验条件下,forsklin血浆浓度测定方法的线性范围为0.5~1000 ng/ml,定量下限为0.5 ng/ml。日内、日间精密度(相对标准差RSD)均小于14.4%;准确度(相对误差RE)在-3.5%和3.8%之间。方法的专属性,绝对回收率,稳定性和基质效应均符合要求。结论该法快速、灵敏、准确,可用于forsklin的药代动力学研究。
Objective To establish a liquid chromatography-tandem mass spectrometry (LC-MS / MS) method for the determination of forsklin in rat plasma. Methods The plasma samples were extracted with tert-butyl methyl ether and eluted with a mobile phase of water (0.1% formic acid) -acetonitrile, and separated on a BetaBasic-C18 column. Electron spray ionization quadrupole tandem mass spectrometry was used for positive ion detection by MRM. The ion pairs for quantitative analysis were m / z 411 → 375.3 (forsklin) and 285 → 193 (diazepam ). Results Under the experimental conditions, the linear range of forsklin plasma concentration was 0.5-1000 ng / ml and the lower limit of quantitation was 0.5 ng / ml. Intra-day and inter-day precision (relative standard deviation RSD) were less than 14.4%; accuracy (relative error RE) was between -3.5% and 3.8%. The specificity, absolute recovery, stability and matrix effects of the method met the requirements. Conclusion The method is rapid, sensitive and accurate and can be used to study the pharmacokinetics of forsklin.