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目的建立超高效液相串联质谱法快速测定大鼠体内8-O-乙酰山栀苷甲酯的浓度。方法用乙腈沉淀蛋白方法处理血浆,色谱柱为ACQUITY UPLC BEH C18柱(50 mm×2.1 mm,1.7μm);流动相为乙腈-0.1%甲酸水,梯度洗脱,流速为0.4 m L·min?1;用正离子多离子反应监测(MRM)扫描,内标为槲皮素。结果血浆中8-O-乙酰山栀苷甲酯的线性范围为2.5~500 ng·m L?1(r=0.997 9),最低定量限为0.5 ng·m L?1。低、中、高3个浓度(3,45和450 ng·m L?1)的质控样品的日内、日间精密度RSD均<10%,3个浓度的相对回收率分别为(103.59±4.75)%,(98.68±4.62)%和(97.06±5.64)%。结论该方法操作简便、快捷,灵敏度高,适于大鼠血浆中8-O-乙酰山栀苷甲酯浓度的测定及其药代动力学研究。
OBJECTIVE To establish a rapid method for the determination of 8-O-acetylgossyparin methyl ester in rat by ultra performance liquid chromatography-tandem mass spectrometry. Methods The plasma was treated with acetonitrile-precipitated protein. The column was ACQUITY UPLC BEH C18 (50 mm × 2.1 mm, 1.7 μm). The mobile phase consisted of acetonitrile-0.1% formic acid water with gradient elution at a flow rate of 0.4 m L · min- 1; positive ionized multiple ion reaction monitoring (MRM) scan, the internal standard for quercetin. Results The linear range of 8-O-acetylglucoside methyl ester in plasma was 2.5-500 ng · m L -1 (r = 0.997 9) and the lowest limit of quantification was 0.5 ng · m L -1. The RSDs of intra-day and inter-day precision of low, middle and high quality control samples (3,45 and 450 ng · m L -1) were all less than 10%, and the relative recoveries of the three concentrations were (103.59 ± 4.75)%, (98.68 ± 4.62)% and (97.06 ± 5.64)%, respectively. Conclusion The method is simple, rapid and sensitive. It is suitable for the determination of 8-O-acetylglucoside methyl ester in rat plasma and its pharmacokinetics.