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目的:建立LC-MS/MS法测定人血浆中氨溴索浓度,并进行生物等效性研究。方法:血浆样品用乙腈沉淀蛋白,内标为卡马西平,采用电喷雾化离子源,监测的氨溴索和内标的离子对分别为m/z379.0/263.9和237.0/194.1,色谱柱为UltimateXB-CN(2.1 mm×150 mm,5μm),流动相为乙腈:0.2%甲酸=40:60,流速为0.3 ml·min~(-1),进样量为10μl。结果:氨溴索标准曲线线性范围为0.53～187.50 ng·ml~(-1),最低定量限为0.53 ng·ml~(-1),低、中、高三种浓度的批内和批间精密度RSD(%)均小于15%,准确度分别为101.41%、105.40%和106.04%,提取回收率分别为82.51%、93.57%和89.19%,基质效应分别为90.48%、92.36%和100.81%,稳定性试验表明样品在本试验条件下稳定。结论:该方法灵敏度高、专属性强、准确、简便,适用于氨溴索的生物等效性研究。
OBJECTIVE: To establish a LC-MS / MS method for the determination of ambroxol in human plasma and to study its bioequivalence. METHODS: Plasma samples were precipitated with acetonitrile and carbamazepine was the internal standard. The electrospray ionization source was used. The ion pairs monitored for ambroxol and internal standard were m / z 379.0 / 263.9 and 237.0 / 194.1, respectively. The column was UltimateXB-CN (2.1 mm × 150 mm, 5 μm) was used. The mobile phase consisted of acetonitrile 0.2% formic acid 40:60, flow rate 0.3 ml · min -1 and injection volume 10 μl. Results: The linear range of ambroxol standard curve was 0.53 ~ 187.50 ng · ml ~ (-1), the lowest limit of quantification was 0.53 ng · ml ~ (-1), and the intra- and inter- The RSD (%) were less than 15% and the accuracy was 101.41%, 105.40% and 106.04%, respectively. The recovery rates were 82.51%, 93.57% and 89.19%, and the matrix effects were 90.48%, 92.36% and 100.81% Stability tests show that the sample is stable under the conditions of this test. Conclusion: This method has high sensitivity, specificity, accuracy and convenience, and is suitable for the bioequivalence study of ambroxol.