LC-MS/MS法同时测定人血浆中氨苄西林氯唑西林浓度

LC-MS/MS determination of ampicillin and clozacillin in human plasma

目的:建立高效液相色谱-串联质谱联用法同时测定人血浆中氨苄西林氯唑西林浓度。方法:选用Shim-pack VP-ODS色谱柱(5μm,150mm×4.6mm),以甲醇-10mmol·L-1醋酸铵为流动相,样品用甲醇进行沉淀蛋白后进样,选用3200 QTRAP型串联质谱多反应监测(MRM)扫描方式进行检测。结果:氨苄西林、氯唑西林的线性范围分别在0.1～30μg·mL-1和0.05～15μg·mL-1,准确度与精密度结果显示方法日间、日内变异均小于15%,方法提取回收率大于90%,稳定性较好。结论:本研究所建立的方法快速、灵敏,专属性强,重现性高,可用于氨苄西林氯唑西林人体药代动力学试验。

Obiective：To develop an LC-MS/MS method for the determination of the ampicillin and clozacillin in human plasma.Method：Ampicillin,clozacillin and the internal standard were extracted from plasma by methanol which used as deproteinated solvent,and separated on a Shim-pack VP-ODS column using methanol and 10 mmol·L^-1 ammonium acetate as mobile phase by gradient elution.Detection was carried out by multiple reaction monitoring on a 3200 QTRAP LC-MS/MS system.Results：The assay of ampicillin and clozacillin was linear over the range 0.1-30 μg·mL^-1 and 0.05^-15 μg·mL^-1.Intra-and inter-day precision were less than 15%,respectively.The recoveries of ampicillin and clozacillin were more than 90% and stabilities were good.Conclusion：This method is rapid,sensitive,selective and reliable for the determination of ampicillin and clozacillin in human plasma and applicable to study of pharmacokinetic of ampicillin and clozacillin.