LC-MS/MS法测定人血浆中克拉霉素的质量浓度  

LC-MS/MS DETERMINATION OF CLARITHROMYCIN IN HUMAN PLASMA

作　　者：李鹏飞[1] 孙健姿[1] 马萍[1] 王燕[1] 王静[1] 张茜[2] 谢小娟[1] 刘丽宏[1] 

机构地区：[1]第二炮兵总医院药学部,北京100088 [2]湖北中医药大学,武汉430065

出　　处：《北京师范大学学报（自然科学版）》2012年第3期323-326,共4页Journal of Beijing Normal University(Natural Science)

摘　　要：建立高效液相色谱-质谱联用法(LC-MS/MS)测定人血浆中克拉霉素的浓度.选用Shim-park VP-ODS色谱柱,以乙腈、φ=0.1%氨水、φ=0.4%甲酸乙腈溶液为流动相,采用梯度洗脱进行分离,样本经乙腈沉淀后进样,选用3200QTRAP型质谱仪的多重反应监测(MRM)扫描方式进行检测.克拉霉素质量浓度线性范围为5～1 000ng.mL-1,定量下限为5ng.mL-1,检测限为0.05ng.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%,相对偏差为-3.43%～2.97%,低、中、高3个质量浓度提取回收率为91.73%～107.73%,稳定性好.本研究所建立的方法快速、灵敏、专属性强、重现性好,可用于人体血浆中克拉霉素质量浓度的测定和药代动力学研究.An LC-MS/MS assay for clarithromycin in human plasma was developed.Plasma protein was precipitated with acetonitrile,the plasma sample was then separated on a Shim-park VP-ODS column using acetonitrile φ=0.1% ammonia water-acetonitrile（containning φ=0.4% formic acid） as the mobile phase by gradient elution.Detection was carried out by multiple reaction monitoring（MRM） on a 3200 QTRAP LC-MS/MS system.The assay was linear over the range 5-1000 ng·mL-1 with a lower limit of quantitation of 5 ng·mL-1 and a lower limit of deterction of 0.05 ng·mL-1.Intra-and inter-day variations were both less than 15%.The relative deviation was from-3.43%-2.97%.Recovery rates of clarithromycin were from 91.73%-107.73% and stabilities were good.This proves a rapid,sensitive,selective and reliable method for the determination of clarithromycin in human plasma.The assay can be used to determine clarithromycin in human plasma and for pharmacokinetics studies.

关 键 词：高效液相色谱-质谱联用法 克拉霉素 药代动力学 

分 类 号：O657.63[理学—分析化学]