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.
出处
《北京师范大学学报（自然科学版）》
CAS
CSCD
北大核心
2012年第3期323-326,共4页
Journal of Beijing Normal University(Natural Science)
