摘要
建立高效液相色谱-质谱联用法同时测定人血浆中免疫抑制剂及合并用药12种药物浓度的方法。选用Kromasil-C18色谱柱(50 mm×4.6 mm×5μm),以甲醇-乙腈-1 mmol/L乙酸铵溶液为流动相,采用梯度洗脱进行分离,样本用甲醇沉淀蛋白后进样,流速:1.1 mL/min;柱温:35℃;进样量:20μL。选用3200QTrap型液相色谱-串联质谱仪的多反应监测(MRM)扫描方式进行检测。12种药物的线性范围为0.2～1000μg/L;定量下限为0.2μg/L。准确度与精密度结果显示方法日间、日内RSD均小于15%;相对偏差"13%～9.33%,稳定性较好。本方法快速、灵敏,专属性强、重现性好,可用于人体血浆中免疫抑制剂及其常用合并用药共12种药物浓度的测定。
This study aims to develop an LC-MS/MS method for the determination of drugs contained immunodepressants and other drugs in human plasma.The drugs and the internal standard were treated by methanol precipitation to remove protein component from human plasma,and then separated on a Kromasil-C18 column（5 μm,50 mm×4.6 mm） with a gradient elution.The mobile phase consisted of methanol-acetonitrile-1 mmol/L ammonium acetate was maintained at 35 ℃.The flow rate was 1.1 mL/min and 20 μL aliquot of residues was injected into the LC-MS/MS system.Detection was carried out by multiple reaction monitoring on a 3200 QTrap LC-MS/MS system.The assay was linear over the range of 0.2-1000 μg/L with a lower limit of quantitation of 0.2 μg/L.Intra-and inter-day precisions were both less than 15%.The relative deviation was in the range of -13%-9.33%.The stabilities of the method were good.It is a rapid,sensitive,selective and reliable method for the determination of the drugs which contain immunodepressants and other drugs in human plasma.The assay can be applied for the determination of these drugs in human plasma.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2012年第10期1573-1578,共6页
Chinese Journal of Analytical Chemistry
基金
首都医学发展科研基金(No.2007-1016)资助
关键词
高效液相色谱-质谱联用法
免疫抑制剂
联合用药
Liquid chromatography tandem mass spectrometry
Immunodepressants
Drug combination
