LC-ESI-MS/MS测定人血浆中氨氯地平的含量  

Determination of Amlodipine in Human Plasma by LC-ESI-MS/MS Method

作　　者：郑枫[1] 吴春勇[1] 邵琳智[1] 钱晓萍[1] 陈磊[1] 刘文英[1] 高署 蒋志文[3] 

机构地区：[1]中国药科大学药分教研室,南京210009 [2]安徽合肥合源医药科技有限公司,合肥230038 [3]蚌埠医学院药学系,安徽蚌埠233003

出　　处：《中国药学杂志》2006年第21期1663-1666,共4页Chinese Pharmaceutical Journal

摘　　要：目的建立高灵敏度的LC-ESI-MS／MS测定人血浆中氨氯地平浓度的方法。方法 血浆样品经氢氧化钠溶液碱化，乙醚液．液萃取后进行分析。色谱柱：COSMOSIL C18柱（2．0mm×150mm，5μm），流动相：甲醇-水-甲酸（60：40：0．1），流速：0．25mL·min^-1，通过电喷雾离子化四极串联质谱，以选择离子反应监测（SRM）扫描方式进行检测。用于定量分析的监测离子分别为：m／z 409→238（氨氯地平）和m／z237→194（内标，卡马西平）。结果 回收率为86％～95％，线性范围为0．1～6μg·L^-1，定量下限为0．1μg·L^-1，检测限为0．01μg·L^-1，应用此法测定了20名健康受试者交叉口服5mg氨氯地平剂量的试验制剂和参比制剂后的血药浓度经时过程。结论 该法具有更高的灵敏度，适用于测定口服低剂量药物后人血浆中氨氯地平的浓度。OBJECTIVE To develop a sensitive and specific LC-ESI-MS/MS method for the determination of amlodipine in human plasma.METHODS Amlodipine and intemal standard carbamazepine were extracted from plasma with ether after being alkalized by NaOH, then separated on a COSMOSIL Cls column. The mobile phase consisted of methanol-water-formic acid（60：40：0.1 ）, at the flow rate of 0.25 mL· min^- 1. A Finnigan TSQ tandem mass spectrometer equipped with electrospray ionization source was used as detector and was operated in the positive ion mode. Selected reaction monitoring（SRM）using the prectwsor→product ion combinations of m/z 409 → 238 and m/z 237→194 was used to quantify amlodipine and internal standard, respectively. RESULTS The recoveries of amlodipine were 86% - 95 %. The standard curve was linear in the range of 0.1 - 6 μg· L^- 1 . The limit of quantification was below 0.1 μg·L^- 1 and the limit of detection was below 0.01 μg·L^-1 .The method was successfully used in the determination of amlodipine in plasma of 20 male volunteers after oral administration of 5 mg amlodipine test and reference tablets by the random two-way cross-over design . CONCLUSION The method is proved to be suitable for the determination of amlodipine in human plasma after oral administration of low dosage, which offers advantage of much greater sensitivity over the previously reported methods.

关 键 词：液相色谱-质谱 氨氯地平 血药浓度 测定 

分 类 号：R969[医药卫生—药理学]