液相色谱-串联质谱法测定人血浆中特拉唑嗪浓度  

Determination of terazosin concentration in human plasma by LC-MS/MS

作　　者：刘罡一[1] 贾晶莹[1] 张梦琪[1] 陆川[1] 金洁美[1] 徐珏[1] 余琛[1] 

机构地区：[1]上海市徐汇区中心医院,上海200031

出　　处：《中国新药与临床杂志》2009年第7期530-533,共4页Chinese Journal of New Drugs and Clinical Remedies

基　　金：上海市科委科研计划项目(08411966700)

摘　　要：目的建立测定血浆中特拉唑嗪的液相色谱-串联质谱(LC-MS/MS)方法。方法血浆样品中加入内标哌唑嗪,直接沉淀法处理血浆样品。色谱柱为CAPCELLPAKC18MGⅡ(100mm×2.0mm,5μm),流动相为含0.02%甲酸水溶液-含0.02%甲酸乙腈溶液(21:79,V/V)。流速为0.3mL·min-1。扫描方式为正离子多离子反应监测(MRM),特拉唑嗪和内标的离子通道分别选择为m/z388.2→290.2和384.2→95.2。结果特拉唑嗪的线性范围为0.2～100μg·L-1,定量下限为0.2μg·L-1,提取回收率为95%～102%,日内、日间RSD均小于10%。结论本方法操作简便,特异性强,灵敏度高,取血量少,符合生物样品的分析要求,可以用于特拉唑嗪的药动学研究及临床血样测定。AIM To establish a method of LC-MS/MS for determination of terazosin in human plasma.METHODS After addition of prazosin （internal standard, IS） into the plasma sample, the analyte was achieved by direct protein precipitation. The chromatographic separation was performed on CAPCELL PAK C18 MG Ⅱ （ 100 mm × 2.0 mm, 5 μm） column with a mobile phase of 0.02% formic acid water solution-0.02% formic acid acetonitrile solution （21 ： 79, V/V） with a flow rate of 0.3 mL-min^-1. The deprotonated ion of analyte was detected in positive ionization by multiple ionic reaction monitoring mode （MRM）. The mass transition pairs of m/z 388.2 → 290.2 and m/z 384.2 → 95.2 were used to detect terazosin and internal standard, respectively. RESULTS The linear concentration ranges of the calibration curves for terazosin was 0.2 - 100 μg· L^-1. The lower limit of quantitation was 0.2 μg· L^-1. The extraction recovery rate was 95% - 102%.Within-day RSD and between-day RSD were both less than 10%. CONCLUSION The processing of this method is simple with high specificity and sensitivity together with less blood sampling, therefore it is suitable for the need of pharmacokinetic and the clinical trial researches for terazosin.

关 键 词：特拉唑嗪 色谱法 高压液相 光谱法 质量 电喷雾电离 血浆 

分 类 号：R969.1[医药卫生—药理学] R972.4[医药卫生—药学]