液相色谱-质谱/质谱联用法测定人血浆中加兰他敏  

LS-MS/MS determination of galanthamine in human plasma

作　　者：张琰[1] 刘梅[1] 文爱东[2] 杨林[2] 李微[2] 袁静[2] 高晓华[2] 

机构地区：[1]第四军医大学唐都医院药学部,西安710038 [2]第四军医大学西京医院药学部,西安710032

出　　处：《药物分析杂志》2007年第7期973-976,共4页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立测定人血浆中加兰他敏浓度的液相色谱-质谱/质谱联用法,用于其人体血药浓度测定。方法:血浆样品经液-液萃取后,以甲醇-水-甲酸(65:35:1)为流动相,Zorbax SB-C_8柱(150mm×4.6mm,5μm)分离,采用大气压化学电离源,以选择反应监测方式进行正离子检测。内标为双氢吗啡酮,用于定量分析的离子反应分别为 m/z 288→m/z 213(加兰他敏)和 m/z 286→m/z 185(内标)。结果:血浆中加兰他敏最低定量限为0.5ng·mL^(-1),其线性范围为0.5～100ng·mL^(-1)。其高、中、低3个浓度的平均提取回收率为80.9%,方法回收率为100.5%,日内及日间 RSD 均<8%。结论:方法选择性强,灵敏度高,快速准确,可作为加兰他敏人体内药动学研究的手段。Objective ： To develop a sensitive, specific LC - MS/MS method for the determination of galanthamine in human plasma. Methods：Galanthamine and internal standard dihydromorphone were extracted from plasma using a simple liquid - liquid extraction, then separated on a Zorbax SB - C18 column （ 150 mm × 4. 6 mm, 5 μm） with the mobile phase consisting of methanol - water - formic acid （65： 35：1 ）. A Finnigan TSQ tandem mass spectrometer equipped with atmospheric pressure chemical ionization source was used as detector and operated in the positive ion mode. Selected reaction monitoring using the precursor →product ion combinations of m/z 288 → 213 and m/z 286 185 was used to quantify galanthamine and internal standard, respectively. The accuracy, precision, selectivity, lower limit of quantification, linearity and extraction recovery were evaluated, as well as the stability of the compound in plasma. Results：The limit of quantification was 0. 5 ng·mL^-1. The standard curve was linear over the range 0. 5 - 100 ng·mL^-1. The mean extraction recovery and method recovery were 80. 9% and 100.5% ,respectively. The within - day and between - day precision studies showed good reproducibility with RSD less than 8% for all the analytes. Conclusion：The method offers advantages of specificity,speed, sensitivity and has been applied to determine the concentration of galanthamine in human plasma.

关 键 词：加兰他敏 血药浓度 液相色谱-质谱/质谱联用法 

分 类 号：R917[医药卫生—药物分析学]