摘要
目的:建立简便液质联用(LC—MS)直接沉淀法测定人体血浆咪哒唑仑及1-羟咪哒唑仑的浓度。方法:Waters XterraC_(18)(150 mm×2.1mm,5μm)色谱柱,流动相为10 mmol·L^(-1)甲酸铵-乙腈(40:60,v/v),流速为0.2 mL·min^(-1),进样体积为20μL,柱温为40℃,样品室温度为5℃。结果:咪哒唑仑线性范围为0,56～287 ng·mL^(-1),1-羟咪哒唑仑线性范围为0.56～285 ng·mL^(-1),咪哒唑仑和1-羟咪哒唑仑最低检测限低于0.14 ng·mL^(-1)和0.28 ng·mL^(-1),方法灵敏、稳定,特异性高,已成功地应用到人体血浆咪哒唑仑及1-羟咪哒唑仑药代动力学研究。结论:该方法简便、准确,重复性好,可以准确地测定人体血浆咪哒唑仑及1-羟咪哒唑仑的浓度。
Objectives：To develop an LC - MS method with direct precipitation of protein in sample to determine the concentration of midazolam and 1 - hydroxymidazolam in human plasma. Methods ： LC - MS equipment with ESI source and Waters Xterra C18 column（ 150 mm ×2.1 mm,5 μm） were used in the experiment. The column temperature was kept at 40 ℃. 10 mmol·L^- 1 ammonium formate -acetonitrile （40： 60, v/v）was used as mobile phase and the flow rate was 0. 2 mL ·min^-1. The sample room temperature was kept at 5 ℃ and the injection volume was 20 μL. Rusults ： midazolam and 1 - hydroxymidazolam were in linear range of 0.56 - 287 ng· mL^ - 1 and 0. 56 - 285 ng · mL^-1 respectively, the limitation of detection for midazolam and 1 - hydroxymidazolam were about 0.14 ng·mL^-1 and 0. 28 ng·mL^-1 , the method was high sensitive, stable and specific and has already been used for phar- macokinetic study of midazolam and 1 - hydroxymidazolam in human successfully. Conclusions： the method is simple, accurate, reproducible for the determination of midazolam and metabolite 1 - hydroxymidazolam in human plasma and suitable for the study in pharmacology.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2008年第6期839-843,共5页
Chinese Journal of Pharmaceutical Analysis
基金
国家自然科学基金项目(30472054)
