LC-MS/MS测定大鼠血浆中1-脱氧野尻霉素及药代动力学研究  

Determination of 1-Deoxynojirimycin in Rat Plasma and Pharmacokinetics by LC-MS/MS

作　　者：冯颖[1] 何俊[1] 王兴蕊[1] 窦婷[1] 欧阳慧子[2] 

机构地区：[1]天津中医药大学中医药研究院天津市现代中药重点实验室,天津300193 [2]天津中医药大学第一附属医院,天津300193

出　　处：《辽宁中医药大学学报》2013年第12期111-113,共3页Journal of Liaoning University of Traditional Chinese Medicine

基　　金：科技部国际科技合作项目(2009DFA31070);天津市科技计划项目(10SYSYJC28900)

摘　　要：目的：建立大鼠血浆中1-脱氧野尻霉素（DNJ）的液相色谱-质谱联用（LC-MS/MS）测定方法,并用于大鼠口服桑叶总生物碱后DNJ的药代动力学研究。方法：血浆样品经甲醇沉淀蛋白后,以乙腈-6.5mmol·L-1甲酸铵水溶液为流动相,采用AgilentEclipsePlusC18柱（2.1mm×150mm,3.5μm）进行分离,梯度洗脱,流速0.4mL·min-1。采用电喷雾离子源,多反应监测（MRM）模式,正离子检测,用于定量的离子反应为m/z164.0→69.0（DNJ）,m/z208.1→146.0（米格列醇,内标）。结果：DNJ在1~500ng·mL-1浓度范围内线性关系良好,日内、日间精密度（RSD）均小于10.9%,准确度在92.4%~112.7%,DNJ和内标的提取回收率均大于84.1%。结论：本方法快速、灵敏、操作简便,可用于1-脱氧野尻霉素的药代动力学研究。Objective： To develop an LC-MS/MS method for the determination of 1-Deoxynojirimycin （ DNJ ） in rat plasma and to investigate its pharmacokinetic characteristic. Methods ： The plasma samples were protein precipitated with methanol. After sample preparation, the samples were separated on a Waters Atlantis Hilie Silica （ 2.1 mm × 100 mm, 3 μ m ） column using acetonitrile and water （ containing of 6.5 mmol· L-1 ammonium formate ） as mobile phase in gradient elution mode. The mass spectrometer was operated under the positive ion mode with the ESI source and the detection was performed by the multiple reaction monitoring （ MRM ） of the transition of m/z 164.0→69.0 for DNJ and m/z 208.1 → 146.0 for miglitol （ internal standard, IS ）. Results ： The calibration curve for DNJ was linear over the range of 1-500 ng · mL-1. The intra-day and inter-day precisions were within 10.9% and the accuracies were ranging between 92.4% and 112.7%. The recoveries of DNJ and IS were all above 84.1%. Conclusion ： The analysis method is rapid, accurate, simple and suitable enough to he applied in the pharmacokinetic study of DNJ.

关 键 词：液相色谱-质谱联用法 1-脱氧野尻霉素 药代动力学 

分 类 号：R927.2[医药卫生—药学]