LC-MS/MS法测定人体血浆中谷氨酰胺的含量  

Determination of glutamine in human plasma by liquid chromatography-tandem mass spectrometry

作　　者：韩雨钊 姜悦[1] 林茂[1] 李野[1] 李淼[1] 刘茜[1] 

机构地区：[1]沈阳药科大学药学院,辽宁沈阳110016

出　　处：《沈阳药科大学学报》2016年第7期572-576,580,共6页Journal of Shenyang Pharmaceutical University

摘　　要：目的建立测定人血浆中谷氨酰胺浓度的液相色谱串联质谱法(LC-MS/MS)。方法血浆样品用质量分数为10%的三氯乙酸沉蛋白,色谱柱:Inertsil-CN柱,流动相:5 mmol·L^(-1)醋酸铵(含体积分数为0.1%的甲酸)-甲醇-乙腈(体积比为70∶15∶15),流速:750μL·min^(-1),质谱:采用多反应检测模式,API2000电喷雾离子源。结果谷氨酰胺的线性为12~384 mg·L^(-1),定量下限为12 mg·L-1,日间日内精密度(relative standard deviation,RSD)均不大于15%。健康男性受试者单剂量口服谷氨酰胺颗粒5 g后的主要药动学参数为:tmax为(0.77±0.13)h,ρmax为(75.3±29.0)mg·L^(-1),t_(1/2)为(1.83±1.93)h,采用梯形法计算,AUC_(0-t)为(109.2±40.1)mg·h·L^(-1),AUC_(0-∞)为(114.0±40.4)mg·h·L^(-1)。结论该法适合于谷氨酰胺颗粒的人体药动学研究。Objective To develop a LC-MS / MS method for the study of the pharmacokinetics of glutamine in volunteers. Methods Glutamine were extracted from human plasma by using 10% trichloroacetic acid solution,and the separation was performed on Inertsil-CN column with the mobile phase consisting of5 mmol·L^-1 ammonium acetate（ including 0. 1% formic acid）-methyl alcohol-acetonitrile（ V ∶ V ∶ V =70∶ 15∶ 15）,at the flowrate of 750 μL·min^-1. Detection was carried out by multiple reaction monitoring with an API 2 000 triple quadrupole mass spectrometer equipped with an electrospray ionization source.Results The linear calibration curve was obtained in the range of 12- 384 mg·L^-1 for glutamine. The lower limit of quantitation was 12 mg·L^-1. The intra-day and inter-day precision RSD was less than 15%. The main pharmacokinetic parameters of volunteers who have taken 5 g of glutamine granules were calculated and shown as follows. Tmaxwas（ 0. 77 ± 0. 13） h,and ρmaxwas（ 75. 3 ± 29. 0） mg·L^-1. Half life of glutamine in plasma（ t（1 /2）） was（ 1. 83 ± 1. 93） h,while the AUC（0-t）and AUC（0-∞）was（ 109. 2 ± 40. 1） mg·h·L^-1and（ 114. 0 ± 40. 4） mg·h·L^-1,respectively. Conclusions The method is suitable for pharmacokinetic study of glutamie.

关 键 词：谷氨酰胺 药动学 液相色谱-串联质谱法 

分 类 号：R917[医药卫生—药物分析学]