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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 establish a liquid chromatography-tandem mass spectrometry (LC-MS / MS) method for the determination of glutamine concentration in human plasma. Methods The plasma samples were stained with trichloroacetic acid (10%) and chromatographed on an Inertsil-CN column. The mobile phase consisted of 5 mmol·L -1 ammonium acetate (0.1% formic acid) Methanol - acetonitrile (volume ratio 70:15:15), flow rate: 750μL · min -1, mass spectrometry: using multi - reaction detection mode, API2000 electrospray ionization source. Results The linearity of glutamine was 12 ~ 384 mg · L -1, and the lower limit of quantitation was 12 mg · L -1. The relative standard deviations (RSDs) were all less than 15% during the day. The main pharmacokinetic parameters of single oral glutamine granules in healthy male subjects were as follows: tmax was (0.77 ± 0.13) h, ρmax was (75.3 ± 29.0) mg · L -1, t_ ( 1/2) was (1.83 ± 1.93) h, and the AUC_ (0-t) was (109.2 ± 40.1) mg · h · L -1 and the AUC_ (0-∞) was (114.0 ± 40.4) mg · h · L -1. Conclusion This method is suitable for human pharmacokinetic study of glutamine granules.