液相色谱-质谱/质谱联用技术分析18种游离氨基酸

The analysis of 18 free amino acids by liquid chromatography/mass spectrometry/mass spectrometry

目的：建立氨基酸的液相色谱-质谱检测方法。方法：无需衍生处理，直接用乙腈：水：甲酸（5：95：0．1．v／v／v）为流动相进行反相液相色谱分离，用电喷雾正离子源进行离子化，选择反应监测方式（SRM）对这18种氨基酸的母离子及子离子进行监测，三级四极质谱测定。结果：该方法抗干扰能力强，方法重现性好，RSD0．4％。3．7％，回收率95％～104％，相关系数0．9931-0．9999，检出限0．5～8mol／ml。结论：该方法简单、快速、准确、灵敏，适合测定各种样品中的游离氨基酸。

Objective：To establish a sensitive method for determination of amino acids by liquid chromatography/mass spectrometry/mass spectrometry. Methods ：The amino acids needn＇t derivation were extracted by water. After filtration, the extract was separated by reverse phase liquid chromatography using acetonitrile： water ： formic acid （5： 95： 0. 1, v/v/v） as the elution solvents at 0.2 ml/min drip rate, confirmed and quantified by mass spectrum in the select reaction monitoring （SRM） mode via positive electrospray ionization （ ＋ ESI）. Results：The method had strong anti -jamming ability, the calibration curves of the amino acids were excellent with correlation coefficients between 0. 9931 and 0. 9998, and RSD were between 0. 4% and 3. 7%, the recoveries were between 95% and 104%, the detection limits were 0. 5 - 8 pmol/ml. Conclusion ：The established method is quite suitable for identification and quantification of amino acids. It is simple, rapid, accurate and sensitive.