液-质联用法同时测定复方鹿角颗粒中18种氨基酸的含量

Assay of amino acids in compound Lujiao granules by liquid chromatography tandem mass spectrometry

目的：建立液相色谱一串联质谱（LC-MS／MS）法，同时测定复方鹿角颗粒水解后18种氨基酸的含量。方法：样品经过150℃水解1h处理后直接进样，无需进行衍生化和固相萃取等烦琐的前处理步骤。液相色谱柱为Agilent Zorbax Eclipse AAA（4．6rm×150mm，5μm）。采用0．1％甲酸水溶液和90％乙腈水溶液为流动相进行梯度洗脱；洗针液为50％乙腈水溶液（含0．1％甲酸），流速为0．2ml·min。结果：18种氨基酸的检出限（LOD）为3．00-30．0ng·ml-1，线性相关系数均大于0．9978，峰面积测定的相对标准偏差（RSD）在5％以内。结论：该方法分析效率高、灵敏度和选择性高，适用于复方鹿角颗粒氨基酸的定性定量分析。

OBJECTIVE To determine contents of amino acids in compound Lujiao granules by liquid chromatography tandem mass spectrometry （LC-MS/MS）. METHODS Compound Lujiao granules were hydrolyzed for 1 hour at 150 ℃ and analyzed directly without derivatization or solid phase extraction. LC separation was carried on a Agilent Zorbax Eclipse AAA （4. 6 ram x 150 ram, 5/μm） column with mobile phase of water solution containing 0. 1 % formic acid and acetonitrile/water （v/v, 90 ：10） at flow rate of 0. 2 ml. min-1 in gradient mode. RESULTS Limits of detection （LOD） of eighteen amino acids were in range of 3.00-30. 0 ng. ml-1 （S/N = 3）, linear correlation coefficients were above 0. 9978 in all cases. Relative standard devia- tions （RSDs） of peak areas of extracted ion chromatograms were in range of 5%. CONCLUSION LC-MS/MS is efficient, sensitive and selective, which is helpful for determination of amino acids incompound Lujiao granules.