超高效液相色谱-串联质谱法直接测定啤酒中20种游离氨基酸含量

Direct determination of 20 kinds of free amino acids in beer by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  啤酒  游离氨基酸

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  beer  free amino acids

中文摘要:

      目的 采用超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS), 建立高效、快速直接测定啤酒中20种游离氨基酸的方法。方法 啤酒样品经水稀释后, 经CAPCELL PAK CR 1:4 ST色谱柱(150 mm×2.1 mm, 5 μm)分离, 乙腈-0.3%甲酸水溶液为流动相进行梯度洗脱, 采用电喷雾离子源正离子模式, 在多反应监测模式下进行检测。结果 20种游离氨基酸在各自相应线性范围内, 线性关系良好, 相关系数(r2)均大于0.99; 加标回收率为81.3%~108.4%, 相对标准偏差在2.5%~7.2%之间, 方法检出限为1~6 ng/mL, 方法定量限在3~15 ng/mL之间。结论 该方法灵敏、准确, 具有良好的重复性和稳定性, 可快速检测出啤酒中的20种游离氨基酸成分。

英文摘要:

      Objective To establish a method for the efficient, fast and direct determination of the 20 kinds of free amino acids in beer by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods Beer samples were diluted with water, then separated on a CAPCELL PAK CR 1:4 ST chromatographic column (150 mm×2.1 mm, 5 μm) with acetonitrile-0.3% formic acid in water with a gradient elution, multiple reaction monitoring mode was used for detection in electrospray ionization with positive ion mode. Results The linear relationships of the 20 kinds of free amino acids within their corresponding linear ranges were good, the correlation coefficient (r2) were all greater than 0.99; the recoveries were between 81.3% and 108.4%, the relative standard deviations were 2.5%?7.2%, the limits of detection were 1?6 ng/mL, and the limits of quantitation were 3?15 ng/mL. Conclusion The method is sensitive, accurate, has good repeatability and stability, and it can be used for quickly determination of the 20 kinds of free amino acids in beer.