建立牛乳中未衍生游离氨基酸的超高效液相色谱串联质谱的测定方法.样品采用酸化乙腈沉淀蛋白,正己烷脱脂,氮吹至近干后初始流动相复溶,超声溶解离心过膜后检测.结果显示:在14 min内所分析目标物得到较好的分离,浓度与峰面积的线性关系良好,相关系数在0.9912~0.9998之间,回收率在76%~124%,相对标准偏差1.0%~12.9%.%A method for determining of underivatized free amino acids in milk was developed with ultra-high performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS). The protein of sample was pre-cipitated with acid acetonitrile, the supematant was purified by n-hexane,then the purified solution was con-centrated by nitrogen,dissolved with the initial mobile phase by ultrasonic assistance,centrifuged and filtered for ultra-high performance liquid chromatographic analysis. The results indicated that good separation of amino acids was obtained within 14 min. The linearity of the investigated compounds between concentrations and their peak areas within the test ranges was good, and the correlation coefficient was from 0.9912 to 0.9998. The av-erage recoveries and relative standard deviations of 14 amino acids at three spiked levels were in the range of 76%-124%and 1.0%-12.9%respectively.
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