浓缩果汁中20种氨基酸的超高效液相色谱-串联质谱法同时测定  

Simultaneous Determination of 20 Amino Acids in Concentrated Juices Using Ultra Performance Liquid Chromatography Tandem Mass Spectrometric Method

作　　者：孔祥虹 付兴隆 张磊[2] 乐爱山 何强 黄江瑞[2] 

机构地区：[1]陕西出入境检验检疫局,陕西西安710068 [2]西安理工大学应用化学系,陕西西安710054

出　　处：《分析测试学报》2010年第4期347-352,共6页Journal of Instrumental Analysis

基　　金：国家质检总局科研资助项目(2007IK166);陕西省科技计划资助项目(2008K01-06)

摘　　要：建立了同时测定浓缩果汁中20种氨基酸含量的超高效液相色谱-串联质谱法（UPLC—MS／MS）。样品经异硫氰酸苯酯（PITC）衍生，0．1％甲酸（含1mmol·L^-1甲酸铵）-乙腈溶液定容后，采用ACQUITYUP—LC BEHC18（1．7μm×2．1mm×50mm）色谱柱分离，以0．1％甲酸（含1mmol·L^-1甲酸铵）-乙腈溶液为流动相，在0．3mL·min^-1流速下梯度洗脱，MS／MS检测、外标法定量。果汁中除天门冬氨酸的检出限（LOD）为500．0ng·g。。外，其它均为100．0ng·g^-1。线性范围为10．0～1000．0μg·L^-1（r≥0．9900），平均加标回收率为79％～120％，相对标准偏差（n=6）小于8．0％。该方法具有杂质干扰小、分析速度快、灵敏度高等特点，适用于果汁中氨基酸的定性定量分析。A method was developed for the determination of twenty amino acids in concentrated juices using ultra performance liquid chromatography - tandem mass spectrometric method （ UPLC - MS/ MS）. The sample was derivatived by phenylisothioeyanate and diluted by the mobile phase. The separation of amino acids was performed on a ACQUITY UPLC BEH C18 （ 1.7 μm×2. 1 mm × 50 mm） column using acetonitrile -0. 1% formic acid containing 1 mmol·L^-1 ammonium formate （30 ： 70, by volume） as mobile phase with gradient elution. The flow rate was 0. 3 mL^-1 min The result indicated that the calibration curves were linear in the range of 10.0 - 1 000.0 μg · L^-1 for amino acids. The detection limits were 500.0 ng·g^-1 for asparagine and 100. 0 ng· g^-1 for other amino acids. The average recoveries for all analytes were between 79% and 120% with RSDs（ n = 6） less than 8.0%. The method showed the advantages of good reproducibility, low detection limit and high sensitivity, and was suitable for analysis of amino acids in concentrated juices.

关 键 词：超高效液相色谱-串联质谱 氨基酸 异硫氰酸苯酯 浓缩果汁 

分 类 号：O657.72[理学—分析化学] R977.4[理学—化学]