摘要
目的建立微波水解-液相色谱串联质谱法(liquid chromatography tandem mass spectrometry,LC-MS)测定保健食品中16种氨基酸的含量。方法取适量样品,加入6 mol/L盐酸溶液15 m L,加入适量苯酚,于150℃微波消解4 h,冷却稀释至80℃减压干燥1 h。样品经0.1%甲酸溶解后经Agilent-C_(18)柱分离,以乙腈-10 mmol/L乙酸铵溶液为流动相进行梯度洗脱,以串联质谱的多反应监测模式进行检测,外标法定量。结果方法的线性范围0.01~0.05 nmol/μL;平均回收率为95.6%~100.7%,相对标准偏差(relative standard deviation,RSD)小于3.0%。结论该方法分析速度快、灵敏度高、准确和重复性好,与现有技术对比,该方法通过微波技术辅助水解,缩短了样品的前处理时间,可适用于保健食品中16种氨基酸的快速检测。
Objective To establish a method for determination of 16 kinds of amino acids in health food by microwave hydrolysis-liquid chromatography tandem mass spectrometry. Methods Adding 15 mL 6 mol/L hydrochloric acid solution and appropriate amount of phenol to sample, it was hydrolyzed by microwave at 150 ℃ for 4 h, cooled to 80 ℃ and dried for 1 h under reduced pressure. The sample was dissolved in 0.1% formic acid and separated by Agilent-C18 column. The gradient elution was performed with acetonitrile-10 mmol/L ammonium acetate as the mobile phase. The sample was detected by multi-reaction monitoring mode of tandem mass spectrometry and quantified by external standard method. Results The linear range of the method was 0.01-0.05 nmol/μL; the average recovery was 95.6%-100.7%, and the relative standard deviation （RSD） was less than 3.0%. Conelusion This method is rapid, sensitive, accurate and repeatable. Comparing with the current technology, it is assisted by microwave hydrolysis to shorten the sample pretreatment time, which can be used for the simultaneous determination of 16 amino acids in health food.
作者
陈彩云
黎小兰
张喜金
蔡伟江
CHEN Cai-Yun;LI Xiao-Lan;ZHANG Xi-Jin;CAI Wei-Jiang(By-Health Co.,Ltd.,Zhuhai 519040,China)
出处
《食品安全质量检测学报》
CAS
2018年第17期4729-4733,共5页
Journal of Food Safety and Quality
关键词
微波水解
液相色谱-串联质谱法
保健品
氨基酸
microwave hydrolysis
liquid chromatography-tandem mass spectrometry
health food
amino acid
