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食品研究与开发:2022,43(9):169-175
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超高效液相色谱-串联质谱法测定红美人中8种酚酸化合物
(台州市食品检验检测中心,浙江 台州 318000)
Determination of 8 Phenolic Acids in Hongmeiren by UPLC-MS/MS
(Taizhou Food Inspection Centre,Taizhou 318000,Zhejiang,China)
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投稿时间:2021-05-12    
中文摘要: 建立超高效液相色谱-串联质谱(ultra performance liquid chromatograph tandem mass spectrometry,UPLC-MS/MS)同时测定红美人中没食子酸、原尔茶酸、对羟基苯甲酸、绿原酸、香草酸、对香豆酸、阿魏酸、芥子酸8种酚酸化合物的方法,分析各酚酸在红美人中的组成和含量。选用2 mol/L氢氧化钠水解提取样品中游离型酚酸、游离酯型酚酸和结合酯型酚酸,提取液经固相萃取小柱净化后,采用Waters ACQUITY UPLC HSS T3色谱柱、乙腈/0.01%甲酸水流动相梯度分离,UPLC-MS/MS多反应监测模式进行测定,外标法定量。结果显示:8种酚酸在5 μg/L~5 000 μg/L浓度范围内线性关系良好(r≥0.999 1),检出限为 0.05 μg/L~0.73 μg/L,定量限为 0.17 μg/L~2.44 μg/L,回收率为 85.7%~103.9%,重复性为0.92%~5.28%。6个产地红美人中8种酚酸均有检出,总酚酸含量在68.82 μg/g~98.96 μg/g之间,其中阿魏酸含量最高,在 38.02 μg/g~53.79 μg/g之间,绿原酸含量次之,在 15.84 μg/g~25.90 μg/g 之间;各产地红美人中的酚酸组成比例基本稳定,其中阿魏酸占比均在51.10%~57.51%,绿原酸占比均在22.29%~27.86%。
Abstract:An ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was developed for simultaneous determination of gallic acid,protocatechuic acid,p-hydroxybenzoic acid,chlorogenic acid,vanillic acid,p-coumaric acid,ferulic acid,and sinapic acid in Hongmeiren.Furthermore,the distribution and proportions of all 8 phenolic acids in samples were analyzed.The 2 mol/L NaOH was used to hydrolyze the raw material for the extraction of phenolic acids(free,esters).The extract was then purified by solid-phase extraction column before being separated by Waters ACQUITY UPLC HSS T3 column with mobile phase of acetonitrile-0.01% formic acid solution.They were then determined by UPLC-MS/MS in multiple reaction monitoring(MRM)mode and quantified with the external standard method.The results indicated that all 8phenolic acidshad good linearity(r≥ 0.9991)within concentration range of 5 μg/L-5 000 μg/L,with the detection limits of 0.05 μg/L-0.73 μg/L and quantification limits of 0.17 μg/L-2.44 μg/L.The recoveries were 85.7%-103.9%,and the repeatabilitys were in the range of 0.92%-5.28%.All the 8 phenolic acids were detected in Hongmeiren of 6 origins,and the content of total phenolic acids was in the range of 68.82 μg/g-98.96 μg/g.Among them,the content ferulic acid was the highest(38.02 μg/g-53.79 μg/g),followed by chlorogenic acid (15.84 μg/g-25.90 μg/g).The proportions of phenolic acids were stable among samples of different origins.The proportions of ferulic acid chlorogenic acid in the total phenolic acids were 51.10%-57.51%and 22.29%-27.86%,respectively.
文章编号:202209023     中图分类号:    文献标志码:
基金项目:台州市科技计划项目(1901ny06)
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