1. 北京市农林科学院林业果树研究所
2. 农业部华北地区园艺作物生物学与种质创制重点实验室
3. 北京市落叶果树工程技术研究中心
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杨媛, 石磊, 杨军军, 等. 超高效液相色谱-质谱联用法测定草莓中鞣花酸[J]. 分析测试学报, 2016,35(12):1591-1595.
Determination of Ellagic Acid in Strawberry by UPLC-MS/MS[J]. 2016,35(12):1591-1595.
建立了测定草莓中鞣花酸含量(包括游离鞣花酸和总鞣花酸)的超高效液相色谱-质谱联用(UPLC-MS/MS)分析方法。草莓中游离鞣花酸在酸性条件下用甲醇提取,经C18分散固相萃取净化后可直接测定;总鞣花酸经酸性水解呈游离态再经分散固相萃取净化后进行测定。净化液经C18色谱柱分离,以甲醇和0.5%甲酸水为流动相进行梯度洗脱,电喷雾负离子(ESI-)模式电离,超高效液相色谱-质谱法(UPLC-MS/MS)测定,外标法定量。结果表明:在10~500 ng/mL浓度范围内鞣花酸的线性关系良好,相关系数为0.998 1,游离鞣花酸的定量下限为0.5 mg/kg,总鞣花酸的定量下限为5.0 mg/kg。在低、中、高3个加标浓度的回收实验中,游离鞣花酸的加标回收率为86.7%~113.6%,相对标准偏差均小于10%。该方法操作简单,灵敏度高,准确性好,适用于草莓中鞣花酸的测定。
A method was developed for the determination of ellagic acid(free ellagic acid and total ellagic acid) in strawberry by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).In this work,the free ellagic acid was extracted from strawberry with 0.1%trifloroacetric acid-methane,purified by C18 dispersive solid phase extraction,and determined by UPLC-MS/MS.Total ellagic acid was hydrolyzed to free ellagic acid with 2 mol/L trifloroacetric acid aqueous,then purified with C18 dispersive solid-phase extraction column,and determined by UPLC-MS/MS.Sample solution was separated on a C18 column by gradient elution using methanol-0.5%formic acid aqueous as mobile phase.The linear range of 10-500 ng/mL for ellagic acid was obtained,with correlation coefficient of 0.998 1.The limit of quantitation was 0.5 mg/kg for free ellagic acid and 5.0 mg/kg for total ellagic acid.The recoveries at low,medium and high spiked levels ranged from 867%to 1136%with relative standard deviations(RSD) not more than 10%.The results indicated that this approach was simple,sensitive and accurate,and was applicable for the determination of content of ellagic acid in strawberry.
超高效液相色谱-质谱联用法(UPLC-MS/MS)游离鞣花酸总鞣花酸草莓
ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)free ellagic acidtotal ellagic acidstrawberry
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