文献类型：期刊文献

中文题名：超高效液相色谱-串联四极杆质谱法测定葡萄中单咖啡酰酒石酸酯、单香豆酰酒石酸酯和单阿魏酰酒石酸酯

英文题名：Determination of caftaric acid,p-coutaric acid and fertaric acid in grape juice,peel and seeds by ultra-high performance liquid chromatography-tandem quadrupole mass spectrometry

作者：张凌怡[1];王智聪[1];张维冰[1]

机构：[1]华东理工大学化学与分子工程学院,上海200237

年份：2013

卷号：31

期号：2

起止页码：122

中文期刊名：色谱

外文期刊名：Chinese Journal of Chromatography

收录：CSTPCD;;Scopus;WOS:【ESCI(收录号:WOS:000434513300006)】；北大核心:【北大核心2011】；CSCD:【CSCD2013_2014】；PubMed;

基金：国家青年科学基金项目(21105027)

语种：中文

中文关键词：超高效液相色谱-串联质谱;羟基桂皮酒石酰酯;单咖啡酰酒石酸酯;单香豆酰酒石酸酯;单阿魏酰酒石酸酯;葡萄汁;葡萄皮;葡萄籽

外文关键词：ultra-high performanceMS/MS） ; hydroxycinnamoyltartaricjuice; grape peel; grape seedliquid chromatography-tandem mass spectrometry （UPLC-esters ; caftaric acid; p-coutaric acid; fertaric acid; grape

摘要：建立了超高效液相色谱-串联四极杆质谱测定葡萄汁、皮和籽中羟基桂皮酒石酰酯类化合物含量的方法。采用的色谱柱为Waters UPLC HSS T3(150 mm×2.1 mm,1.7μm),流动相为含0.1%甲酸的水-乙腈体系,梯度洗脱,流速0.3 mL/min,柱温35℃;质谱采用电喷雾离子源、负离子多反应检测模式。对单香豆酰酒石酸酯和单阿魏酰酒石酸酯,其含量以单咖啡酰酒石酸酯当量表示。结果表明,单咖啡酰酒石酸酯在25～2 000μg/L范围内线性关系良好(r2=0.998 9);检出限为0.25μg/L,定量限为25μg/L;在250、750、1 200μg/L添加水平下单咖啡酰酒石酸酯的平均回收率为97.7%～99.5%,相对标准偏差小于2.5%。实验结果表明,葡萄汁、皮和籽中羟基桂皮酒石酰酯类化合物的含量差异显著。该方法简单快速、灵敏度高、回收率高、准确性好,可用于葡萄产品中单咖啡酰酒石酸酯、单香豆酰酒石酸酯和单阿魏酰酒石酸酯的分析。
An ultra-high performance liquid chromatography-tandem quadrupole mass spectrometry （UPLC-MS/MS） method was developed for the determination of hydroxycinnamoyltartaric esters, such as caftaric acid, p-coutaric acid and fertaric acid in grape juice, peel and seed. The target analytes were separated on a Waters UPLC HSS T3 column （ 150 mm x 2. l mm, 1.7μm） at 35 .C with gradient elution at a flow rate of 0.3 mL/min. The grape juice was freeze-centrifuged, the supernatant was diluted with 20% methanol. The grape peel and grape seed samples were extracted with 80% ethanol. The extract was cleaned-up on-line with the analytical column by valve switching technology. The mobile phases were water-acetonitrile （both containing 0. 1% formic acid）. The identification and quantification were achieved by MS/MS in multiple reaction monitoring （MRM） mode via negative electrospray ionization. As lack of commercial standards, p-coutaric acid and feraric acid were quantified by caftaric acid equivalent. The developed method showed a good linearity over the range of 25 -2 000μg/L with good correlation coefficient （r2 = 0. 998 9）. The limit of detection was 0.25 μg/L, and the limit of quantification was 25 μg/L. The average recoveries of eaftaric acid were between 97.7% - 99.5% and the precisions were within 2.5% at the spiked levels of 250, 750 and l 200μg/L. The working solutions were stable for 74 h at room temperature. The results showed that there are significant differences of hydroxycinnamoyltartaric esters distribution in grape juice, peel and seeds. Therefore, this method, owing to its simplicity, rapidity, good recovery, high sensitivity and accuracy, can be used for the analysis of caftaric acid, p-coutaric acid and fertaric acid in grape juice, peel and seeds.