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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
  • ISSN号:1000-8713
  • 期刊名称:色谱
  • 时间:2013.2.28
  • 页码:122-126
  • 分类:O658[理学—分析化学;理学—化学]
  • 作者机构:[1]华东理工大学化学与分子工程学院,上海200237
  • 相关基金:国家青年科学基金项目(21105027).
  • 相关项目:双酶孔径梯度杂化整体蛋白质在线酶反应器研究
中文摘要:

建立了高效液相色谱-串联四极杆质谱法测定葡萄汁、皮和籽中羟基桂皮酒石酸酯酰酯类化合物含量的方法。采用的色谱柱为Waters UPLC HSS T3(150mm×2.1mm,1.7μm),流动相为含0.1%甲酸的水-乙腈体系,梯度洗脱,流速0.3mL/min,柱温35℃;质谱采用电喷雾离子源、负离予多反应检测模式。对单香豆酰酯“酸酯和单阿魏酰酒石酸酯,其含量以单咖啡酰酒石酸酯当最表示。结果表明,单咖啡酰酒石酸酯在25-2000μg/L范围内线性关系良好(r2=0.9989);检出限为0.25μg/L,定量限为25μg/L;在250、750、1200μg/L添加水平下单咖啡酰酒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酒石酸酯类化合物的含量差异显著。该方法简单快速、必敏度高、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。

英文摘要:

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.

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期刊信息
  • 《色谱》
  • 北大核心期刊(2011版)
  • 主管单位:中国科学技术协会
  • 主办单位:中国化学会 中国科学院大连化学物理研究所
  • 主编:张玉奎
  • 地址:大连市中山路457号
  • 邮编:116023
  • 邮箱:sepu@dicp.ac.cn
  • 电话:0411-84379021
  • 国际标准刊号:ISSN:1000-8713
  • 国内统一刊号:ISSN:21-1185/O6
  • 邮发代号:8-43
  • 获奖情况:
  • 1998年获中国科学院科学出版基金择优支持(1998-2...,2001年获第四届中国科学院优秀期刊二等奖,2002年获第三届中国科协优秀期刊三等奖,连续多年被评为辽宁省一级期刊
  • 国内外数据库收录:
  • 俄罗斯文摘杂志,美国化学文摘(网络版),波兰哥白尼索引,荷兰文摘与引文数据库,美国生物医学检索系统,美国剑桥科学文摘,日本日本科学技术振兴机构数据库,中国中国科技核心期刊,中国北大核心期刊(2004版),中国北大核心期刊(2008版),中国北大核心期刊(2011版),中国北大核心期刊(2014版),英国英国皇家化学学会文摘,中国北大核心期刊(2000版)
  • 被引量:26730