色谱2013，Vol.31Issue(2)：122-126,5.DOI:10.3724/SP.J.1123.2012.09047
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
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
摘要
Abstract
An ultra-high performance liquid chromatography-tandem quadrupole mass spec-trometry (UPLC-MS/MS) method was developed for the determination of hydroxycinnamoyltar-taric 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 × 2. 1 mm, 1. 7 μm) at 35 ℃ 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 fertaric acid were quantified by caftaric acid equivalent. The developed method showed a good linearity over the range of 25 - 2 000 μg/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 caftaric acid were between 97. 7% -99. 5% and the precisions were within 2. 5% at the spiked levels of 250, 750 and 1 200 μg/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.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Key words
ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)/ hydroxycinnamoyltartaric esters/ caftaric acid/ p-coutaric acid/ fertaric acid/ grape juice/ grape peel/ grape seed分类
化学化工引用本文复制引用
张凌怡,王智聪,张维冰..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[J].色谱,2013,31(2):122-126,5.基金项目
国家青年科学基金项目(21105027). （21105027）
