河北工业科技2017,Vol.34Issue(6):428-433,6.DOI:10.7535/hbgykj.2017yx06007
LC-MS-MS法测定葡萄中的脱落酸含量
Analysis of abscisic acid content in grape by LC-MS-MS
摘要
Abstract
Grape contains much sugar,pigment and pectin,which has interference and makes it difficult for quantitative analy-sis of trace abscisic acid.To solve this problem,LC-MS-MS method for the determination of abscisic acid in grape is estab-lished.Several key aspects including extractant,extract methods,enrichment,chromatographic conditions and mass spectrom-etry are studied.The test sample is prepared through pulverization and homogenate of grape sample,and analyzed with metha-nol + formic acid (V/V=99.5/0.5)as the extractant,after oscillation extraction for 30 min,and with MAX Cartridge SPE as the enrichment and purification extractant.The research shows that the elution efficiency is better and the impurities can be removed effectively when the solvent is methanol of 20%~50%(mass fraction);the chromatographic condition is of ODS2 (2.1 mm×150 mm,5μm)column,acetonitrile as the phase A,0.1% formic acid as mobile phase B,flow rate at 0.2 mL/min, and gradient elution is performed;263.1~153.2 is used as the qualitative-quantitative ion pair in the negative ion monitoring mode,the samples are characterized by the retention time and the SRM atlas,and the external standard method is quantified by the peak area.The method has a calibration curves of good linearity over the range from 19.05 to 381.00 ng/mL.The recovery rate is 92.2%~110.4%,and RSD is less than 8.1%.This research provides an efficient and accurate method for the determina-tion of abscisic acid in grapes.关键词
食品检验学/LC-MS-MS法/测定/葡萄/脱落酸含量Key words
food inspection/LC-MS-MS/analysis/grape/ABA(abscisic acid)content分类
农业科技引用本文复制引用
孙震,任瑞,李增良,毕波..LC-MS-MS法测定葡萄中的脱落酸含量[J].河北工业科技,2017,34(6):428-433,6.基金项目
河北省科技计划项目(14225503D) (14225503D)