LC-MS/MS测定风味发酵乳中的矢车菊素-3-葡萄糖苷和矢车菊素-3-芸香糖苷  

Analysis of Cyanidin-3-glucoside and Cyanidin-3-rutinoside in Flavored Fermented Milk Using LC-MS/MS

作　　者：李丽[1] Li Li(Zhenjiang Vocational Technology School,Zhenjiang Branch of Jiangsu Union Vocational Technical Institute,Jiangsu,212000)

机构地区：[1]江苏联合职业技术学院镇江分院镇江高等职业技术学校,江苏212000

出　　处：《当代化工研究》2021年第24期1-4,共4页Modern Chemical Research

基　　金：“江苏高校‘青蓝工程’资助”(苏教师2019[3])。

摘　　要：目的:建立了风味发酵乳中矢车菊素-3-葡萄糖苷(Cyanidin-3-glucoside,C3G)和矢车菊素-3-芸香糖苷(Cyanidin-3-rutinoside,C3R)的液相色谱串联质谱检测方法(Liquid Chromatography Tandem Mass Spectrometry,LC-MS/MS)。方法:样品经三氯乙酸去除蛋白后,再用冷冻离心和正己烷去除脂肪。待测组分经Poly-Sery MCX固相萃取柱净化,采用多反应监测(MRM)模式进行检测,外标法定量。结果:目标化合物在一定范围内(3.12μg/L~100μg/L)线性关系良好,相关系数(R^(2))均大于0.995。样品中上述两种待测组分的定量限(LOQ)和检出限(LOD)均分别为5.00μg/kg、2.50μg/kg。不同加标浓度样品5.00μg/kg(LOQ)、10.0μg/kg(2×LOQ)、 50.0μg/kg(10×LOQ),C3G的加标回收率为103%~115%,相对标准偏差(RSDs)为4.17%~5.88%;C3R的加标回收率为105%~119%,相对标准偏差(RSDs)为5.32%~6.07%。8份市售发酵乳中均未检出这两种化合物。结论:该方法确认参数均能满足相关的技术规范的要求,为风味发酵乳中C3G和C3R的定性定量测定提供了技术支撑。Objective:Analytical method for Cyanidin-3-glucoside and Cyanidin-3-rutinoside in flavored fermented milk using LC-MS/MS has been accomplished.Methods:Protein in sample was precipitated with trichloroacetic acid solution.Oil and fat contained in sample was eliminated using refrigerated centrifugation and n-hexane.After further purification with Poly-Sery MCX solid-phase extraction column,the analytes were analyzed by LC-MS/MS in multi-reaction monitoring model and quantified by external standard method.Results:The calibration curve showed good linearity in the certain range (3.12 μg/L-100 μg/L) with the correlation coefficients greater than 0.995(R^(2)).The limit of quantification (LOQ) and detection (LOD) for both substances is 5.00 μg/kg and 2.50 μg/kg,respectively.As to three spiked levels,i.e.5.00 μg/kg(LOQ)、10.0 μg/kg(2×LOQ) and 50.0 μg/kg(10×LOQ),the average recoveries fell into 103%~115%(n=6) with RSDs of 4.17%~5.88% for C3G;105%~119% and 5.32%~6.07% for C3R respectively.Conclusion:This method’s validation parameters meet technological requirements.which can give technical support to qualitative and quantitative determination of C3G and C3R in flavored fermented milk.

关 键 词：液相色谱串联质谱仪 矢车菊素-3-葡萄糖苷 矢车菊素-3-芸香糖苷 风味发酵乳 

分 类 号：TQ[化学工程]