盐析辅助液液萃取-HPLC-MS/MS法检测液态乳中13种双酚类和烷基酚类物质  

Salting-out assisted liquid-liquid extraction coupled with HPLC-MS/MS for determination of 13 kinds of bisphenols and alkyl phenol compounds in liquid dairy products

作　　者：姜侃 张慧[2] 曹慧 王瑾 周学军 厉小燕 JIANG Kan;ZHANG Hui;CAO Hui;WANG Jin;ZHOU Xue-jun;LI Xiao-yan(Zhejiang Institute of Product Quality and Safety Science,Hangzhou,Zhejiang 310018,China;Zhejiang University of Science&Technology,Hangzhou,Zhejiang 310023,China)

机构地区：[1]浙江省产品质量安全科学研究院,浙江杭州310018 [2]浙江科技学院,浙江杭州310023

出　　处：《食品与机械》2022年第12期32-36,225,共6页Food and Machinery

基　　金：浙江省市场监督管理局NQI项目(编号:20200101);浙江省市场监督管理局科技项目(编号:20210101);浙江省基础公益研究计划(编号:LGN20C200011)。

摘　　要：目的:建立盐析辅助液液萃取-HPLC-MS/MS法同时检测液态乳中13种双酚类和烷基酚类化合物的方法。方法:采用盐析辅助液液萃取前处理方法,三重四极杆质谱负离子源多反应监测(MRM)模式下进行检测,基质外标法定量分析;研究萃取溶剂种类、盐析助剂的选择和用量对回收率的影响;并评估方法性能。结果:以乙腈为提取溶剂、0.4 g氯化钠为盐析助剂对液态乳进行液液萃取,13种酚类物质线性关系良好,相关系数均>0.99;牛奶和酸奶中的加标回收率分别为81.5%~118.1%和80.8%~107.6%,相对标准偏差分别为1.89%~12.3%和1.12%~11.9%;方法检出限为0.15~0.75μg/kg,定量限为0.5~2.5μg/kg。市售液态乳样品中有1个样品检出含有4-NP,含量为9.28μg/kg。结论:试验所建方法适合液态乳中13种双酚类和烷基酚类化合物的快速检测。Objective:An analytical method was established for determination of 13 kinds of bisphenols and alkylphenol compounds in liquid dairy products by salting-out-assisted liquid-liquid extraction coupled with HPLC-MS/MS.Methods:The salting-out-assisted liquid-liquid extraction pre-treatment method was adopted,and the detection was performed in the mode of negative ion source multiple reaction monitoring(MRM)by triple quadrupole mass spectrometry,and quantitative analysis was performed by matrix external standard method.Besides,the effect of extraction solvent type,selection and the usage of salting-out agents on the recoveries were studied and the performance of the method was evaluated.Results:The liquid dairy products were liquid-liquid extracted with acetonitrile as extraction solvent and 0.4 g sodium chloride as salting-out agents.The 13 kinds of phenols had a good linear relationship,and the correlation coefficients were all>0.99.The standard recovery rates of milk and yoghurt were 81.5% to 118.1% and 80.8% to 107.6%,respectively,and the relative standard deviations were 1.89% to 12.3% and 1.12% to 11.9%.The detection limits were 0.15 to 0.75μg/kg,and the quantification limits were 0.5 to 2.5μg/kg.One of the commercially available liquid dairy product was found to contain 4-NP,and the concentrations was 9.28μg/kg.Conclusion:The established method is suitable for the rapid detection of 13 kinds of bisphenols and alkylphenol compounds in liquid dairy products.

关 键 词：盐析 液液萃取 HPLC-MS/MS 液态乳 双酚类 烷基酚类 检测 

分 类 号：TS252.1[轻工技术与工程—农产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]