超高效液相色谱-串联质谱法检测乳制品中18种邻苯二甲酸酯含量  

Determination on 18 phthalic acid esters(PAEs) in dairy by ulta performance liquid chromatography-tandem quadrupole mass spectrometry(UPLC-MS/MS)

作　　者：赵志红[1] 朱慧[1] 刘明[1] 李言郡[1] 张逢秋[1] 朱峰[1] 

机构地区：[1]杭州娃哈哈集团有限公司分析中心,杭州310018

出　　处：《食品科技》2014年第6期288-293,共6页Food Science and Technology

基　　金：杭州市社会发展专项课题(20120433B57)

摘　　要：建立超高效液相色谱-串联质谱法(UPLC-MS/MS)同时检测乳制品中18种邻苯二甲酸酯的方法。采用正己烷提取样品中邻苯二甲酸酯,Waters Acquilty UPLC BEH Cl8色谱柱(2.1 mm×100mm,1.7μm),0.1%甲酸水和0.1%甲酸乙腈流动相梯度洗脱程序下分离,电喷雾正电离,多反应监测模式测定,采用Waters PFCs Isolator kit消除分析系统背景干扰。在该优化方法条件下,l8种邻苯二甲酸酯中DEHP、DNOP、DNP、DINP及DIDP线性范围50～2000μg/L,其余13种线性范围5～200μg/L之间,定量限范围为1～500μg/kg,三水平加标方法回收率范围65.4%～110%,相对标准偏差(RSD)为1.9%～21%。应用该方法分析了乳制品中18种邻苯二甲酯含量,与国标气质方法相比,方法操作简单、快速,系统响应信号稳定,可以作为乳制品中18种邻苯二甲酸酯类化合物的检测方法。A quick confirming method was developed in this article to determine 18 phthalic acid esters （PAEs） in dairy by ulta performance liquid chromatography-tandem quadrupole mass spectrometry （UPLC-MS/MS）. Methods： PAEs in samples were extracted by n-hexane. UPLC-MS/MS method was achieved on Acquilty UPLC BEH C18 column （2.1 mm×100 mm, 1.7 μm）, the mobile phase consisted of acetonitrile with 0.1% formic acid （A）-0.1% formic acid solution （B） with gradient elution. Waters PFCs Isolator kit was used to eliminate the interference in background. The [M＋H]^＋ precursor ion of each component was detected in the positive ion mode. Results： With the optimized condition, the method was linear in the concentration range of 50-2000 μg/L for DEHP, DNOP, DIDP and DINP, The others 13 PAEs were 5-200 μg/L. The limits of quantification （LOQ） of the 18 PEAs were 1-500 μg/kg. The overall recovery of three levers varies from 65.4% to 110%, and the relative standard deviations （RSD） were between 1.9% and 21%. Conclusions： Compared with the national standard method GC-MS/MS, it was simple, rapid, accurate and feasible to determine phthalic acid esters in dairy.

关 键 词：超高效液相色谱-串联质谱法 乳制品 18种邻苯二甲酸酯 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程]