油脂类食品中脂肪酸单氯丙醇单酯和双酯的分离测定  

Separation and Determination of Fatty Acid Mono- and Diesters of Monochloropropane-1,2-diol in Fat-rich Foods

作　　者：傅武胜[1,6,7] 吴少明[2,7] 华娟[3] 吴永宁[4] 唐昌东[1] 方勤美[5] 

机构地区：[1]福建省人兽共患病研究重点实验室,福建省疾病预防控制中心,福州350001 [2]福建省产品质量检验研究院,福州350002 [3]福建农林大学食品科学学院,福州350002 [4]卫生部食品安全风险评估重点实验室,国家食品安全风险评估中心,北京100021 [5]福建省人兽共患病研究重点实验室,福建省疾病预防控制中心,福州350001 [6]福建省农科院生物技术研究所,福州350003 [7]食品安全分析与检测技术教育部重点实验室,福州大学,福州350108

出　　处：《分析化学》2014年第4期469-474,共6页Chinese Journal of Analytical Chemistry

基　　金：国家自然基金(No.81172671);卫生部公益性科研专项课题(No.200902009);福建省杰出青年基金(No.2011J06011);福建省医学创新课题(No.2011-CX-21);supported by the National Natural Science Foundation of China(No.81172671);by Medical Elite Cutivation Program of Fujian P.R.C

摘　　要：建立了食品中脂肪酸单氯丙醇单酯与双酯含量的测定方法.称取0.1g的油脂样品,加入内标后,转入氨基固相萃取柱,先以6.0 mL正己烷洗脱脂肪酸单氯丙醇双酯（MCPD双酯）,再以6.0 mL正己烷-乙酸乙酯混合溶剂洗脱脂肪酸单氯丙醇单酯（MCPD单酯）,分别收集洗脱液并浓缩至近干,残余物经甲醇钠水解和苯基硼酸（PBA）衍生后,供气相色谱/质谱（GC-MS）分析.MCPD单酯、MCPD双酯的检出限在83～142 μg/kg（均以MCPD计）之间,线性范围为25～ 500 μg/L（R2 ＞0.9990）.以花生油和婴幼儿奶粉脂肪提取物为基质,在250～ 1000 μg/kg范围内进行3种浓度水平的加标回收实验,MCPD单酯与双酯的回收率在86.5％～ 104.0％之间,相对标准偏差（RSD）为2.4％ ～ 13.2％ （n=6）.此外,本方法成功应用于市售食用植物油和婴幼儿奶粉中MCPD单、双酯的污染调查.Abstract A new method for the determination of fatty acid mono and diesters of monochloropropanediol （MCPD） was developed. The isotopically labelled standard solution was added to the sample solution and adsorbed on the aminopropyl column. Then MCPD diesters were eluted by 6.0 mL n-hexane and MCPD monoesters were eluted by a 6.0 ml mixture of n-hexane/ethylacetate （7： 3, V/V）. The concentratrated elution were hydrolyzed with methoxide and derivatizated with phenylboronic acid （PBA） before GC/MS analysis. The method was precise and sensitive, the limits of detection for MCPD monoesters and MCPD diesters were 83.0 μg/kg and 142 μg/kg, respectively. There was an excellent linear correlation （R2〉 0. 9990） in the range of 25-500 μg/L of MCPD monoesters ＆ diesters （calculated by MCPD）. The recovery rate of MCPD fatty acid esters spiked into edible oil and infant formula samples was in the range of 86.5% - 104.0%. The relative standard deviation （RSD） was from 2.4% to 13.2%. The method was successfully applied to the analysis of commercial edible oils and infant formula samples.

关 键 词：脂肪酸 3-氯-1 2-丙二醇单酯 3-氯-1 2-丙二醇双酯 2-氯-1 3-丙二醇单酯 2-氯-1 3-丙二醇双酯 食用植物油 奶粉 气相色谱-质谱法 固相萃取法 

分 类 号：O657.63[理学—分析化学] TS207.3[理学—化学]