固相支持液液萃取-气相色谱-质谱法测定膳食样品中氯丙二醇酯  

Determination of fatty acid esters of chloropropanediols in diet samples by gas chromatography-mass spectrometry coupled with solid-supported liquid-liquid extraction

作　　者：高洁[1] 刘卿[1] 韩枫[2] 苗虹[1] 赵云峰[1] 吴永宁[1] 

机构地区：[1]国家食品安全风险评估中心卫生部食品安全风险评估重点实验室,北京100021 [2]中国疾病预防控制中心营养与食品安全所

出　　处：《卫生研究》2014年第3期449-454,共6页Journal of Hygiene Research

基　　金："十二五"国家科技支撑计划课题(No.2012BAK01B01)

摘　　要：目的建立膳食样品中3-氯-1—2-丙二醇（3-MCPD）酯和2．氯．1，3-丙二醇（2-MCPD）酯的固相支持液液萃取-气相色谱-质谱（SLE-GC-MS）检测方法。方法膳食样品经正己烷超声提取，用甲醇钠／甲醇水解后，以硅藻土作为吸附剂进行固相支持液液萃取净化，经七氟丁酰咪唑衍生后，进行GC．MS测定，采用氘代同位素标准进行内标法定量。结果3-MCPD酯和2-MCPD酯在不同膳食样品中的检出限分别为0．002～0．005mg／kg和0．002～0．006mg／kg，膳食样品中3-MCPD酯和2-MCPD酯在0．05mg／kg和0．1mg／kg水平的加标回收率分别为65．9％～104．2％和75．4％-118．0％，相对标准偏差分别为2．2％～14．2％和0．8％～13．9％。结论该方法简便、准确、可靠，适用于膳食样品中3-MCPD酯和2-MCPD酯的检测。Objective To establish a method for the determination of fatty acid esters of 3-monochloropropane-1, 2-diol （ 3-MCPD ） and 2-monochloropropane-1, 3-diol （2-MCPD） in diet samples by gas chromatography-mass spectrometry （GC-MS）with solid- supported liquid-liquid extraction （SLE）. Methods Diet samples were ultrasonically extracted by hexane, followed by ester cleavage reaction with sodium methylate in methanol, and then purified by solid-supported liquid-liquid extraction. （SLE） using diatomaceous earth as the sorbent. After derivatization with heptafluorobutyrylimidazole, the analytes were detected by GC-MS and quantified by the deuterated internal standards. Results The limits of detection （LODs） of 3-MCPD esters and 2-MCPD esters in different diet samples were 0. 002 -0. 005 mg/kg and 0. 002 -0. 006 mg/kg. The average recoveries of 3-MCPD esters and 2-MCPD esters at the spiking levels of 0.05 and 0. 1 mg/kg in the diet samples were in the range of 65.9% - 104.2% and 75.4% - 118.0%, respectively, with the relative standard deviations in the range of 2.2% - 14.2% and 0. 8% -13.9%. Conclusion The method is simple, accurate and rugged for the determination of fattyacid esters of 3-MCPD and 2-MCPD in diet samples.

关 键 词：氯丙二醇酯 膳食样品 固相支持液液萃取 气相色谱-质谱 

分 类 号：TS201.5[轻工技术与工程—食品科学] R155.51[轻工技术与工程—食品科学与工程]