气相色谱-质谱法测定黄酒中17种邻苯二甲酸酯的方法研究  

Study on the Determination of 17 Kinds of Phthalate Esters in Yellow Rice Wine by GC-MS

作　　者：宋海燕[1] 曾金红[1] 郑云峰[1] 江涛[1] 余燕飞[1] 林海娃[1] 黄晓丽[1] 李丹[1] 曾红燕[1] 

机构地区：[1]绍兴市质量技术监督检测院,国家黄酒产品质量监督检验中心,浙江绍兴312071

出　　处：《酿酒科技》2014年第4期89-92,共4页Liquor-Making Science & Technology

基　　金：浙江省质监系统科研计划项目(20120254):黄酒包装容器材料中邻苯二甲酸酯的检测与迁移规律的研究

摘　　要：采用改进的液一液萃取提取方法：样品在置于具塞试管中，于80℃水浴敞开加热20min，用正己烷萃取，微孔膜过滤，建立气相色谱一质谱（GC—MS）法测定黄酒中17种邻苯二甲酸酯类化合物的方法。该方法线性相关系数〉O．997．检出限为O．005-0．05mg／kg之间；在0．1mg／kg和1．0mg／kg添加水平时样品加标回收率为74．62％～103．35％，RSD（n=6）为2-36％～8．65％。并运用该方法对市售的黄酒进行了检测。结果表明，在62批陶坛盛装的黄酒样品中，有6批黄酒检出4种邻苯酸二甲酯类化合物，分别是邻苯二甲酸二甲酯（DMP）、邻苯二甲酸二丁酯（DBP）、邻苯二甲酸二异丁酯（DIBP）、邻苯二甲酸二辛酯（DEHP），它们的含量范围分别是：0．13～0．23mg／kg、0．04～0．21mg／kg、0．05～0．10mg／kg和0．03～0．39mg／kg。该方法灵敏度高，准确，抗干扰能力强，能同时测定黄酒中包括邻苯二甲酸二异壬酯（DINP）在内的17种邻苯二甲酸酯类化合物的含量。In this study, the improved liquid-liquid extraction method was adopted as follows： wine sample palced in a test tube, then 20 min heat- ing by 80℃water bathing, and hexane used for the extraction, and microporous membrane used for the filtration. Finally, GC-MS was used for the determination of 17 kinds ofphthalate esters. Under the above conditions, the linear relation coefficients were above 0.997, and the limits of detection （LOD） were in the range of 0.005-0.05 mg/kg, the average recoveries of the spiked samples （0. lmg/L andl.0 mg/L） were in the range of 74.62 %-103.35 % with RSDs （n = 6） between 2.36 %-8.65 %. The results showed that, among 62 pottery jars filled with rice wine, there were 4 kinds of PAEs detected in 6 batches office wine including dimethyl phthalate （DMP）, dibutyl phthalate （DBP）, phthalic acid diisobutyl （D1BP）, and phthalic acid di （2- ethylhexyl） phthalate （DEHP） with their content range as 0.13 -0.23 mg/kg,0.04-0.21 mg/kg,0.05 -0.10 mg/kg and 0103 -0.39 mg/kg respectively. Such detecting method had the advantages including high sensitivity, high accuracy, and strong anti-interfer- ence capacity. It could be used for simultaneous detection of the content of 17 kinds of PAEs （including DINP） in yellow rice wine.

关 键 词：黄酒 邻苯二甲酸酯 气相色谱一质谱 分析方法 

分 类 号：TS262.4[轻工技术与工程—发酵工程] TS261.4[轻工技术与工程—食品科学与工程]