GC-MS面积比法测定食用植物油中3-氯丙醇酯的研究  

Determination of 3-MCPD esters in edible vegetable oil by GC-MS with area ratio method

作　　者：黄翠莉[1,2] 王天明[3] 杨宁[4] 王力清[1,2] 王瑛瑶[4] 吴炜亮[1,2] 

机构地区：[1]广东产品质量监督检验研究院,广东佛山528300 [2]国家食品质量监督检验中心(广东),广东佛山528300 [3]郑州轻工业学院,郑州450002 [4]国家粮食局科学研究院,北京100037

出　　处：《中国油脂》2015年第11期74-78,共5页China Oils and Fats

基　　金：国家粮食公益性行业科研专项(201313011-7)

摘　　要：建立了以d5-3-氯-1,2-棕榈酸二酯为内标物,面积比法定量测定食用植物油中3-氯-1,2-丙二醇酯(3-MCPD酯)的气相色谱-质谱检测方法。样品加内标后经甲基叔丁基醚溶解,与甲醇钠-甲醇溶液酯交换反应4 min后加酸性溴化钠终止反应。使用液液萃取法进行萃取后,加0.2 m L苯基硼酸于45℃下衍生20 min,进气相色谱-质谱检测。结果表明:该方法操作简单、灵敏度高,最低检出限为10μg/kg。利用该方法研究了不同植物油精炼过程和冷冻储存时间对3-MCPD酯含量的影响,试验表明脱臭工段是产生3-MCPD酯的主要来源,随着植物油储存时间的延长3-MCPD酯含量呈降低趋势。A gas chromatography - mass spectrometry （ GC - MS） analysis method was developed for deter- mination of fatty acid esters of 3 -chloro- 1,2 -propane diol （3 -MCPD esters） in edible vegetable oil employing area ratio method for quantitative measurement. Samples were dissolved in methyl tert - butyl ether after addition of internal standard d5 - 3 - chloro - 1,2 - dipalmitate. Then the samples were trans- esterified with sodium methoxide methanol solution for 4 min and the reaction was terminated by acidic so- dium bromide. The transesterification products had a derivatization reaction with 0.2 mL phenylboric acid at 45 ℃ for 20 min after liquid - liquid extraction, then the specimens were determined by GC - MS. The results showed that the method had the items of high sensitiveness and simple operation, and the limit of detection was 10 p,g/kg. The effects of refining process and freezing storage time of different vegetable oils on the content of 3 -MCPD esters were investigated. The results demonstrated that the generation of 3 -MCPD esters mainly came from deodorization section, but it had a decrease with the storage time prolonging.

关 键 词：3-MCPD酯 面积比法 食用植物油 气相色谱-质谱 

分 类 号：O657.63[理学—分析化学] TS227[理学—化学]