气相色谱质谱联用法测定酱油中的3-氯-1,2-丙二醇  

Gas chromatography mass spectrometry determination of 3-chloro-1, 2-propanediol in soy sauce

作　　者：赵雅松[1] 赵俊平 路勇[1] 吴颖[3] 黄华[1] 史娜[1] 

机构地区：[1]北京市食品安全监控中心,北京100041 [2]北京市食品质量监督检验二站,北京100050 [3]北京市产品质量监督检验所,北京100029

出　　处：《食品科技》2010年第10期283-286,共4页Food Science and Technology

摘　　要：采用气相色谱-质谱联用(GC-MS)法,快速测定酱油中3-氯-1,2-丙二醇(3-MCPD)的含量。采用柱层析预处理的方法,将试样与Extrelut拌匀、装柱,用正己烷与乙醚的混合溶液提取,经弗罗里硅土柱净化,再经三氟乙酸酐在55℃衍生30min后,用GC-MS测定食品中的3-MCPD含量。试验结果表明该方法准确、稳定,3-氯-1,2-丙二醇的添加范围在0.05～1mg/kg时,回收率为85%～95%,检出限为10μg/kg。该方法对前处理中的上样方式、衍生化时间、样品浓缩方法进行了探索比较,建立了有效的净化及衍生化方法,适用于酱油样品中3-MCPD含量的测定。Using gas chromatography mass spectrometry （GC-MS） method to determinate 3-chloro-1,2-pro-panediol （3-MCPD） of soysauce. We use column chromatography as the pre-treatment method to sample：mix Extrelut loaded column with n-hexane and ether solution, Florisil column purification. Then the sample was derivatives with trifluoro acetic anhydride at 55 ℃ for 30 min. The mixture was then injected into a gas chromatograph with a DB -5MS capillary column. We improve a better method of purification and derivatization, the former dealing with the kind of approach, derivatization time, sample concentration methods are explored.The experimental results show that this method is accurate and stable, when the range of 3- MCPD is in 0.05 ～1 mg/kg, recovery was 85%～95%, could reach the limit of quantitation of 10 μg/kg. The method is applied to soy sauce samples of 3-MCPD in the determination of residues.

关 键 词：3-氯-1 2-丙二醇 酱油 水解植物蛋白 

分 类 号：O657.63[理学—分析化学]