高效液相色谱测定牛奶中邻苯二甲酸酯的方法研究  

Determination of Phthalic Acid Esters in Milk by High Performance Liquid Chromatography

作　　者：徐向华[1] 方晓明[2] 丁卓平[1] 陶宁萍[1] 李文斌 

机构地区：[1]上海海洋大学食品学院,上海200090 [2]上海出入境检验检疫局,上海200135 [3]迪马公司,天津300400

出　　处：《化学通报》2008年第6期420-424,共5页Chemistry

基　　金：上海市科学技术委员会科研计划项目(06DZ05133);上海市重点学科建设项目(T1102)资助

摘　　要：建立了针对欧盟指令2007／19／EC中禁止与食品接触的6种邻苯二甲酸酯（BBP、DBP、DEHP、DNOP、DINP和DIDP）的RP-HPLC测定方法。样品用甲醇、正己烷-甲基叔丁基醚（VIV=1：1）提取，经冷冻去脂、液液萃取和硅胶固相萃取净化后，用ODS柱（250×4．6mm，5μm）分离，UV224nm检测。结果表明，BBP和DBP在0．05～80μg／mL、DEHP和DNOP在0．1～80μg／mL、DINP和DIDP在0．5～80μg／mL的质量浓度范围内，峰面积与质量浓度呈线性关系，相关系数（r^2）均大于0．998。方法检测限分别为：BBP0．15μg／g、DBP 0．1μg／g、DEHP和DNOP 0．2μg／g、DINP和DIDP 0．6μg／g；6种PAEs的添加量在最大残留限量值的0．2、1和2倍时，其平均回收率为80．7％～102．3％，相对标准偏差为1．7％～9．0％。所建立的方法经济、准确、可靠，满足欧盟指令中6种邻苯二甲酸酯限量的检测要求。The high-performance liquid chromatographic method was developed for the determination of six phthalic acid esters （PAEs） in milk, including BBP, DBP, DEHP, DNOP, DINP and DIDP, which are banned in 2007/19/EC. The PAEs were extracted with methanol and hexane/methyl t-butyl ether （ V/V = 1 ： 1 ）, the fat was removed by cryoapplication. Extracts were purified by LLE and silica SPE cartridge. Separation was carded on ODS column （250 × 4.6mm, 5 /μm） coupled with UV detection at 224nm. The linear range was over 0.05 - 80μg/mL for BBP and DBP, 0.1 80μg/mL for DEHP and DNOP, 0.5 - 80μg/mL for DINP and DIDP （ r^2 〉 0.998）. The detection limits were： BBP 0.15μg/g, DBP 0.1μg/g, DEHP and DNOP 0.2μg/g, DINP and DIDP 0.6μg/g, respectively. The assay was validated by analyzing samples spiked with 0.2, 1, 2 fold of MRL, the average recoveries and the relative standard deviations were in the range of 80.7% - 102.3% and 1.7% - 9.0% . The method is economic, accurate and reliable, which meets the criteria of European Union Commission Directive 2007/19/EC.

关 键 词：高效液相色谱 牛奶 邻苯二甲酸酯 增塑剂 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程]