淀粉类食品中顺丁烯二酸的高效液相色谱测定方法  

Multi-target analysis of maleic acid in starch products by HPLC

作　　者：王丹[1] 方从容[1] 鲁杰[1] 周爽[1] 赵云峰[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

出　　处：《中国卫生检验杂志》2014年第14期1977-1979,1983,共4页Chinese Journal of Health Laboratory Technology

基　　金：质检总局公益性行业专项-食品中违禁成分精准判别及快速检测技术验证(2012104003-1)

摘　　要：目的建立测定淀粉类食品中顺丁烯二酸的高效液相色谱方法,并对部分市售淀粉类食品进行顺丁烯二酸污染排查。方法试样以50%甲醇溶液萃取,0.5 mol/L氢氧化钾皂化(必要时)后,以Platisil ODS C18柱分离,紫外检测器214 nm波长检测。结果方法线性范围0.1 mg/L^5.0 mg/L,定量限2 mg/kg。空白样品3个加标水平回收率在80%~110%之间,相对标准偏差均<3%。市售淀粉及淀粉制品的检测结果显示,顺丁烯二酸含量低于定量限。组织了5家实验室对检验方法进行了实验室间协同性验证,5个实验室的HORRAT评分<2.0。结论本文在建立淀粉类食品中顺丁烯二酸检测方法的同时,对可能干扰其检测的常见有机酸进行分离,避免顺丁烯二酸测定的干扰。方法操作简便,满足实验室间重现性要求;稳定可靠,适用于常规检测和大规模样品筛查。Objective To develop a HPLC method for determination of maleic acid in starch and starch related products, and investigate the maleic acid contamination in commercial starch products. Methods The test samples were extracted with 50% methanol, saponified with 0.5 mol/L potassium hydroxide（ if necessary）, then separated on Platisil ODSC18 column for HPLC analysis, and detected at 214 nm with UV detector. Results This method showed a linear range of 0. 1 mg/L - 5.0 mg/L. The sample LOQ was 2 mg/kg, with recoveries from 80% to 110% and RSD bellow 3%. The detection results of commercial starch and starch products showed the maleic acid content was less than the LOQ. Five laboratories were invited for inter- laboratory study, and the HORRAT value was less than 2.0. Conclusion Based on careful optimization, a HPLC method for surveillance of maleic acid in starch foods was successfully established, which also had avoided the interference of other organic acids. The simple operation and low requirement of instrument have made this method an ideal alternative for fast screening and routine analysis of starch products.

关 键 词：高效液相色谱法 顺丁烯二酸 淀粉类食品 

分 类 号：O657.72[理学—分析化学]