奶粉中饱和烃与芳香烃矿物油的高灵敏检测方法建立  

Development of A Highly Sensitive Method for the Determination of Mineral Oil Saturated Hydrocarbons(MOSH)and Aromatic Hydrocarbons(MOAH)in Milk Powder

作　　者：刘玲玲 李冰宁 杨梦奇 李婷 武彦文 LIU Lingling;LI Bingning;YANG Mengqi;LI Ting;WU Yanwen(Institute of Analysis and Testing,Beijing Academy of Science and Technology(Beijing Center for Physical and Chemical Analysis),Beijing 100094,China)

机构地区：[1]北京市科学技术研究院分析测试研究所(北京市理化分析测试中心),北京100094

出　　处：《食品工业科技》2023年第20期298-304,共7页Science and Technology of Food Industry

基　　金：北京市自然科学基金(青年项目)(6234043);北京市改革与发展专项(23CB017);北京市科学技术研究院北科萌芽计划(BGS202104)。

摘　　要：近年来,奶粉,特别是婴幼儿配方奶粉中的矿物油污染受到公众关注,相关国际监管逐渐升级。然而,目前还没有针对奶粉中矿物油的标准检测方法。本文依据欧盟的限量规定和分析要求,改进和优化了样品前处理方法,依次采用皂化法、正己烷提取、硅胶净化、环氧化反应方法,最后利用高效液相色谱-气相色谱联用技术(HPLC-GC)建立了奶粉中饱和烃矿物油(MOSH)和芳香烃矿物油(MOAH)的高灵敏检测方法。结果表明,该方法的定量限(LOQ)达到0.5 mg/kg,回收率为81.1%~112.0%(RSD=0.3%~3.8%),满足欧洲联合研究中心(JRC)的方法要求。应用该方法分析了国际能力验证样品,结果发现,C_(16)~C_(25)和C_(25)~C_(35)的MOSH和MOAH的检测结果均接近真值,其z'比分数的绝对值均小于2,说明方法通过验证,建议可参考本方法制定奶粉中MOSH和MOAH的含量检测标准。In recent years,contamination of mineral oil hydrocarbons(MOH)in milk powder,especially infant formula,has become a public concern,and related international regulation has gradually escalated.However,there is no standard method for the determination of MOH in milk powder.In this paper,the sample pretreatment method based on the EU limits and analytical requirements were improved and optimized,and the saponification method,hexane extraction,silica gel clean-up,epoxidation reaction method in order were used,and a highly sensitive method for the determination of mineral oils of saturated hydrocarbons(MOSH)and mineral oils of aromatic hydrocarbons(MOAH)in milk powder by on-line high performance liquid chromatography-gas chromatography(HPLC-GC)were established.Results showed that,the method achieved a limit of quantification(LOQ)of 0.5 mg/kg and recoveries of 81.1%~112.0%(RSD=0.3%~3.8%),meeting the method requirements of the European Joint Research Center(JRC).The method was applied to analyze the international proficiency testing samples,and the results showed the detection results of MOSH and MOAH from C_(16) to C_(25) and C_(25) to C_(35) were close to the true values,and the absolute values of their z'-scores were less than 2.This indicated that the method passed the validation,and the method could be referred to as the standard for the determination of MOSH and MOAH in milk powder.

关 键 词：奶粉 饱和烃矿物油(MOSH) 芳香烃矿物油(MOAH) 高灵敏检测 高效液相色谱- 气相色谱联用(HPLC-GC) 

分 类 号：TS295.4[轻工技术与工程—农产品加工及贮藏工程]