食品中矿物油分析方法的考察验证与结果确证  

Method validation and result confirmation for determination of mineral oil hydrocarbons in foods

作　　者：武彦文[1] 刘玲玲[1] 李冰宁[1] 欧阳杰[2] WU Yan-Wen;LIU Ling-Ling;LI Bing-Ning;OUYANG Jie(Beijing Center for Physical&Chemical Analysis,Beijing Food Safety Analysis and Testing Engineering Research Center,Beijing 100094,China;Department of Food Science and Engineering,College of Biological Sciences and Technology,Beijing Forestry University,Beijing 100083,China)

机构地区：[1]北京市理化分析测试中心,北京市食品安全测试工程技术研究中心,北京100094 [2]北京林业大学生物科学与技术学院食品科学与工程系,北京100083

出　　处：《食品安全质量检测学报》2020年第18期6281-6288,共8页Journal of Food Safety and Quality

基　　金：北京市自然科学基金项目(2182020);北京市科学技术研究院创新工程预研究项目(PXM2020_178305_000007)。

摘　　要：矿物油是指来源于石油和合成油的C10~C50烷烃(mineral oil saturated hydrocarbons,MOSH)和芳烃(mineral oil aromatic hydrocarbons, MOAH)物质的总称,其化学组成复杂。食品基质中含有多种矿物油干扰物,使得分析食品中的矿物油相当困难。通常,矿物油的分析步骤包括提取、净化分离和测定3个环节。为了保证分析方法的准确、可靠,样品中必须添加9个标准化合物(包括3个分离标记物、2个挥发损失标记物和2对定量内标物),用于监测矿物油的净化、分离与测定效果;同时需要经常插入空白实验和正构烷烃混合标准用于考察操作规范、试剂纯度、仪器性能等。由于矿物油与食品基质的复杂性,实际分析中还需要给出每类样品的定量限和回收率等方法学考察数据,以证明分析方法的灵敏度和准确性。对于部分干扰严重的样品,还需要采用全二维气相色谱-飞行时间质谱法进行分析结果的确证。本文结合食用油、奶粉、巧克力和大米等分析实例,综述了分析食品中矿物油的考察验证与结果确证方法。Mineral oil hydrocarbons in various foods refer to mineral oil saturated hydrocarbons(MOSH)and mineral oil aromatic hydrocarbons(MOAH)ranging from C10~C50 derived from petroleum and synthetic oils,which consist of a large quantity of chemical compounds with different types of structures.It is usually difficult to accurately determine MOSH and MOAH in variety of foods which contain many interferences of mineral oils.Generally,the procedures for determining MOSH and MOAH include extraction,purification,separation and detection.In order to ensure the reliability of the analytical method,9 standards,which usually consist of 3 separation markers,2 volatilization loss watchdogs and 2 pairs of quantitative internal standards,should be added to the samples for monitoring the performance of purification,separation and detection of MOSH and MOAH.Moreover,it is necessary to frequently determine blank samples and mixed standards of n-alkanes during sample analysis for inspecting the operation specification,reagent purity and instrument conditions of the whole analytical procedures.Since both the sources of mineral oils and interference in variety of foods are diverse,the method validation of quantitative limit,recovery rate and precision for determining certain kind of samples should be involved in order to prove the sensitivity and accuracy of the analysis method.Also the comprehensive two-dimensional gas chromatography hyphened with time-of-flight mass spectrometry is usually used to verify the determination results of samples with complex matrix interferences in particular.Based on the analytical examples of edible oil,milk powder,chocolate and rice,this paper fully described the method validation and verification for determining mineral oils in these foods.

关 键 词：矿物油 食品 混合标准物质 方法验证 结果确证 

分 类 号：TS207.3[轻工技术与工程—食品科学]