植物油基鱼罐头中矿物油污染物高灵敏检测方法的建立

Establishment of Highly Sensitive Determination Method for Mineral Oil Contaminants in Vegetable Oil-based Canned Fish Products

本文建立了植物油基鱼罐头中矿物油(MOH)的高灵敏测定方法并调查了部分市售商品的MOH含量。方法采用皂化反应、环氧化反应进行提取和净化,以高效液相色谱-气相色谱联用法(HPLC-GC)分级、富集和定量检测。结果表明:所建立的植物油基鱼罐头中饱和烃矿物油(MOSH)和芳香烃矿物油(MOAH)测定方法的定量限(LOQ)为0.5 mg/kg,加标回收率为90.0%~106.0%,精密度(RSD)为1.6%~12.7%,满足欧洲联合研究中心(JRC)关于高油脂食品中矿物油的分析要求。应用该方法检测了北京地区10个市售鱼罐头产品,发现所有样品均含有MOSH,含量为2.6~53.7 mg/kg,其中5个检出MOAH,含量为0.7~5.5 mg/kg;谱图分析表明这些罐头的MOH污染与其植物油和鱼肉来源密切相关。

A method for the high-sensitive determination of mineral oil hydrocarbons(MOH) in vegetable oil-based canned fish was established, and applied in some commercial products. The samples were extracted and purified by saponification and epoxidation, and were fractionated, concentrated and quantitatively determined by on-line high performance liquid chromatography coupled with gas chromatography(HPLC-GC) for mineral oil saturated hydrocarbons(MOSH) and mineral oil aromatic hydrocarbons(MOAH). The results showed that the limit of quantification(LOQ) of the method was 0.5 mg/kg and the spiked recovery was 90.0%~106.0%, and the precision(RSD) was 1.6%~12.7%, which met the requirements of the European Joint Research Center(JRC) for the analysis of MOH in the higher-fat/oil-content foods. This method was applied to detect ten canned fish products sold in Beijing. It was found that all of those contained MOSH with contents of 2.6~53.7 mg/kg, of which five detected MOAH with a content of 0.7~5.5 mg/kg. The MOH chromatographic profiles indicated that the contaminants were closely related to the sources of the vegetable oils and fish meat in those products.