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离线固相萃取-大体积进样-气相色谱法分析市售植物油中的矿物油饱和烃

Offline Solid-phase Extraction Large-volume Injection-Gas chromatography for the Analysis of Mineral Oil-saturated Hydrocarbons in Commercial Vegetable Oils.

作者信息

Liu Lingling, Huang Hua, Wu Yanwen, Li Bingning, Ouyang Jie

机构信息

Beijing Center for Physical and Chemical Analysis, Beijing Food Safety Analysis and Testing Engineering Research Center.

Beijing Municipal Center for Food Safety Monitoring and Risk Assessment.

出版信息

J Oleo Sci. 2017 Sep 1;66(9):981-990. doi: 10.5650/jos.ess17081. Epub 2017 Aug 8.

Abstract

An offline solid-phase extraction (SPE) approach combined with a large-volume injection (LVI)-gas chromatography-flame ionization detector (LVI-GC-FID) is improved for routine analysis of mineral oil saturated hydrocarbons (MOSH) in vegetable oils. The key procedure of the method consists in using offline SPE columns for MOSH purification. The SPE column packed with 1% Ag-activated silica gel was used to separate MOSH from triglycerides and olefins in variety of vegetable oils. The eluent of MOSH fraction was only 3 mL and the concentration step was quick with little evaporation loss. The limit of quantification (LOQ) of the method was 2.5 mg/kg and the linearity ranged from 2 to 300 mg/kg. The accuracy was assessed by measuring the recoveries from spiked oil samples and was higher than 90%. Twenty-seven commercial vegetable oils were analyzed, and different levels of MOSH contamination were detected with the highest being 259.4 mg/kg. The results suggested that it is necessary to routinely detect mineral oil contamination in vegetable oils for food safety.

摘要

一种离线固相萃取(SPE)方法与大体积进样(LVI)-气相色谱-火焰离子化检测器(LVI-GC-FID)相结合,用于植物油中矿物油饱和烃(MOSH)的常规分析。该方法的关键步骤在于使用离线SPE柱对MOSH进行净化。填充1%银活化硅胶的SPE柱用于从各种植物油中的甘油三酯和烯烃中分离MOSH。MOSH馏分的洗脱液仅为3 mL,浓缩步骤快速且蒸发损失小。该方法的定量限(LOQ)为2.5 mg/kg,线性范围为2至300 mg/kg。通过测量加标油样的回收率评估准确性,回收率高于90%。分析了27种市售植物油,检测到不同水平的MOSH污染,最高为259.4 mg/kg。结果表明,为了食品安全,有必要对植物油中的矿物油污染进行常规检测。

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