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采用相转移催化剂辅助皂化和超分子溶剂微萃取结合高效液相色谱-荧光检测法测定食用油中的苯并[a]芘

Determination of benzo[a]pyrene in edible oils using phase-transfer-catalyst-assisted saponification and supramolecular solvent microextraction coupled to HPLC with fluorescence detection.

作者信息

Wang Jin, Liu Laping, Shi Ludi, Yi Tingquan, Wen Yuxia, Wang Juanli, Liu Shuhui

机构信息

Shaanxi Key Labotory of Natural Products & Chemical Biology, College of Science, Northwest A&F University, Yangling, Shaanxi, China.

College of Food Sciences and Engineering, Northwest A&F University, Yangling, Shaanxi, China.

出版信息

J Sep Sci. 2017 Jan;40(2):480-487. doi: 10.1002/jssc.201600864. Epub 2016 Dec 20.

DOI:10.1002/jssc.201600864
PMID:27862973
Abstract

For the analysis of edible oils, saponification is well known as a useful method for eliminating oil matrices. The conventional approach is conducted with alcoholic alkali; it consumes a large volume of organic solvents and impedes the retrieval of analytes by microextraction. In this study, a low-organic-solvent-consuming method has been developed for the analysis of benzo[a]pyrene in edible oils by high-performance liquid chromatography with fluorescence detection. Sample treatment involves aqueous alkaline saponification, assisted by a phase-transfer catalyst, and selective in situ extraction of the analyte with a supramolecular solvent. Comparison of the chromatograms of the oil extracts obtained by different microextraction methods showed that the supramolecular solvent has a better clean-up effect for the unsaponifiable matter from oil matrices. The method offered excellent linearity over a range of 0.03- 5.0 ng mL (r > 0.999). Recovery rates varied from 94 to 102% (RSDs <5.0%). The detection limit and quantification limit were 0.06 and 0.19 μg kg , respectively. The proposed method was applied for the analysis of 52 edible oils collected online in China; the analyte contents of 23 tested oil samples exceeded the maximum limit of 2 μg kg for benzo[a]pyrene set by the Commission Regulation of the European Union.

摘要

对于食用油分析而言,皂化作为一种消除油基质的有用方法广为人知。传统方法是使用碱醇进行;它消耗大量有机溶剂,并且阻碍通过微萃取回收分析物。在本研究中,开发了一种低有机溶剂消耗方法,用于通过高效液相色谱 - 荧光检测分析食用油中的苯并[a]芘。样品处理包括在相转移催化剂辅助下的碱性水溶液皂化,以及用超分子溶剂对分析物进行选择性原位萃取。通过不同微萃取方法获得的油提取物色谱图比较表明,超分子溶剂对油基质中的不皂化物具有更好的净化效果。该方法在0.03 - 5.0 ng/mL范围内具有出色的线性(r > 0.999)。回收率在94%至102%之间(相对标准偏差<5.0%)。检测限和定量限分别为0.06和0.19 μg/kg。所提出的方法应用于中国在线收集的52种食用油的分析;23个测试油样的分析物含量超过了欧盟委员会法规设定的苯并[a]芘2 μg/kg的最大限量。

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