Wang Jin, Liu Laping, Shi Ludi, Yi Tingquan, Wen Yuxia, Wang Juanli, Liu Shuhui
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.
J Sep Sci. 2017 Jan;40(2):480-487. doi: 10.1002/jssc.201600864. Epub 2016 Dec 20.
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.
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。