Department of Analytical Chemistry, Institute of Fine Chemistry and Nanochemistry, University of Cordoba, Edificio Anexo Marie Curie, Campus de Rabanales, 14071 Córdoba, Spain.
Department of Analytical Chemistry, Institute of Fine Chemistry and Nanochemistry, University of Cordoba, Edificio Anexo Marie Curie, Campus de Rabanales, 14071 Córdoba, Spain.
J Chromatogr A. 2014 Apr 4;1336:23-33. doi: 10.1016/j.chroma.2014.02.008. Epub 2014 Feb 14.
We report herein a multiresidue method for canned food determination of 12 bisphenols [bisphenol A (BPA), bisphenol B (BPB), bisphenol F (BPF), bisphenol E (BPE)], bisphenol diglycidyl ethers [bisphenol F diglycidyl ether (BFDGE), bisphenol A diglycidyl ether (BADGE)] and their derivatives [BADGE·2H2O, BADGE·H2O, BADGE·HCl·H2O, BADGE·HCl, BADGE·2HCl and BFDGE·2HCl]. The method was based on the microextraction of the target contaminants in 200mg food sample with 600 μL of a supramolecular solvent made up of inverse aggregates of tetradecanol, followed by analysis of the extract by liquid chromatography/fluorescence detection using external calibration. Chromatographic separation of all target compounds, including the ortho-ortho, ortho-para and para-para isomers of BFDGE and BFDGE·2HCl, was achieved with baseline separation (Resolution ≥ 1.52). No concentration of the extracts was required, the microextraction took about 30 min and several samples could be simultaneous treated. Method validation was carried out according to the recommendations of the European Commission Decision 2002/657/EC. Quantitation limits for the different analytes ranged between 0.9 and 3.5 μg kg(-1). Repeatability and reproducibility, expressed as relative standard deviation, were in the ranges 1.8-6.8% and 4.4-8.1%. The method was applied to the analysis of the target compounds in different food categories including vegetables, legumes, fruits, fish and seafood, meat product and grain. Recoveries in samples were within the range 80-110%. Only BPF and BPE were undetected in the canned food analyzed. The concentration found for the rest of bisphenols, diglycidyl ethers and derivatives was in the range 7.1-959 μg kg(-1). The study of the isomeric distribution of BFDGE and BFDGE·2HCl in food showed that they are preferentially present as one of the isomeric forms, that highlighting for further studies. The analytical and operational characteristics of this multiresidue method make it suitable for monitoring programs intended for the assessment of human exposure to bisphenols, diglycidyl ethers and derivatives from diet.
我们在此报告了一种用于罐装食品中 12 种双酚（双酚 A（BPA）、双酚 B（BPB）、双酚 F（BPF）、双酚 E（BPE））、双酚二缩水甘油醚（双酚 F 二缩水甘油醚（BFDGE）、双酚 A 二缩水甘油醚（BADGE））及其衍生物[BADGE·2H2O、BADGE·H2O、BADGE·HCl·H2O、BADGE·HCl、BADGE·2HCl 和 BFDGE·2HCl]的多残留分析方法。该方法基于在 200mg 食品样品中用 600μL 由十四烷醇形成的超分子溶剂微萃取目标污染物，然后通过使用外部校准的液相色谱/荧光检测分析提取物。所有目标化合物的色谱分离，包括 BFDGE 和 BFDGE·2HCl 的邻-邻、邻-对和对-对异构体，均实现了基线分离（分辨率≥1.52）。无需对提取物进行浓缩，微萃取耗时约 30 分钟，可同时处理多个样品。方法验证按照欧洲委员会第 2002/657/EC 号决定的建议进行。不同分析物的定量限在 0.9 至 3.5μgkg(-1)之间。重复性和再现性（表示为相对标准偏差）在 1.8-6.8%和 4.4-8.1%之间。该方法应用于不同食品类别（包括蔬菜、豆类、水果、鱼和海鲜、肉类产品和谷物）中目标化合物的分析。样品中的回收率在 80-110%范围内。在分析的罐装食品中仅未检出 BPF 和 BPE。其余双酚、二缩水甘油醚及其衍生物的浓度在 7.1-959μgkg(-1)之间。对 BFDGE 和 BFDGE·2HCl 的异构体分布研究表明，它们优先以一种异构体形式存在，这突显了进一步研究的必要性。该多残留方法的分析和操作特性使其适用于监测计划，旨在评估饮食中双酚、二缩水甘油醚及其衍生物对人体的暴露情况。
