REQUIMTE, Laboratory of Bromatology and Hydrology, Faculty of Pharmacy, University of Porto, Porto, Portugal.
Anal Bioanal Chem. 2012 Nov;404(8):2453-63. doi: 10.1007/s00216-012-6389-5. Epub 2012 Sep 21.
A new simple and reliable method combining an acetonitrile partitioning extractive procedure followed by dispersive solid-phase cleanup (QuEChERS) with dispersive liquid-liquid microextraction (DLLME) and further gas chromatography mass spectrometry analysis was developed for the simultaneous determination of bisphenol A (BPA) and bisphenol B (BPB) in canned seafood samples. Besides the great enrichment factor provided, the final DLLME extractive step was designed in order to allow the simultaneous acetylation of the compounds required for their gas chromatographic analysis. Tetrachloroethylene was used as extractive solvent, while the acetonitrile extract obtained from QuEChERS was used as dispersive solvent, and anhydride acetic as derivatizing reagent. The main factors influencing QuEChERS and DLLME efficiency including nature of QuEChERS dispersive-SPE sorbents, amount of DLLME extractive and dispersive solvents and nature and amount of derivatizing reagent were evaluated. DLLME procedure provides an effective enrichment of the extract, allowing the required sensitivity even using a single quadropole MS as detector. The optimized method showed to be accurate (>68 % recovery), reproducible (<21 % relative standard deviation) and sensitive for the target analytes (method detection limits of 0.2 μg/kg for BPA and 0.4 μg/kg for BPB). The screening of several canned seafood samples commercialized in Portugal (total = 47) revealed the presence of BPA in more than 83 % of the samples with levels ranging from 1.0 to 99.9 μg/kg, while BPB was found in only one sample at a level of 21.8 μg/kg.
一种新的简单可靠的方法，结合乙腈分配提取程序，随后进行分散固相净化（QuEChERS）与分散液液微萃取（DLLME），并进一步进行气相色谱质谱分析，用于同时测定罐头海鲜样品中的双酚 A（BPA）和双酚 B（BPB）。除了提供的巨大富集因子外，还设计了最终的 DLLME 萃取步骤，以便允许同时乙酰化化合物，以进行气相色谱分析。四氯乙烯被用作萃取溶剂，而从 QuEChERS 获得的乙腈提取物被用作分散溶剂，并用酐乙酸作为衍生化试剂。影响 QuEChERS 和 DLLME 效率的主要因素包括 QuEChERS 分散 SPE 吸附剂的性质、DLLME 萃取和分散溶剂的量以及衍生化试剂的性质和量。DLLME 程序提供了对提取物的有效富集，甚至使用单个四极杆 MS 作为检测器，也能达到所需的灵敏度。优化后的方法具有准确性（>68%的回收率）、重现性（<21%的相对标准偏差）和对目标分析物的灵敏度（BPA 的方法检测限为 0.2μg/kg，BPB 的方法检测限为 0.4μg/kg）。对葡萄牙市售的几种罐头海鲜样品（总计=47 个）进行筛查，结果发现超过 83%的样品中存在 BPA，其含量范围为 1.0 至 99.9μg/kg，而 BPB 仅在一个样品中发现，含量为 21.8μg/kg。
