Department of Analytical Chemistry, Faculty of Chemistry, Universidad Complutense Madrid, Ciudad Universitaria, 28040 Madrid, Spain.
Food Chem. 2014 Mar 1;146:141-8. doi: 10.1016/j.foodchem.2013.09.055. Epub 2013 Sep 19.
A new and reliable miniaturised QuEChERS-based extraction method combined with a dispersive SPE cleanup procedure for extracting triclosan and methyltriclosan from fish roe and surimi samples was proposed. The effectiveness of different extraction/partition conditions for QuEChERS method was systematically investigated, and the use of acetonitrile extraction solvent and MgSO4, PSA, C18 and Florisil as cleanup reagents was recommended in the final method. Other method based on ultrasonic extraction with ethylacetate and clean-up with SPE was also evaluated for these samples. Different polymeric and silica sorbents for clean up were tested and the combination of Florisil and PSA was finally selected. The performance of these miniaturised sample preparation methods combined with GC-MS with quadrupole detection were compared. Extraction efficiency as well as cleaning effectiveness, laboriousness and speed were taken as criteria for method evaluation. Satisfactory validation parameters, such as linearity, recovery, precision and LODs and LOQs for both developed analytical methods were obtained from fish roe and surimi samples. Finally, both methods were applied to real samples. The sensitivity of the proposed methods was good enough to ensure reliable determination of target analytes at concentration levels commonly found in this kind of samples.
提出了一种新的、可靠的基于 QuEChERS 的微型提取方法，结合分散固相萃取净化程序，用于从鱼卵和鱼糜样品中提取三氯生和甲基三氯生。系统研究了 QuEChERS 方法不同提取/分配条件的有效性，并推荐在最终方法中使用乙腈提取溶剂和 MgSO4、PSA、C18 和 Florisil 作为净化试剂。还评估了基于超声提取和 SPE 净化的其他方法用于这些样品。测试了不同的聚合物和硅胶吸附剂用于净化，并最终选择了 Florisil 和 PSA 的组合。比较了这些与 GC-MS 结合四极杆检测的微型样品制备方法的性能。提取效率以及净化效果、繁琐程度和速度被用作方法评估的标准。从鱼卵和鱼糜样品中获得了两种开发的分析方法的令人满意的验证参数，如线性、回收率、精密度和 LODs 和 LOQs。最后，两种方法均应用于实际样品。所提出方法的灵敏度足以确保在通常在这类样品中发现的浓度水平下可靠地测定目标分析物。
