Papadakis Emmanouil N, Vryzas Zisis, Papadopoulou-Mourkidou Euphemia
Aristotle University, Pesticide Science Laboratory, P.O. Box 1678, 54006 Thessaloniki, Greece.
J Chromatogr A. 2006 Sep 15;1127(1-2):6-11. doi: 10.1016/j.chroma.2006.06.010. Epub 2006 Jun 23.
A method for the multiresidue analysis of 16 organochlorine insecticides in sesame seeds has been developed. The method is based on the microwave-assisted extraction (MAE) of the sesame seeds by the use of a water-acetonitrile mixture followed by Florisil clean-up of the extracts and subsequent analysis by gas chromatography-mass spectrometry (GC/MS) in the selected ion monitoring (SIM) mode. MAE operational parameters (extraction solvent, temperature and time, extractant volume) were optimized with respect to extraction efficiency of the target compounds from sesame seeds with 46% oil content. Recoveries >80% with relative standard deviations (RSD) <12% were obtained for all compounds under the selected parameters. The Florisil clean-up step proved sufficient for the removal of co-extracted substances so that no adverse effect on the chromatographic system was observed. Limit of quantification (LOQ) values were in the range of 5-10 microg/kg. The proposed method was applied in the analysis of sesame seed samples imported to Greece.
已开发出一种用于芝麻中16种有机氯杀虫剂多残留分析的方法。该方法基于使用水 - 乙腈混合物对芝麻进行微波辅助萃取（MAE），随后对萃取物进行弗罗里硅土净化，并通过气相色谱 - 质谱联用仪（GC/MS）在选择离子监测（SIM）模式下进行后续分析。针对从含油量为46%的芝麻中萃取目标化合物的效率，对MAE操作参数（萃取溶剂、温度和时间、萃取剂体积）进行了优化。在选定参数下，所有化合物的回收率均>80%，相对标准偏差（RSD）<12%。结果表明，弗罗里硅土净化步骤足以去除共萃取物，因此未观察到对色谱系统有不利影响。定量限（LOQ）值在5 - 10μg/kg范围内。所提出的方法应用于对进口到希腊的芝麻样品的分析。
