Torres C M, Picó Y, Mañes J
Laboratori de Bromatologia i Toxicologia, Facultat de Farmàcia, Universitat de València, Spain.
J Chromatogr A. 1997 Aug 22;778(1-2):127-37. doi: 10.1016/s0021-9673(97)00287-2.
Methods for the determination of thirteen fungicide and insecticide residues by solid-phase extraction with C18 and graphitized carbon black (GCB) were evaluated. The extraction of the residues was achieved by using matrix solid-phase dispersion (MSPD) and more conventional polar solvent extraction followed by liquid-solid phase partitioning. Determination was carried out by capillary gas chromatography with electron-capture and mass spectrometry detectors. The recoveries were determined by fortifying six different crops (apples, oranges, pears, tomatoes, lettuces and paprikas) with the pesticides studied (bromopropylate, chlorpyrifos methyl, cypermethryn, deltamethryn, fenarimol, fenvalerate, imazalil, lindane, permethryn, phentoate, procymidone, propiconazole and vinclozoline). Although, the data showed that the two extraction methods and both sorbents were able to isolate the pesticide residues from fruit and vegetables, the best results were obtained using MSPD with C18 which gave recoveries ranging from 70 to 105% and practical detection limits between 5.0 and 50.0 micrograms/kg for all the compounds. Ten of these pesticides have been detected in samples taken from Valencia markets, at levels of 0.02-20.50 mg/kg using the described methodology.
评估了采用C18和石墨化炭黑(GCB)固相萃取法测定13种杀菌剂和杀虫剂残留的方法。通过基质固相分散(MSPD)以及更传统的极性溶剂萃取,随后进行液固分配来实现残留物的萃取。采用带有电子捕获和质谱检测器的毛细管气相色谱法进行测定。通过在所研究的六种不同作物(苹果、橙子、梨、番茄、生菜和甜椒)中添加农药(溴螨酯、甲基毒死蜱、氯氰菊酯、溴氰菊酯、氯苯嘧啶醇、氰戊菊酯、抑霉唑、林丹、氯菊酯、稻丰散、腐霉利、丙环唑和乙烯菌核利)来测定回收率。尽管数据表明两种萃取方法以及两种吸附剂均能够从水果和蔬菜中分离出农药残留,但采用C18的MSPD方法获得了最佳结果,所有化合物的回收率在70%至105%之间,实际检测限在5.0至50.0微克/千克之间。使用所述方法在从巴伦西亚市场采集的样品中检测到其中10种农药,含量为0.02 - 20.50毫克/千克。