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使用固相萃取净化柱测定水果和蔬菜中的有机氯和拟除虫菊酯类农药。

Determination of organochlorine and pyrethroid pesticides in fruit and vegetables using solid phase extraction clean-up cartridges.

作者信息

Sharif Zawiyah, Man Yaakob Bin Che, Hamid Nazimah Sheikh Abdul, Keat Chin Cheow

机构信息

National Public Health Laboratory, Ministry of Health, Malaysia Lot 1853, Kpg. Melayu Sungai Buloh, 47000 Sungai Buloh, Selangor, Malaysia.

出版信息

J Chromatogr A. 2006 Sep 15;1127(1-2):254-61. doi: 10.1016/j.chroma.2006.06.007. Epub 2006 Jul 20.

Abstract

A method to determine six organochlorine and three pyrethroid pesticides in grape, orange, tomato, carrot and green mustard based on solvent extraction followed by solid phase extraction (SPE) clean-up is described. The pesticides were spiked into the sample prior to analysis, extracted with ethyl acetate, evaporated and reconstituted with a solvent mixture of acetone:n-hexane (3:7). Three different sorbents (Strong Anion Exchanger/Primary Secondary Amine (SAX/PSA), Florisil and C18) were used for the clean-up step. Pesticides were eluted with 5mL of acetone:n-hexane (3:7, v/v) and determined by gas chromatography and electron-capture detection (GC-ECD). SAX/PSA was the sorbent, which provided chromatograms with less interference and the mean recoveries obtained were within 70-120% except for captafol. The captafol recoveries for grape were within acceptable range with C18 clean-up column.

摘要

描述了一种基于溶剂萃取然后固相萃取(SPE)净化来测定葡萄、橙子、番茄、胡萝卜和青菜中六种有机氯农药和三种拟除虫菊酯农药的方法。在分析前将农药添加到样品中,用乙酸乙酯萃取,蒸发后用丙酮:正己烷(3:7)的混合溶剂复溶。净化步骤使用了三种不同的吸附剂(强阴离子交换剂/伯仲胺(SAX/PSA)、弗罗里硅土和C18)。用5mL丙酮:正己烷(3:7,v/v)洗脱农药,并用气相色谱和电子捕获检测(GC-ECD)进行测定。SAX/PSA是能提供干扰较少的色谱图的吸附剂,除了克菌丹外,获得的平均回收率在70-120%范围内。使用C18净化柱时,葡萄中克菌丹的回收率在可接受范围内。

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