一种改进的菜籽油样品提取制备方法,用于随后气相色谱法测定菜籽油中唑类杀菌剂的含量

Mikhail F. Zayats , Sergey M. Leschev , Marina A. Zayats
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引用次数: 15

摘要

在20±1℃条件下,研究了19种唑类农药在正己烷/水-有机混合体系和菜籽油(或正己烷油溶液)/有机溶剂中的分布。计算了烃与极性相的分布常数P和系数D。结果表明,所研究的农药均具有疏水性,即在正己烷-水体系中,其对数P < 0。用有机溶剂代替水导致log P急剧下降,它们的值变为负值。结果表明,强无机酸在无水乙腈溶液中最充分、有选择性地从己烷和植物油中提取出唑类农药。特别是乙腈的酸化作用使大多数被研究农药的D值下降50-2000倍。利用这一现象开发了一种改进的技术,用于定量分析广泛使用的一种可以在菜籽油中微量存在的唑类农药。所提出的方法是基于高氯酸在无水乙腈中解离萃取(DE)唑,然后用己烷和正磷酸氢二钾水溶液清理乙腈提取物中的有机杂质,最后用GC-ECD(气相色谱-电子捕获检测)测定唑类杀菌剂。加样回收率在85% ~ 115%之间,RSD < 10%。所获得的定量限范围为3.0 ~ 300 μg kg−1,低于欧盟为大多数农药设定的最大残留限量(MRLs)。该方法成功地应用于不同菜籽油样品。
本文章由计算机程序翻译,如有差异,请以英文原文为准。

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An improved extraction method of rapeseed oil sample preparation for the subsequent determination in it of azole class fungicides by gas chromatography

The distribution of 19 azole class pesticides in hexane/aqueous–organic mixtures systems and rapeseed oil (or oil solution in hexane)/organic solvents has been studied at 20 ± 1 °C. The distribution constants (P) and coefficients (D) between hydrocarbon and polar phase are calculated. It is found that all the studied pesticides are hydrophobic, i.e., in hexane–water system log P  0. Replacement of water by organic solvents results in sharp log P falling, and their values become negative. It is revealed that solutions of strong inorganic acids in anhydrous acetonitrile extract azole class pesticides from hexane and vegetable oils most fully and selectively. In particular, the acidification of acetonitrile causes a drop of D values in 50–2000 times for the majority of the studied pesticides. This phenomenon was used for the development of the improved technique for the quantitative analysis of a widely used azole class pesticides, which can be presented at trace levels in rapeseed oil. The proposed methodology is based on dissociation extraction (DE) of azoles using perchloric acid in anhydrous acetonitrile, with following clean-up of acetonitrile extract from organic impurities by hexane and aqueous solution of dipotassium hydrogen orthophosphate, and final GC–ECD (gas chromatography with electron capture detection) determination of azole fungicides. The values of obtained recoveries were between 85% and 115% with RSD values below 10%. The obtained limits of quantitation, ranged from 3.0 to 300 μg kg−1, are below the maximum residue levels (MRLs) set by the European Union for the majority of pesticides. The developed method was successfully applied to different rapeseed oil samples.

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