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采用基质固相分散结合气相色谱电子捕获检测法优化测定土壤中氯代农药。

Optimization of matrix solid phase dispersion coupled with gas chromatography electron capture detection for determination of chlorinated pesticides in soil.

机构信息

Environmental Sciences Research Institute (ESRI), Shahid Beheshti University, G.C., Evin, Tehran 1983963113, Iran.

出版信息

Talanta. 2012 Nov 15;101:504-9. doi: 10.1016/j.talanta.2012.10.009. Epub 2012 Oct 12.

Abstract

A fast, simple and efficient technique based on matrix solid phase dispersion has been presented for extraction and clean-up of some chlorinated pesticides and derivative products; α-BHC, β-BHC, γ-BHC, δ-BHC, heptachlor, aldrin, dieldrin, endrin, endosulfan 1, endosulfan 2, 4,4'-DDT, 4,4'-DDE, 4,4'-DDD, heptachlor epoxide, endrin aldehyde, endosulfan sulfate. Box-Behnken response surface methodology was employed for optimization of the extraction efficiency. As the optimized procedure, 0.5 g of dried and sieved soil samples were mixed with 2.0 g of 10% C18 in silica (w/w) as dispersant and after transferring into the extraction tube they were extracted with 8 mL of dichloromethane-n-hexane (1:1, v/v). Gas chromatography with electron capture detector was used for selective and sensitive determination of the analytes. Recoveries for the extraction of the proposed analytes were calculated and were satisfying (more than 75%), except for endrin aldehyde (59%) and endosulfan sulfate (62%). Also the method was linear over the calibration range (R(2)>0.991) and the quantitative results were reasonably reproducible and sensitive (LODs ranged between 0.3 and 1.8 ng g(-1)).

摘要

一种基于基质固相分散的快速、简单、高效的技术已被提出,用于提取和净化一些氯代农药及其衍生物;α-六六六、β-六六六、γ-六六六、δ-六六六、七氯、艾氏剂、狄氏剂、异狄氏剂、硫丹 1、硫丹 2、4,4'-滴滴涕、4,4'-滴滴伊、4,4'-滴滴滴、七氯环氧化物、异狄氏醛、硫丹硫酸盐。Box-Behnken 响应面法被用于优化提取效率。作为优化的程序,将 0.5 g 干燥和过筛的土壤样品与 2.0 g 10% C18 在硅胶(w/w)作为分散剂混合,然后将其转移到萃取管中,用 8 mL 二氯甲烷-正己烷(1:1,v/v)萃取。电子捕获检测器气相色谱法用于分析物的选择性和灵敏检测。所提出的分析物的提取回收率计算结果令人满意(超过 75%),除了异狄氏醛(59%)和硫丹硫酸盐(62%)。该方法在校准范围内呈线性(R²>0.991),定量结果具有良好的重现性和灵敏度(LOD 范围在 0.3 至 1.8 ng g⁻¹之间)。

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