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Preconcentration and determination of high leachable pesticides residues in water using solid-phase extraction coupled with high-performance liquid chromatography

机译:固相萃取-高效液相色谱法对水中高沥出农药残留量进行富集和测定

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摘要

A multi-residue procedure was developed for analysis of four common pesticides in water using solid-phase extraction and high-performance liquid chromatography in combination with UV detection at 230 nm. The investigated pesticides (atrazine, dicloran, metazachlor and simazine) are highly leachable and easily migrate within the soil. Multi-walled carbon nanotubes (MWCNTs) adsorbent outperformed C_(18) bonded silica and graphitized carbon black for preconcentration of the pesticides from solution. The optimum experimental conditions for pesticides extraction were carefully studied and optimised. At the optimum preconcentration conditions (sample volume: 700 mL; adsorbent mass: 300 mg; solution pH: 5.0; flow rate: 3.0mLmin~(-1); and elution medium: methanol), a quantitiative recovery for pesticides was reported and a high preconcentration factor (1400) was attained. The detection limits of the proposed method were found in the range: 5-15 ng L~(-1). The dynamic range for simazine and atrazine determination was extended from 15 to 1000 ngL~(-1) while for metazachlor and dicloran the range was within 60-1000ngL~(-1). Five replicate determinations of 70ng of pesticides mixture present in 700 mL solution gave good results with RSD values within the range 2.5 to 4.6%. The present method gave recoveries from 92.7 to 95.3% for determination of 100ngL~-1 of pesticides in tap water and recoveries from 85.3 to 87.0 in well water with satisfactory RSD values (≤6%).
机译:开发了一种多残留程序,使用固相萃取和高效液相色谱法结合230 nm的紫外检测,可以分析水中的四种常见农药。被调查的农药(阿特拉津,双氯兰,间草胺和西马津)具有很高的浸出性,并易于在土壤中迁移。多壁碳纳米管(MWCNTs)吸附剂的性能优于C_(18)键合的二氧化硅和石墨化炭黑,可从溶液中预浓缩农药。仔细研究和优化了农药提取的最佳实验条件。在最佳预浓缩条件下(样品量:700 mL;吸附剂质量:300 mg;溶液pH:5.0;流速:3.0mLmin〜(-1);洗脱介质:甲醇),报告了农药的定量回收率,并且获得了很高的预浓缩系数(1400)。该方法的检出限为5-15 ng L〜(-1)。 simazine和atrazine测定的动态范围从15扩展到1000 ngL〜(-1),而间草胺和双氯仑的动态范围在60-1000ngL〜(-1)之内。对700 mL溶液中存在的70ng农药混合物进行了五次重复测定,结果良好,RSD值在2.5%至4.6%之间。本方法测定自来水中100ngL〜-1农药的回收率为92.7%至95.3%,在井水中的回收率为85.3至87.0,RSD值令人满意(≤6%)。

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