加速溶剂提取-气相色谱法同时测定土壤中的22种有机氯和有机磷农药

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我国环境污染调查评价测试项目中开展了大量有关土壤中有机氯及有机磷农药残留的测定工作,多种有机污染物同时分析测试的方法是研究的新热点。本文以正己烷-丙酮(体积比1∶1)为提取剂,采用加速溶剂提取,毛细管柱气相色谱法测定土壤中六氯苯等9种有机氯及敌敌畏等13种有机磷农药残留。方法回收率为79.1%~107.7%,相对标准偏差为3.62%~9.94%(n=7),检出限为0.02~0.45μg/kg。本方法将两类农药同时提取且实现了各组分的完全分离,拓展了方法的适用范围,与传统的超声提取和索氏提取法相比,提取时间缩短至20 min,提取溶剂体积降至50 mL,缩短了分析时间,降低了成本,精密度和回收率能够满足全国环境污染调查评价的需要。 China’s environmental pollution investigation and evaluation test carried out a large number of soil organic chlorine and organophosphorus pesticide residues in the determination of a variety of organic pollutants simultaneously analysis and testing method is a new hot spot. In this paper, 13 kinds of organophosphorus pesticide residues such as hexachlorobenzene and other dichlorvos in the soil were determined by accelerated solvent extraction and capillary gas chromatography with n-hexane-acetone (1: 1 by volume) as extraction solvent. The method recoveries ranged from 79.1% to 107.7%. The relative standard deviations were from 3.62% to 9.94% (n = 7). The detection limits were 0.02-0.45 μg / kg. Compared with the traditional ultrasonic extraction and Soxhlet extraction method, the extraction time is shortened to 20 min and the volume of the extraction solvent is reduced to 50 mL, shorten the analysis time, reduce the cost, precision and recovery rate to meet the needs of the national environmental pollution investigation and evaluation.
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