加速溶剂萃取-凝胶净化色谱-气相色谱质谱法测定农用地土壤中有机氯农药方法研究

Determination of Organochlorine Pesticides in Agricultural Soil by Accelerated Solvent Extraction-Gel Permeation Chromatography-Gas Chromatography-Mass Spectrometry

通过对加速溶剂萃取、平行蒸发及净化方法等环节的优化实验,建立了加速溶剂萃取凝胶净化色谱气相色谱质谱法测定农用地土壤中23种有机氯农药的检测方法。结果表明,方法检出限为0.0034~0.0052 mg/kg;对化合物质量分数为0.25 mg/kg的土壤加标样品进行平行实验,回收率为82.0%~93.7%;测定结果的相对标准偏差(RSD)≤8.7%。对土壤有证标准质控样品进行分析,测定结果均在验收范围之内。该方法准确可靠,灵敏度较高,样品净化效果较好,能够满足农用地土壤中有机氯农药残留痕量分析的要求。

In this study,an accelerated solvent extraction-gel permeation chromatography-gas chromatography-mass spectrometry method was established for the determination of 23 organochlorine pesticides in agricultural soil,the optimization experiments were carried out on accelerated solvent extraction,parallel evaporation and purification methods.The method detection limits of the targets were in the range of 0.0034~0.0052 mg/kg.Six parallel analyses were performed on spiked soil samples with 0.25 mg/kg,and the recoveries ranged from 82.0%to 93.7%,the relative standard deviations(RSD)were less than 8.7%.The certified quality control samples were analyzed,and the results were all within the acceptance range.The method is accurate,reliable,sensitive,and has good sample purification effect,which can meet the requirements of trace analysis of organochlorine pesticide residues in soil of agricultural land.