超声波提取-GC/MS法同时测定农用土壤中有机氯农药和多氯联苯

Ultrasonic Extraction-GC/MS Simultaneous Determination of Organochlorine Pesticides and Polychlorinated Biphenyl Residues in Agricultural Soil

[目的]建立同时测定农用土壤中有机氯农药和多氯联苯残留量的方法。[方法]土样采用超声波进行提取,氟罗里硅土柱进行净化和毛细管气相色谱质谱柱进行分析,并优化样品制备和气相色谱质谱分析条件。[结果]通过优化,5g土样用20ml混合溶剂(正己烷:丙酮=1:1,V:V),于30℃超声波中萃取20min;萃取液净化浓缩后以脉冲不分流进样;质谱扫描方式为选择离子扫描。在此条件下,9种有机氯农药和6种多氯联苯在一定浓度范围内线性关系良好,15种组分的平均回收率为85.4%～105.2%,相对标准偏差为4.5%～9.4%,检出限为0.10～1.10ng/g。[结论]该方法适合用于农用土壤中有机氯农药和多氯联苯残留量的快速检测。

[Objective] The study aimed to establish simultaneous determination method of Organochlorine pesticides and polychlorinated biphenyl residues in agricultural soil.[Method] The soil sample was treated with ultrasonic extraction,the Florisil column was used for purification and GC/MS capillary column was used for analysis.And the sample preparation and GC/MS analysis conditions were optimized.[Result] After optimization,5 g soil with 20 ml mixed solvent （N-hexane：acetone=1：1,V：V）at 30 ℃ for ultraction extraction,the time was 20 min;nine kinds of Organochlorine the extraction solution was purified and concentrated,and then injected with pulse splitless mode;the MS scan mode was selected ionscan.Under these conditions,nine kinds of organochlo rine pesticides and six kinds of polychlorinated biphenyls had good linear relationships in some concn.range.The mean recoveries,RSDs and determination limits of 15 components were 85.4%-105.2%,4.5%-9.4% and 0.10-1.10 ng/g resp.[Conclusion] This method was suitable for rapid determination on organochlorine pesticides and polychlorinated biphenyl residues in agricultural soil.