【作者】 陈静；

【导师】 钱传范；

【作者基本信息】 中国农业大学 ， 农药学， 2004， 硕士

【摘要】 本研究用两种检测器（氮磷检测器和火焰光度检测器仪器）和两种不同极性色谱梓（中极性毛细管色谱柱DB-1701、非极性毛细管色谱柱DB-1）作为研究手段，比较了20种有机磷杀虫剂在两种色谱柱（DB-1、DB-1701）、两种检测器（FPD、NPD）上的保留时间及最小检测量，建立了用不同极性色谱柱上有机磷农药的保留时间可作为有机磷农药双柱定性确证的的方法；建立了DB-1701，GC-FPD测定蔬菜中20种有机磷杀虫剂的气相色谱法，该方法的最小检测量为5×10^-11～2×10^-12g，线性范围在2×10^-9～1×10^-11g时，相关性良好。 通过四种提取方法的比较，确立了蔬菜中20种有机磷杀虫剂多残留的分析方法为：乙酸乙酯提取剂、高速匀浆法提取，经离心，浓缩，GC-FPD法测定。该方法的添加同收率73％～121％，相对标准偏差0～16.2％，最低检测浓度0.002～0.05mg／kg，符合农药残留分析要求。 对蔬菜中20种有机磷杀虫剂多残留分析净化处理进行了探讨，分别做了20种有机磷杀虫剂在三种层析柱（弗罗里硅土、中性氧化铝和活性炭+助滤剂545混合填料）柱上回收率试验，用葱、卷心菜试样做空白、添加农药标准样本的柱上净化试验，结果表明弗罗里硅土和中性氧化铝层析柱可有效除去卷心菜中的干扰物，活性炭混合填料层析柱能部分除去葱样本里的干扰物。 对云南省昆明市蔬菜中9种有机磷杀虫剂残留进行了测定，152个蔬菜实测样本有51个蔬菜样本被检出有超标农药，超标率为34.2％。更多还原

【Abstract】 In order to compare the retention time (RT) and limits of detection of 20 organophosphorous insecticides in different conditions the experiments were carried out using a medium polar capillary column (DB-1701) and a no polar capillary column (DB-1) with two detectors (GC-FPD and NPD). The RT of 20 organophosphorous insecticides in two different polar capillary columns was a retention qualitative method for 20 organophosphorous insecticides. DB-1701 capillary column coupled with GC-FPD detector was used in the following study, the limits of detection were in range of 5x10-11~2X 10-12 g, the linear range was 2X 10-9~1 X 10-11g .Multi-residue analysis of 20 organophosphorous insecticides in vegetable was performed by DB-1701 capillary column coupled with GC-FPD detector in this study. Ethyl acetate was used to extract the pesticides from vegetable samples using a homogenizer. The extract was separated, concentrated and detected by GC-FPD. Recoveries were in range of 73% ~ 121 %. Limits of quantification for different pesticides were in range of 0.002~0.05mg/kg. The relative standard deviations were in range of 0~16.2%.A study was carried out to clean up interferences from vegetable samples(cabbage and shallot) for multi residue analysis of 20 organophosphorous insecticides in vegetable. Recoveries from three different chromatographic cleaning-up columns(fiorisil, neutral alumina and charcoal)were studied. The interferences from cabbage and shallot can be removed effectively by florisil or neutral alumina column and charcoal column respectively.The residue of 9 organophosphorous insecticides in vegetable in kunming ,Yunnan province was detected using the multi-residue method. The residue of 9 organophosphorous insecticides was detected in 51 of 152 vegetables. The residue of 34.2% samples was higher than their MRL.更多还原