【摘要】 建立了测定水稻中烯啶虫胺及其代谢物2-[N-(6-氯-3-吡啶甲基)-N-乙基]氨基-2-甲基亚氨基乙酸(CPMA)、N-(6-氯-3-吡啶甲基)-N-乙基-N’-甲基甲脒(CPMF)的液相色谱-质谱检测方法。水稻样品采用QuEChERS前处理技术,经Shim-pack GIST C18色谱柱分离,采用电喷雾正离子模式,通过多反应监测方式测定,基质匹配标准曲线外标法定量。试验结果表明,稻壳、秸秆和糙米基质中烯啶虫胺及其代谢物在选择的浓度范围内线性关系良好,相关系数(r)均不小于0.9982,方法检出限为0.0025 mg/L。在3个不同的添加浓度水平下,烯啶虫胺及其代谢物CPMA、CPMF在水稻稻壳、秸秆、糙米3种基质中的平均添加回收率为80.13%～104.42%,相对标准偏差为0.97%～2.94%。该方法操作简单、高效、快速,对于定量检测同类样品中烯啶虫胺及其代谢物残留量有较好的实际应用效果。更多还原

【Abstract】 A new method for the simultaneous identification and quantification of nitenpyram and its metabolites 2-[N-(6-chloro-3-pyridylmethyl)-N-ethyl] amino-2-methyliminoacetic acid(CPMA) and N-(6-chloro-3-pyridylmethyl)-N-ethyl-N’-methylformamidine(CPMF) in rice by liquid chromatography tandem mass spectrometry was established. The rice samples are pretreated by QuEChERS. The analytes were separated on a Shim-pack GIST C18 column, detected in the positive ion mode(ESI+) using multiple reaction monitoring(MRM), and quantified by an external standard method. The linear relationships of the nitenpyram and its metabolites in rice husk, straw and brown rice samples were good in the selected concentration range, and the correlation coefficients were all not less than 0.9982,the limits of detection(LODs) was 0.0025 mg/L. The average rate of recovery of nitenpyram and its metabolites in rice husk, straw and brown rice were 80.13%～104.42% at three spiked levels in the blank samples, and the relative standard deviation was 0.97%～2.94%. The method has the advantages of simple operation, efficient and fast. It has a good practical application effect for quantitative detection of the residue of nitenpyram and its metabolites in similar samples.更多还原