液质联用法测定水稻中烯啶虫胺及其代谢物  

Determination of Nitenpyram and Its Metabolites in Rice by LC-MS

作　　者：杜亭 方国林 乔琳 朱仁发[2] DU Ting;FANG Guo-lin;QIAO Lin;ZHU Ren-fa(School of Biological Food and Environment Hefei University,Hefei 230601;School of Energy Materials and Chemical Engineering,Hefei University,Hefei 230601;Anhui Huachen Testing Technology Research Institute Limited Company,Hefei 230601,China)

机构地区：[1]合肥学院生物食品与环境学院,合肥230601 [2]合肥学院能源材料与化工学院,合肥230601 [3]安徽华辰检测技术研究院有限公司,合肥230601

出　　处：《合肥学院学报（综合版）》2021年第2期64-69,共6页Journal of Hefei University：Comprehensive ED

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。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.

关 键 词：烯啶虫胺 代谢物 CPMA CPMF 液相色谱串联质谱 水稻 

分 类 号：O657[理学—分析化学] TQ453[理学—化学]