GC-MS/MS法测定乳油和可溶液剂型液体农药制剂中3种高风险吡咯烷酮类农药助剂  

Determination of Three High Risk Pyrrolidone Pesticide Adjuvants in EC and SL Pesticide Formulations by GC-MS/MS

作　　者：唐祥凯[1] 冯德建[1] 李怀平[1] 史谢飞[1] 许洋[1] 陈璐 吴微 TANG Xiang-kai;FENG De-jian;LI Huai-ping;SHI Xie-fei;XU Yang;CHEN Lu;WU Wei(Standard and Testing Technology of Tea Key Laboratory of Sichuan Province,National Institute of Measurement and Testing Technology,Chengdu 610021,China)

机构地区：[1]中国测试技术研究院,茶叶标准与检测技术四川省重点实验室,四川成都610021

出　　处：《质谱学报》2021年第2期163-171,共9页Journal of Chinese Mass Spectrometry Society

基　　金：四川省中央引导地方科技发展专项(2020ZYD044);四川省重点研发项目(2020YFN0003);四川省应用基础研究项目(2018JY0178)资助。

摘　　要：建立了气相色谱-串联质谱(GC-MS/MS)法同时测定乳油和可溶液剂型液体农药制剂中3种高风险吡咯烷酮类农药助剂。农药制剂经甲醇稀释,20℃下以8000 r/min离心5 min,取上清液,过0.22μm滤膜后检测分析。采用VF-WAXms毛细管柱(60 m×0.25 mm×0.25μm)分离,多反应监测(MRM)模式测定,外标法定量。结果表明,3种农药助剂在1.0~40.0 mg/L浓度范围内线性关系良好,相关系数(R^(2))均大于0.999,方法定量限为3.1~6.8 mg/kg,乳油型和可溶液剂型农药样品平均加标回收率分别为98.2%~108.9%和98.1%~111.7%,相对标准偏差分别为0.4%~2.6%和0.4%~3.4%(n=6)。采用该方法检测市售94份乳油型和27份可溶液剂型农药制剂样品,其中6份检出N-甲基吡咯烷酮(含量范围0.022%~11.328%),2份检出2-吡咯烷酮(含量范围0.018%~0.023%)。该方法具有操作简便、灵敏度高、准确度好等优点,适用于同时测定乳油和可溶液剂型液体农药制剂中3种高风险吡咯烷酮类农药助剂。A method based on gas chromatography-tandem mass spectrometry(GC-MS/MS)was developed for the simultaneous determination of three high risk pyrrolidone pesticide adjuvants in emulsifiable concentrate(EC)and soluble concentrate(SL)pesticide formulations.After diluting with methanol,the pesticide formulation was centrifuged at 8000 r/min for 5 min at 20℃,and the supernatant was filtered through 0.22μm membrane.After separation on a VF-WAXms column,the analytes were detected by GC-MS/MS at multiple reaction monitoring(MRM)mode and quantified using the external standard method.Good linearities were obtained for the three pyrrolidone pesticide adjuvants in the linear range of 1.0-40.0 mg/L with the correlation coefficients(R^(2))larger than 0.999.The limits of quantitation(LOQs)were 3.1-6.8 mg/kg.The average recoveries in EC and SL samples were 98.2%-108.9%and 98.1%-111.7%,and the relative standard deviations(RSDs,n=6)were 0.4%-2.6%and 0.4%-3.4%,respectively.94 samples of EC and 27 samples of SL pesticide formulations sold in the market were detected.N-methyl pyrrolidone was detected in 6 samples with the contents ranging from 0.022%to 11.328%,and 2-pyrrolidone was detected in 2 samples with the contents ranging from 0.018%to 0.023%.This method has certain advantageous,such as simpler operation,higher sensitivity,and better accuracy,which is suitable for the simultaneous determination of three pyrrolidone pesticide adjuvants in EC and SL pesticide formulations.

关 键 词：农药制剂 农药助剂 吡咯烷酮 气相色谱-串联质谱(GC-MS/MS) 

分 类 号：O657.63[理学—分析化学]