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

  • 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8 000 r/min离心5 min,取上清液,过0.22 μm滤膜后检测分析。采用VF-WAXms毛细管柱(60 m×0.25 mm×0.25 μm)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(R2)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。

     

    Abstract: 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 8 000 r/min for 5 min at 20 ℃, and the supernatant was filtered through 0.22 μm 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 (R2) 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.

     

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