气相色谱-质谱联用法测定农药制剂中29种助剂

建立了气相色谱-质谱联用法（GC-MS）同时测定农药制剂中29种助剂的方法。农药制剂经甲醇稀释，取上清液过0.22 μm滤膜后检测分析。采用VF-1701MS毛细管柱（60 m×0.25 mm×0.25 μm）分离，选择离子监测模式下（SIM）测定，外标法定量。结果表明，29种农药助剂在6.2~400.0 mg/L范围内线性关系良好，相关系数（R²）均大于0.99，方法定量限为4.4~439.1 mg/kg，乳油型和可溶液剂型农药样品的平均加标回收率分别为82.0%~111.9%和82.6%~112.9%，相对标准偏差为0.4%~7.2%和0.3%~8.2%（RSD，n=6）。应用该方法对110份农药制剂样品进行检测，其中28份检出苯酚、N-甲基吡咯烷酮、二氯甲烷、正己烷等共11种农药助剂，含量范围为0.05%~15.65%。此方法操作简单，灵敏度高，准确性好，适用于农药制剂中29种助剂的同时检测。

Determination of 29 adjuvants in pesticide formulations by gas chromatography-mass spectrometry

A method based on gas chromatography-mass spectrometry (GC-MS) was developed for the simultaneous determination of 29 adjuvants in pesticide formulations. The pesticide formulation was diluted with methanol, and the supernatant was filtered through a 0.22-μm membrane. After separation on a VF-1701MS column, the analytes were detected by mass spectrometry in the selected ion monitoring (SIM) mode and quantified using the external standard method. Good linearities were obtained for the 29 pesticide adjuvants in the linear range of 6.2-400.0 mg/L, with correlation coefficients (R²) larger than 0.99. The limits of quantification (LOQs) were 4.4-439.1 mg/kg. The average recoveries in emulsifiable concentrate (EC) and soluble concentrate (SL) samples ranged from 82.0% to 111.9% and from 82.6% to 112.9%, respectively. The relative standard deviations (RSDs, n=6) ranged from 0.4% to 7.2% and from 0.3% to 8.2%, respectively. Finally, 110 pesticide formulation samples were detected; 11 kinds of pesticide adjuvants, including phenol, N-methyl pyrrolidone, dichloromethane, and n-hexane, were detected in 28 samples with contents ranging from 0.05% to 15.65%. The proposed method is simple, sensitive, and accurate, and is suitable for the simultaneous determination of the 29 adjuvants in pesticide formulations.