加速溶剂萃取-气相色谱-串联质谱法测定菊花中多种农药残留

Determination of multi-pesticides in chrysanthemum by accelerated solvent extraction-gas chromatography-tandem mass spectrometry

中文关键词:  菊花  加速溶剂萃取  石墨化碳/氨基固相萃取  气相色谱-串联质谱法  农药残留

英文关键词:chrysanthemum  accelerated solvent extraction  Carb/NH2 solid phase extraction  gas chromatography-tandem mass spectrometry  pesticide residues

中文摘要:

      目的 建立一种加速溶剂萃取结合气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry, GC-MS/MS)同时检测菊花中123种农药残留的方法。方法 样品采用乙腈提取, 经加速溶剂萃取, 石墨化碳/氨基固相萃取小柱净化, SH-Rxi-5SilMS (30 m×0.25 mm, 0.25 μm)毛细管色谱柱分离, 在气相色谱串联质谱多反应监测离子(multiple reaction monitoring, MRM)扫描模式下进行测定, 基质外标法定量。结果 在0.005~0.5 mg/L范围内, 123种农药有良好的线性关系(r2≥0.9967), 方法检出限为0.5~29.1 μg/kg, 定量下限为1.7~97.1 μg/kg, 在100、200、400 μg/kg 3个添加水平下, 123种农药的平均回收率在70.0%~128.8 %之间, 相对标准偏差(RSD)在0.5%~10.1%。结论 该方法提取效率高、准确、灵敏, 可应用于菊花中多种农药残留的筛查与测定。

英文摘要:

      Objective To establish a method for simultaneous determination of 123 pesticide residues in chrysanthemum by accelerated solvent extraction coupled with gas chromatography-tandem mass spectrometer (GC-MS/MS). Methods Chrysanthemum samples were extracted by acetonitrile, and purified through Carb/NH2 solid phase extraction (SPE) cartridges after accelerated solvent extraction. The residues were separated on the SH-Rxi-5SilMS (30 m×0.25 mm, 0.25 μm) capillary column, analyzed by GC-MS/MS with multiple reaction monitoring mode, and quantified by external standard method. Results The results showed that 123 kinds of pesticides had good linear relationships at the range of 0.005-0.5 mg/L, with correlations coefficients more than 0.9967. The limits of detection were 0.5-29.1 μg/kg, and the limits of quantitation were 1.5-97.1 μg/kg. The average recoveries of 123 compounds at three spiked levels of 100, 200, 400 μg/kg ranged from 70.0% to 128.8%, with relative standard deviations of 0.5%-10.1%. Conclusions This method is accurate and sensitive with higher extraction efficiency, which can be applied to the screening and simultaneous determination of multiresidue in chrysanthemum．