水果和蔬菜中苯醚甲环唑残留量的气相色谱-串联质谱测定方法研究

目的建立气相色谱-串联质谱法测定水果和蔬菜中苯醚甲环唑残留的分析方法.方法试样用乙腈提取,经Sep-Pak Carbon NH2固相萃取柱净化,气相色谱分离,串联质谱多反应监测模式下测定,外标法定量.结果苯醚甲环唑质量浓度在0.01mg/L~2.5mg/L范围内线性关系良好,相关系数R0.996.苯醚甲环唑在不同基质中平均回收率为73.40%~115.1%,相对标准偏差为4.86%~13.24%,检出限为0.005mg/kg.结论该方法灵敏度高,选择性好,抗干扰能力强,适合苯醚甲环唑残留量的定性确证分析和定量分析.

Determination of Difenoconazole Residues in Fruits and Vegetables by Gas Chromatography-Tandem Mass Spectrometry

Objective： An analytical method was established to determine difenoconazole residues in fruits and vegetables by gas chromatography/tandem mass spectrometer（GC-MS/MS）. Methods： Difenoconazole residues were extracted from test samples by acetonitrile and cleaned up by Sep-Pak Carbon NH2 SPE cartridge. Chromatographic separation was achieved by GC and the determination was performed by tandem mass spectrometry in a multiple reaction-monitoring mode. External standard method was used for the quantification of difenoconazole. Results：A good linear relationship was established in the difenoconazole concentration range of 0.01-2.5mg/L and the correlation coefficient was above 0. 996. The recovery rates of difenoconazole from different spiked samples were in the range of 73.40-115.1%. The relative standard deviations （RSD） was in the range of 4.86-13.24% and the limit of detection for difenoconazole was 0. 005mg/kg. Conclusion. Therefore, the developed method is suitable for determination of difenoconazole residues in fruits and vegetables qualitatively and quantitatively with satisfactory sensitivity, selectivity, accuracy and precision.