气相色谱/质谱法测定食品中甲氧基丙烯酸酯类杀菌剂残留

建立了一种专属、灵敏的气相色谱-质谱分析方法,用于检测水果、蔬菜、饮料、粮谷类、坚果类和肉、蛋、奶类等多种类型食品中嘧菌酯、醚菌胺、嘧蟎酯、氟嘧菌酯、醚菌酯、Z-苯氧菌胺、E-苯氧菌胺、肟醚菌胺、啶氧菌酯、唑菌胺酯和肟菌酯等11种甲氧基丙烯酸酯类杀菌剂残留量。对于不同类型的样品,使用不同有机溶剂对甲氧基丙烯酸酯类杀菌剂进行超声波提取,经凝胶渗透色谱对样品提取液进行净化、富集,采用气相色谱-质谱法以选择离子监测模式进行定性,外标法定量。上述各种杀菌剂在0.05~5.0 mg/kg浓度范围内呈线性,相关系数r>0.99。在空白样品中,添加甲氧基丙烯酸酯类杀菌剂的回收率在60.3%~120.0%之间,精密度(RSD)为1.54%~13.41%。各组分检出限均在0.002~0.015 mg/kg之间。

Determination of Strobilurin Fungicide Residues in Food by Gas Chromatography-Mass Spectrometry

A sensitive and selective method was developed for the determination of residues including azoxystrobin,dimoxystrobin,fluacrypyrim,fluoxastrobin,kresoxim-methyl,Z-metominostrobin and E-metominostrobin,orysastrobin,picoxystrobin,pyraclostrobin and trifloxystrobin in food such as fruits,vegertables,baverages,cereals,nuts,meats,egg and milk.Disparity organic solvents were used to ultrasound extract fungicide residues in variety samples.The extract was cleaned up by gel permeation chromatography purification system,and the elute solution was evaporated and re-resolution in a definite volume.Determination and confirmation was made by gas chromatography-mass spectrometry at selective ions monitoring mode with external standard method.The calibration curves were good linear between area and the concentration of from 0.05-5.0 mg/kg with the correlation coefficient r more than 0.99.The average recoveries from spiked samples at the three concentrations of 0.01,0.1,1.0 mg/kg ranged from 60.3% to 120.0% with relative standard deviation ranged from 1.5% to 13.4%.The limits of detection were 0.002-0.015 mg/kg in variesou matrixes.