气相色谱-质谱法检测食品中残留的丙炔氟草胺

Determination of flumioxazin residue in foods using gas chromatography-mass spectrometry

建立了多种食品中丙炔氟草胺残留量的气相色谱-质谱检测方法。样品采用乙腈或乙酸乙酯提取,经旋转蒸发去除提取液后,用乙腈-甲苯（体积比为3∶1）溶解残渣,经氨基固相萃取柱净化,净化液由气相色谱-选择离子监测质谱测定,外标法定量。方法的线性范围为0.02～1.0mg/L,多种食品基质中的平均回收率为79.4%～101%,相对标准偏差（RSD）为0.242%～7.15%（n=10）,检测限均为0.01mg/kg。该方法灵敏度高,选择性好,可作为多种食品中丙炔氟草胺残留量的常规检测方法。

A method for the determination of flumioxazin residue in foods by gas chromatography-mass spectrometry （GC-MS） has been developed. The food sample was extracted with acetonitrile or ethyl acetate, concentrated in a rotary evaporator, then dissolved in acetonitrile-methyl benzene （3∶1, v/v） and purified with an NH2-solid phase extraction （SPE） column. The final extract was analyzed by gas chromatography-mass spectrometry with selected ion monitoring mode （GC-MS-SIM）. External standard method was used for the quantification. The mean recoveries of flumioxazin spiked in foods were 79.4%-101%, and the relative standard deviations were 0.242%-7.15%（n=10）. The detection limit for each was 0.01 mg/kg. This method has high sensitivity, veracity and is suitable for the determination of pesticide residues in foods.