气相色谱-质谱法测定纺织品中22种农药残留

GC-MS Determination of Residual Amounts of 22 Pesticides in Textiles

提出了气相色谱-质谱法测定纺织品中22种农药残留量的方法。样品以正己烷-丙酮(1+1)混合溶液为提取剂,经加速溶剂萃取仪提取后,在40℃旋转蒸发仪中浓缩、氮气吹干后,用正己烷-丙酮(1+1)混合溶液溶解定容至2.0 mL,通过Agilent HP-5MS石英毛细管色谱柱(30m×0.25mm,0.25μm)分离,采用电子轰击离子源选择离子监测模式进行质谱测定。22种农药的检出限(3S/N)在0.003～0.03mg·kg-1之间。以空白棉布样品为基体,加入标准溶液进行回收试验,测得回收率在80.1%～95.9%之间,相对标准偏差(n=6)均小于13%。

GC-MS was applied to the determination of residual amounts of 22 pesticides in textiles. The sample was extracted with a mixture of n-hexane-acetone （1＋ 1） by accelerated solvent extraction, and the extract was concentrated in a rotary evaporator at 40℃ and evaporated to dryness by N2 blowing. The residue obtained was dissolved and made up to 2. 0 mL with n-hexane-acetone （1 ＋1 ） solution, which was used for GC-MS analysis. The Agilent HP-5MS （30 m×0. 25 mm, 0.25 μm）. capillary chromatographic column was used for separation, and the electron impact ionization source with selected ion monitoring （SIM） was adopted in MS. Values of detection limit of 22 pesticides found were in the range of 0. 003-0.03 mg·kg-1 On the base of blank sample of cotton fabric, test for recovery was made by standard addition method, values of recovery found were in the range of 80.1%-95.9%, with RSD＇s （n=6） less than 13%.