凝胶色谱净化-毛细管气相色谱法测定黄瓜、番茄和青椒中15种有机磷农药

Determination of 15 Organophosphorus Pesticides in Cucumber, Tomato and Pepper Samples by Capillary Gas Chromatography with Gel Permeation Chromatographic Clean-up

建立了凝胶色谱柱净化蔬菜样本,毛细管气相色谱 火焰光度检测器测定15种有机磷农药的方法。用环己烷 乙酸乙酯(体积比为1∶1)淋洗液以1mL/min的流量洗脱凝胶色谱柱(10mmi d ×200mm,SX 3),分别用气相色谱检测各段流出液中农药的含量,得到了15种有机磷农药的凝胶色谱流出曲线。采用该方法检测,15种有机磷农药在黄瓜、番茄和青椒中的最小检出质量比均低于5×10-3mg/kg,在蔬菜中不同添加浓度的平均回收率为77 8%～106%,相对标准偏差(RSD)为0 10%～16 6%,其准确度和精密度均达到了农药残留分析的要求。

Fifteen organophosphorus pesticide residues in vegetable samples were extracted and cleanedup by gel permeation chromatography and detected by capillary GCFPD. An alternative validation method was established based on GCNPD detection on an HP1701 column. The eluting profiles of 15 compounds on a gel permeation column (10 mm id×200 mm, SX3) eluted by 1 mL/min cyclohexaneethyl acetate (volume ratio of 1∶1) were established according to GC quantitation. Minimum detection limits of this method were between 5×10-4 mg/kg to 5×10-3 mg/kg. The average fortified recoveries and coefficients of variation of the method were determined. The results show that recoveries are between 778%-106%, with an average RSD of 010%-166%. 