毛细管气相色谱法测定蔬菜和水果中三氯杀螨醇残留

Determination of Dicofol Residues in Vegetables and Fruits by Capillary Gas Chromatography

[目的]建立蔬菜和水果中三氯杀螨醇残留量的毛细管气相色谱检测方法。[方法]样品经有机溶剂超声提取，硫酸净化，采用分流不分流进样方式，用中等极性毛细柱程序升温分离，电子俘获检测器检测，外标法定量。[结果]两水平的平均回收率分别为87．4％、83．7％，RSD分别为3．77％、3．70％。在浓度1.00～0．01μg／ml间线形关系良好，回归方程P=1096064X＋6511，r=0．9996，方法检出限为0．0015mg／kg（S／N=3）。被测样品中存在不同程度的三氯杀螨醇残留。[结果]本法操作简便，分离效果及重复性好。

[Objective]To establish a method for determination of dicofol residues in vegetables and fruits by capillary gas chromatography, [-Methods]Samples were ultrasonic extracted with organic solvents, purified with sulfuric acid and injected with splitless/split mode. The temperature was increased and the sample was separated with the program of capillary column of BP-608 middle polar column and the dicofol residues were detected with electron capture detector and calculated by external standard method.[Results]The average recoveries were 83.7% and 87.4% at two spiked dicofol levels and the RSDs were 3.70% and 3.74%, respectively. The linear relation was good at the concentration between 1.00～ 0.01μg/ml . Regression equation was Y 1 096 064 X ＋6511, r =0. 999 6. Limit of identification of the method was 0. 001 5 mg/kg（S/N=3）. The tested vegetable and fruit samples contained dicofol residues in different levels. [Conclusion]This method is easy in operation and good at separation and repeatability.