气相色谱法测定食品中三氯杀螨醇残留量的研究

Study on the determination of Dicofol residue in food with gas chromatography

为实施食品中三氯杀螨醇限量卫生标准 ,建立了毛细管气相色谱法测定食品中三氯杀螨醇残留量的方法 ,试样以石油醚提取 ,浓硫酸净化 ,用DB - 1型毛细管柱分离测定。测定条件 :柱温 2 4 0℃ ;检测器 (ECD)温度 30 0℃ ;进样口温度 2 80℃ ;载气 (N2 )流量 5 0mL min ;压力 15 0kPa ;分流比 5 0∶1。该方法前处理简单 ,分离效果与重现性好 ,回收率为 91%～ 99 5 % ,相对偏差为 4 0 %～9 3% ,线性范围为 0 0～ 1 0 μg mL ,最低检测限为 8 0× 10 -3 ng。该方法可以满足检测食品中三氯杀螨醇残留的需要。

A method for determining the dicofol residue in food was established by using gas chromatography.The samples with dicofol were extracted by using petroleum benzine and purified by using sulfuric acid. Dicofol was determined by capillary gas chromatography,the optimized conditions were:column temperature:240℃;electron capture detector temperature:300℃;injector temperature:280℃;the flow rate of N\-2:50 mL/min;pressure:150 kPa;split ratio:50∶1.The method was simple in preparation,good in separation and reproduction while actual samples were determined.The variation coefficient of dicofol while determined was 4 0%～9 3% and the recovery rate was 91 0%～99 5%,the linear range was 0 0～1 0 μg/mL,the detection limit was 8 0×10 -3 ng.The results of the detection could meet the requirement of the national standard for testing the dicofol residue in foods.