气相色谱法测定水产品中敌百虫、敌敌畏残留量

Determination of trichlorfon and dichlorvos residues in fishery products by gas chromatography

通过对色谱条件和样品前处理方法的研究比较,建立了水产品中敌百虫、敌敌畏残留量测定的气相色谱法。样品用丙酮-水溶液(2+1,v/v)提取,乙酸锌去脂,活性碳脱色,二氯甲烷萃取,浓缩后用气相色谱-火焰光度检测器(GC-FPD)测定。敌百虫在0.1～20μg/mL、敌敌畏在0.025～5μg/mL内线性关系良好(r2≥0.9995);0.01～4mg/kg添加浓度水平的回收率在74.8%～106.8%之间,相对标准偏差(RSD)为1.12%～13.7%;敌百虫的定量限为0.04mg/kg、敌敌畏的定量限为0.01mg/kg。该方法操作简捷,准确可靠,能满足水产品中敌百虫、敌敌畏残留的检测要求。

Gas chromatography method was developed for determination of trichlorfon and dichlorvos residues in fishery products by comparing chromatography conditions and the sample pretreatment. The samples were extracted with acetone-water （2＋1,v/v） and discolored by activated carbon,lipids were removed by ZnAC,then the residues were re-extracted by dichloromethane and determined by gas chromatography with flame photometric detector（GC-FPD）. The linear range of trichlorfon and dichlorvos were 0.1～20 μg/mL and 0.025～5 μg/mL （r2≥0.999 5）. When spiked with 0.04,0.4,4 mg/kg of trichlorfon and 0.01,0.1,1 mg/kg of dichlorvos,the average recoveries ranged from 74.8% to 106.8% and their relative standard deviations （RSD） were between 1.12% and 13.7%. The detection limits of trichlorfon and dichlorvos were 0.04 mg/kg and 0.01 mg/kg separately. This method is simple,reliable and can be applied to detection of trichlorfon and dichlorvos residues in fishery products.