双柱定性-气相色谱测定蔬菜中多种农药残留

Determination of Multiple Pesticide Residues in Vegetables by Gas Chromatography with Dual-column Identification

建立固相萃取-双柱定性-气相色谱法测定蔬菜中多种有机氯、拟除虫菊酯类农药残留的方法。样品中的有机氯、拟除虫菊酯类农药经乙腈溶剂超声提取后,CARB/NH2固相萃取柱净化,采用HP-5与DB1701毛细管色谱柱双柱定性,气相色谱-电子捕获检测法(GC-ECD)进行定量分析。在一定浓度范围内质量浓度与峰面积有良好的线性关系,其线性相关系数为0.999 1~0.999 8,加标回收率在86%~110%之间,相对标准偏差(RSD)为0.73%~4.1%,方法检出限在5.0×10^(-4)mg/kg^1.0×10^(-3)mg/kg。该方法充分利用双柱定性的优势,检测结果准确、可靠,达到农残检测的要求,适用于蔬菜中多种有机氯、拟除虫菊酯类农药的同时测定。

A method for the determination of organochlorine and pyrethroid pesticide residues in vegetables by solid phase ex-traction（SPE）coupled with dual-column gas chromatography（GC）was developed and validated.The samples were extracted by acetonitrile with ultrasonic wave extraction and purificated with Carb-NH2 SPE column,then qualitatived by DB-1701 and HP-5,and quantitatived by GC-ECD.The results demonstrated that the linear ranges were gotten in a proper concentration range with the linear correlation coefficient from0.999 1 to 0.999 8.The average recoveries ranged from 86 % to 110 % with the relative standard deviations of0.73 %-4.1 %,and the limits of detection were from 5.0×10^-4mg/kg to 1.0×10^-3mg/kg. The method makes full use of the advantage of dual-column identification,which is accurate,sensitive and suitable for the analysis of organochlorine and pyrethroid residues in vegetables.