基于QuEChERs-GC/ECD快速检测贝类中有机氯农药及多氯联苯残留

Simultaneous analysis of polychlorinated biphenyls and organochlorine pesticides in marine products by QuEChERS coupled with GC-ECD

建立基于QuEChERS前处理方法和气相色谱-电子捕获检测器同时测定贝类样品中17种持久性有机污染物残留的方法。样品经QuEChERS法进行预处理,选用已腈为提取剂,N-丙基乙二胺(PSA):C18(4∶6,m/m)净化,外标法定量。17种持久性有机污染物在1.0~50.0μg/kg范围内质量浓度与峰面积呈现良好的线性关系,相关系数均大于0.9957。17种持久性有机污染物的方法检出限(信噪比为3)和定量限(信噪比为10)分别为0.01~0.25μg/kg和0.25~1.0μg/kg。添加浓度为10.0、15.0、25.0μg/kg时,17种持久性有机污染物的平均回收率为84.1%~119.2%,相对标准偏差为3.9%~12.6%。本方法具有快速简便、定量准确,可应用于贝类样品中17种持久性有机污染物的快速检测。

A modified QuEChERS method coupled with GC-ECD was used to establish a method for the simultaneous determination of 17 persistent organic pollutants in marine products. The acetonitrile was selected as the extraction solvent,and N-propyl ethylenediamine （PSA） ： C18 （4 ： 6,m/m）was optimized for purification. Under the optimal conditions,the excellent linear correlation was obtained in the range of 1.0-50.0 μg/kg with the R2 above 0.9957. The limit of detection （S/N=3） and the limit of quantification （S/N=I0） were 0.01-0.25 μg/kg and 0.25-1.0 μg/kg,respectively. Meanwhile,the recoveries in the range of 84.1%-119.2% were obtained at the spiked concentrations of 10.0, 15.0,25.0 μg/kg with the relative standard deviation of 3.9%-12.6%. These findings demonstrate that the applicability of the developed method for quickly determination of 17 POPs in shellfish samples.