气相色谱-离子阱质谱法测定海洋贝类中多残留有机氯农药、多氯联苯和多环芳烃

本研究建立了凝胶渗透色谱和铝硅胶柱前处理,气相色谱-离子阱质谱法测定海洋贝类体内20种有机氯农药、28种多氯联苯和16种多环芳烃的多残留分析方法。通过对凝胶渗透色谱的组分收集时间和铝硅胶柱的正戊烷淋洗体积的实验条件优化,实现了样品索氏提取液的凝胶渗透色谱初步净化、铝硅胶柱色谱的组分分离和进一步去除干扰物质。结果表明,多氯联苯、有机氯农药和多环芳烃各化合物的方法检出限分别为0.01~0.14,0.02~0.17和0.52~0.81ng/g(湿重),样品的加标回收率和相对标准偏差分别为:多氯联苯84.1%~120.2%、5.6%~15.9%;多环芳烃62.3%~123.1%、8.7%~20.5%;有机氯农药77.3%~127.5%、3.1%~18.7%。本方法降低了样品的前处理成本,缩短了样品处理时间,可应用于海洋贝类体内持久性有机污染物的实际监测。

Multiresidual Analysis of Organochlorine Pesticides, Polychlorinated Biphenyls and Polycyclic Aromatic Hydrocarbons in Marine Shellfishes by Gas Chromatography-Ion Trap Mass Spectrometry

A gas chromatography-ion trap mass spectrometric (GC-ITMS) method with the pretreatment of gel permeation chromatography (GPC) and aluminosilicate column techniques was developed for the identification and determination of 20 organochlorine (OC) pesticides, 28 polychlorinated biphenyls (PCBs) and 16 polycyclic aromatic hydrocarbons (PAHs) compounds in marine shellfishes. The Soxhlet extract of the shellfish sample was preliminarily cleaned up by GPC, then treated by aluminosilicate column for separating OC pesticides, PCBs and PAHs into two groups and further eliminating the remaining interfering substances. The good results were achieved by optimizing the fraction collection time of GPC and the cut-off volume of eluting solvents from aluminosilicate column. The results showed that the method detection limits were 0.01-0.14 for PCBs, 0.02-0.17 for OC pesticides and 0.52-0.81 ng/g (wet weight) for PAHs. The recovery percentages and RSDs of two-level spiked samples were 84.1%-120.2% and 5.6%-15.9% for PCBs, 62.3%-123.1% and 8.7%-20.5% for PAHs, and 77.3%-127.5% and 3.1%-18.7% for OC pesticides, respectively. This approach reduced cost and time for sample pretreatment and has been applied in the actual POPs monitoring in shellfishes of marine environment.