紫菜中六六六、滴滴涕和扑草净的检测  

Residual Determination Method of HCHs, DDTs and Prometryn in Porphyra

作　　者：周明莹[1] 曲克明[1] 陈碧鹃[1] 谢寒冰 王联珠[1] 邵会[3] 顾晓慧[4] 

机构地区：[1]农业部海洋渔业可持续发展重点实验室中国水产科学研究院黄海水产研究所,青岛266071 [2]山东省青岛市菜篮子商品质量监督检测中心,青岛266071 [3]青岛大学医学院,青岛266021 [4]中国海洋大学,青岛266100

出　　处：《渔业科学进展》2014年第6期128-132,共5页Progress in Fishery Sciences

基　　金：国家海洋局环保项目[DOMEP(MEA)-02];“十二五”国家科技支撑计划(2012BAD29B06)共同资助

摘　　要：利用气相色谱-质谱联用技术测定紫菜中六六六、滴滴涕和扑草净的残留量。试样用乙腈提取,经石墨化炭黑/氨基复合柱净化,采用气相色谱-电子轰击源质谱测定,检测模式采用选择离子监测(SIM),外标法定量。研究结果显示,六六六方法定量限为5.0μg/kg,滴滴涕为2.5–5.0μg/kg,扑草净为2.5μg/kg。各组分加标回收率在78.5%–112.0%之间,相对标准偏差在3.6%–10.3%之间。结果表明,该方法简便、快速,其准确度和精密度能够满足紫菜中六六六、滴滴涕和扑草净同时检测的要求。Seaweed is one kind of phycophyta living on the rock in shallow intertidal. Porphyra is a kind of important economic algae, and it mainly includes Porphyra haitanensis, Porphyra yezoensis and Porphyra suborbiculata Kjellm. The organic pollutants in the marine environment are easily adsorbed by the ocean algae, causing high levels of pesticide residues. Pesticide pollutants in seaweed have seriously restricted the development of Chinese seaweed industry, which inhibits the expanding of international market. However, there are no nationwide standard methods to measure HCHs, DDTs and prometryn in algae. The current study developed new methods to measure the pollutants. Gas chromatography-mass spectrometry （GC-MS） was used to determine HCHs, DDTs and prometryn in porphyra. Pesticide residues were extracted with acetonitrile, cleaned-up by Cleanert PestiCarb/NH2 SPE cartridge, and were determined by GC-EI/MS in the selected ion monitoring mode （SIM）. The data was identified and quantified with the exterior standard method. The results showed that the limit of quantification （LOQ） in porphyra of HCHs , DDTs, and prometryn were 5.0, 2.5–5.0, and 2.5μg/kg, respectively. The efficiencies of extract pesticides were between 78.5% and 112.0%, and the relative standard deviations were from 3.6% to 10.3%. These results suggest that we have developed an easy, fast, and accurate method to simultaneously determine HCHs, DDTs and prometryn in algae.

关 键 词：气相色谱-质谱 六六六 滴滴涕 扑草净 紫菜 

分 类 号：X836[环境科学与工程—环境工程]