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气相色谱-质谱法测定动物源性水产品中16种除草剂
乔 丹,刘小静,韩典峰,黄 会,张华威,徐英江,宫向红,张秀珍
作者单位
乔 丹 上海海洋大学食品学院 上海 201306山东省海洋资源与环境研究院 山东省海洋生态修复重点实验室 烟台 264006 
刘小静 山东省海洋资源与环境研究院 山东省海洋生态修复重点实验室 烟台 264006 
韩典峰 山东省海洋资源与环境研究院 山东省海洋生态修复重点实验室 烟台 264006 
黄 会 山东省海洋资源与环境研究院 山东省海洋生态修复重点实验室 烟台 264006 
张华威 山东省海洋资源与环境研究院 山东省海洋生态修复重点实验室 烟台 264006 
徐英江 山东省海洋资源与环境研究院 山东省海洋生态修复重点实验室 烟台 264006 
宫向红 山东省海洋资源与环境研究院 山东省海洋生态修复重点实验室 烟台 264006 
张秀珍 山东省海洋资源与环境研究院 山东省海洋生态修复重点实验室 烟台 264006 
摘要:
本研究建立了动物源性水产品中16种除草剂的凝胶色谱-固相萃取净化、气相色谱-质谱分析方法。结果显示,样品通过二氯甲烷–乙酸乙酯混合溶液提取、凝胶渗透过滤及固相萃取柱净化,采用气相色谱–质谱联用方法测定,选择离子监测、外标法定量。二甲戊乐灵、草净津在4–200 μg/L浓度范围内,其余14种在2–100 μg/L浓度范围内与其响应值呈良好的线性关系,相关系数(r)不低于0.9970。扑灭津、阿特拉津、特丁津、西玛津、敌草净、扑草净、莠灭净、异丙甲草胺定量限均为1.0 μg/kg;乙草胺、甲草胺、丁草胺、丙草胺、环草津、西草净定量限均为1.5 μg/kg;二甲戊乐灵、草净津定量限均为2.0 μg/kg。平均回收率为67.2%–103.0%,相对标准偏差为5.1%–9.5%。研究表明,该方法重现性好,回收率高,在精密度、准确度方面能满足残留检测要求,适用于水产品中16种除草剂残留的同时检测。用此方法检测了海参、牡蛎、扇贝等水产品中除草剂残留量,检出率最高的是莠灭净,其次是阿扑草净、特拉津、西草净、乙草胺,同时为进一步探讨除草剂污染对水产品质量安全的影响奠定基础。
关键词:  动物源性水产品  除草剂  气相色谱-质谱法  凝胶色谱
DOI:10.11758/yykxjz.20160412001
分类号:
基金项目:
Detection of Sixteen Herbicides in Animal Origin Aquatic Products Using Gas Chromatography-Mass Spectrometry
QIAO Dan,LIU Xiaojing,HAN Dianfeng,HUANG Hui,ZHANG Huawei,XU Yingjiang,GONG Xianghong,ZHANG Xiuzhen
Abstract:
With the development of modern agriculture, pesticide is extensively used in agricultural production. The herbicide as an important part of pesticide has also been widely used, causing significant environmental and food safety concerns. Currently, effect of herbicide contamination on the aquatic food product is not well understood. Furthermore, detection of herbicide residues in aquatic products is lack of efficient multi-residue detection method. This study established a reliable method for determining 16 herbicide residues in animal origin aquatic products. The method involves gel permeation chromatography- solid phase and extraction-gas chromatography-mass spectrometry. The sample was extracted using dichloromethane and ethyl acetate mixed solution, followed by a clean-up step using gel permeation chromatography. The product was then purified by solid phase extraction column. Results were determined by monitoring selected ion and quantified by external marker method. Good linearity was observed in the range of 4-200 μg/L in pendimethalin and cyanizine, whereas other herbicides showed good linearity in the range of 2-100 μg/L, with correlation coefficient higher than 0.9970 in both cases. The quantitation limit for propazine, atrazine, terbutylazine, simazine, desmetryn, prometryn, ametryn and metolachlor was 1.0 μg/kg. The quantitation limit for acetochlor, alachlor, butachlor, pretilachlor, cyprazine and simetryn was 1.5 μg/kg, and the quantitation limit for pendimethalin and cyanizine was 2.0 μg/kg. Average recovery rates ranged in 67.2%-103.0% and relative standard deviation of the method was 5.1%-9.5%. The method had good reproducibility and high recovery rate. In terms of residue detection, the precision and accuracy can meet the testing requirements, and the method could be used for determining 16 herbicide residues in aquatic products. The established method was applied to detect herbicides in sea cucumber, oyster, scallop etc. The results showed that ametryn had the highest detection rate in these samples and followed by atrazine, terbutylazine, simetryn and acetochlor. This study established the method for simultaneous detection of herbicide residues in aquatic products and built the foundation for further study of the impact of herbicide pollution on the quality and safety of aquatic products.
Key words:  Animal origin aquatic products  Herbicides  Gas chromatography-mass spectrometry (GC-MS)  Gel permeation chromatography