渔业科学进展2017，Vol.38Issue(4)：172-179,8.DOI:10.11758/yykxjz.20160412001
气相色谱-质谱法测定动物源性水产品中16种除草剂
Detection of Sixteen Herbicides in Animal Origin Aquatic Products Using Gas Chromatography-Mass Spectrometry
摘要
Abstract
With the development of modem 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 concems.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.关键词
动物源性水产品/除草剂/气相色谱-质谱法/凝胶色谱Key words
Animal origin aquatic products/Herbicides/Gas chromatography-mass spectrometry (GC-MS)/Gel permeation chromatography分类
化学化工引用本文复制引用
乔丹,刘小静,韩典峰,黄会,张华威,徐英江,宫向红,张秀珍..气相色谱-质谱法测定动物源性水产品中16种除草剂[J].渔业科学进展,2017,38(4):172-179,8.基金项目
山东省现代农业产业技术体系贝类产业创新团队(SDAIT-14-08)和藻类产业创新团队项目(SDAIT-26-05)共同资助[This work was supported by Shandong Province Modern Agricultural Technology System Shellfish Industry Innovation Team (SDAIT-14-08),and Shandong Province Modern Agricultural Technology System Algae Industrial Innovation Team(SDAIT-26-05)]. （SDAIT-14-08）
