PDF全文下载:2011040365
王树娟, 李娇, 张晖, 田霞, 范志先*
(青岛科技大学 化工学院,山东 青岛 266042)
摘要:采用GC-ECD建立了毒死蜱在鲜桃上残留量测定的分析方法。以乙腈为提取剂,正己烷和水液-液分配,硅胶柱净化,DB-1701P毛细管色谱柱分离,对桃样品进行了测定,方法检出限0.001 mg·kg-1。2个添加水平0.05 mg·kg-1和0.5 mg·kg-1,平均回收率分别为88 %和90 %,相对标准偏差12.63 %和11.92 %。该方法灵敏、可靠,能满足桃上毒死蜱残留量的测定。青岛市场上桃样品测定结果表明:在大棚鲜桃样品中未检出毒死蜱;大田样品分析有施用毒死蜱的迹象,检出量为0.001 0~0.416 1 mg·kg-1,低于国际食品法典(CODEX)的最大残留限量(0.5 mg·kg-1)。
关键词:毒死蜱; 桃; GC-ECD; 农药残留
中图分类号: TS 272.7文献标志码: A
Determining of Chlorpyrifos Residue in Fresh Peach by GC-ECD
WANG Shu-juan, LI Jiao, ZHANG Hui, TIAN Xia, FAN Zhi-xian
(College of Chemical Engineering, Qingdao University of Science and Technology, Qingdao 266042, China)
Abstract: A method was established for determining of residue of chlorpyrifos in fresh peach by GC-ECD. The sample was extracted with acetonitrile, liquid-liquid distribution with n-hexane and water and cleaned up with silica gel. The sample was separated in the quartz elastic capillary column DB-1701P with N2(99.997%) as carrier gas. The limit of detection was 0.001 mg·kg-1. As the samples were fortified with chlorpyrifos at concentrations of 0.05 mg·kg-1 and 0.5 mg·kg-1, the recoveries were 88 % and 90 %, and the RSD was 12.63 % and 11.92 % respectively. This method is sensitive and accurate, so it is suitable for the determining of trace chlorpyrifos in fresh peach. Final results of the peach from some farmer markets and supermarkets of Qingdao show that it was below the detection of limit in plastic houses, while it was detected in the field, and the residues were 0.001 0-0.416 1 mg·kg-1 and it is below the MRLs of CODEX(0.5 mg·kg-1).
Key words: chlorpyrifos; peach; GC-ECD; pesticide residue
收稿日期: 2011-03-13
作者简介: 王树娟(1983—),女,硕士研究生. *通信联系人.