分散固相萃取分离-气相色谱法测定银鱼中拟除虫菊酯类农药残留量  

GC Determination of Residual Amount of Pyrethroid Pesticides in Whitebait with Separation by Dispersive Solid Phase Extraction

作　　者：曹军[1] 陈勇[1] 杨瑞章[1] 徐邦兴[1] 王太全[1] 黄月芳 

机构地区：[1]盐城出入境检验检疫局,盐城224002 [2]南通市水产品检测中心,南通226006

出　　处：《理化检验（化学分册）》2010年第10期1176-1178,1181,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：江苏出入境检验检疫局科研计划(2009KJ33)

摘　　要：以冰乙酸-乙腈溶液为萃取溶剂,采用乙二胺-N-丙基硅烷（PSA）、C18和石墨化炭黑固相材料分散净化技术,以气相色谱-电子捕获检测器测定银鱼中6种拟除虫菊酯类农药（联苯菊酯、甲氰菊酯、高效氯氟氰菊酯、氯氰菊酯、氰戊菊酯和溴氰菊酯）。该方法在0.05~1.0 mg.L-1范围内呈线性关系。方法的检出限（3S/N）：氯氰菊酯为0.02 mg.kg-1,其余5种拟除虫菊酯均为0.01 mg.kg-1。以银鱼试样为基体,加入两种不同浓度的6种拟除虫菊酯标准溶液作回收试验,测得回收率在82.9%~106.1%之间,相对标准偏差（n=6）在2.9%~7.1%之间。Six pyrethroid pesticides,namely bifenthrin,fenpropathrin,cyhalothrin,cypermethrin,fenvalerate and deltamethrin,in whitebait were determined simultaneously by GC with ECD after separation by dispersive solid phase extraction（DSPE）.Sample of whitebait was extracted homogeneously with glacial acetic acid-acetonitrile solution as dispersion agent.The extract obtained was purified by DSPE through cycle-shaking with ethylene diamine-N-propylsilane（PSA）,C18 and graphitized carbon black.The supernatant was used for GC-ECD analysis.Linearity ranges found were in the same range of 0.05-1.0 mg·L-1 for the 6 pyrethroid pesticides.Detection limits（3S/N） of the method obtained were 0.01 mg·kg-1 for cypermethrin and 0.02 mg·kg-1 for the other 5 pyrethroid pesticides.Tests for recovery and precision were made by addition of standard solutions of the 6 pyrethroid pesticides with 2 different concentrations to whitebait sample which was then analyzed by the proposed method.Values of recovery obtained were in the range of 82.9%-106.1% and values of RSD′s（n=6） were in the range of 2.9%-7.1%.

关 键 词：气相色谱法 分散固相萃取 拟除虫菊酯类农药 银鱼 

分 类 号：O657.7[理学—分析化学]