新型固相微萃取膜的制备及其用于茶叶中拟除虫菊酯的测定  

Preparation of Solid Phase Microextraction Membrane and Determination of Pyrethroid Pesticides in Tea

作　　者：申书昌[1] 邹明宇 刘艳萍[1] 吕伟超[1] 

机构地区：[1]齐齐哈尔大学分析测试中心

出　　处：《化学试剂》2018年第2期142-146,共5页Chemical Reagents

基　　金：黑龙江省教育厅基本科研业务专项项目(135209221)

摘　　要：合成了聚硅氧烷改性聚乙二醇型聚氨酯,涂布于铝箔纸上制成固相微萃取膜,与气相色谱仪联用,测定了茶叶中联苯菊酯、甲氰菊酯、氯氰菊酯、氰戊菊酯、溴氰菊酯的残留量。样品经80℃水超声提取,固相微萃取膜富集,V（丙酮）∶V（正己烷）=7∶3溶剂洗脱后,用气相色谱（GC-ECD）检测,外标法定量。考察了萃取温度、萃取时间、盐用量对萃取效率的影响,选择最佳洗脱溶剂。在0.005～1.0μg/mL范围内,5种农药的色谱峰面积与浓度呈良好的线性关系,相关系数（R2）分别为0.998 5、0.999 4、0.998 9、0.999 3和0.999 1,方法检出限分别为0.047、0.035、0.039、0.034和0.031μg/L。The silicone modified polyethylene glycol polyurethane solid phase microextraction membrane on aluminum foil was prepared.Five pyrethroidpesticides,such as bifenthrin,fenpropathrin,cypermethrin,fenvalerate and deltamethrin in the tea were determined by membrane solid phase microextraction coupled with gas chromatography.The pyrethroid pesticides were extracted in 80℃ water and ultrasonicwave,enriched on solid phase microextraction membrane,evaluated in acetone and n-hexane（V（acetone）∶V（n-hexane）=7∶3）,determinated by GC-ECD,quantitated analysis byexternalst and ardcurve.The effects of the temperature,time and salt content on extraction ratio were investigated and the best elution solvent was chosen.In the range from 0.005~1.0 μg/mL,the relationship between the peak area and concentration of bifenthrin,fenpropathrin,cypermethrin,fenvalerate and deltamethrin were linear.The correlation coefficients（R2） were 0.998 5,0.999 4,0.998 9,0.999 3 and 0.999 1,respectively.The detection limits for five pyrethroid pesticides were 0.047,0.035,0.039,0.034 and 0.031 μg/L,respectively.

关 键 词：固相微萃取膜 气相色谱 拟除虫菊酯 茶叶 

分 类 号：O657.7[理学—分析化学]