固相微萃取-气相色谱法测定橙汁中残留有机氯杀虫剂  

GC Determination of Organochlorine Insecticides in Orange Juice with Solid Phase Microextraction

作　　者：田孟魁[1] 冯喜兰[1] 

机构地区：[1]河南科技学院化学化工学院,新乡453003

出　　处：《理化检验（化学分册）》2008年第9期833-836,839,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：自制碳纳米管涂层萃取探头,顶空固相微萃取-气相色谱法测定橙汁中有机氯杀虫剂六六六和滴滴涕,优化了影响萃取效率的因素:萃取时间和温度、离子强度、有机溶剂、顶空体积、pH和样品的稀释度等。在0.05～6.0μg·L^(-1)范围内呈线性关系,方法的检出限在0.003～0.022μg·L^(-1)之间。该方法用于橙汁样品的测定,对不同的杀虫剂,加标回收率为71.0%～131.0%,相对标准偏差小于10%。A new extraction probe prepared by coating nanocarbon tube on stainless steel wire was used in the solid-phase microextraction （SPME） of organochlorine insecticides which were determined by GC with electron- capture detection. In the GC-analysis, SPME was integrated with the head-space technique （HS-SPME）. Various factors influential to the HS-SPME, i. e. time and temperature of extraction, ionic strength, kind of organic solvents, volume of headspace, pH value of the sample solution and its dilution, etc. , were studied and optimized. Eight insecticides were determined with ranges of linearity within 0. 05-6. 0μg · L^-1 , and detection limits （S/N= 3） ranged from 0. 003-0. 022μg · L^-1. Using orange juice sample as matrix, tests for recovery and precision were made by addition of standard solutions of the insecticides, giving values of recovery in the range 71.0%-131.0%, and RSD＇s （n=6） less than 10%.

关 键 词：碳纳米管 顶空固相微萃取 气相色谱法 有机氯杀虫剂 橙汁 

分 类 号：O657.37[理学—分析化学]