羟基聚甲基苯基硅氧烷固相微萃取纤维的制备及在蔬菜中农药残留分析的应用  

Application of Polymethylphenylsiloxane-coated SPME Fiber for Pesticide Analysis in Vegetables

作　　者：陈良壁[1] 曾景斌[2] 赵瑨云[1] 王翊如[2] 陈曦[2] 

机构地区：[1]武夷学院化学与环境工程系,福建武夷山354300 [2]厦门大学化学化工学院化学系,现代分析科学教育部重点实验室,福建厦门361005

出　　处：《分析科学学报》2009年第6期634-638,共5页Journal of Analytical Science

基　　金：福建省自然科学基金(No.2006J0393);福建省科技计划重点项目(No.2007Y0032)

摘　　要：通过合成羟基聚甲基苯基硅氧烷（PMPS—OH）材料，制备固相微萃取（SPME）纤维涂层。通过与商品化聚二甲基硅氧烷（PDMS）、聚丙烯酸酯（PA）和PDMS／聚二乙烯基苯（DVB）纤维对六六六异构体（α，β，γ，δ-BHC）、DDT及其衍生物（p，p’-DDD，p，p’-DDE，o，p＇-DDT，p，p＇-DDT）、联苯菊酯、甲氰菊酯、高效氟氯氰菊酯、三氟氯氰菊酯、氯氰菊酯和氰戊菊酯等选定农药萃取效果的比较，所制备的PMPS—OH纤维具有更好的萃取效率。对SPME实验条件进行了研究和优化，测定方法对各种农药的线性范围多在0．01～2ng／g之间，相应的检出限在0．001～0．05ng／g范围，回收率在50．5％～103％。方法已被应用于蔬菜样品中农残的检测。Hydroxyl-terminated polymethylphenylsiloxane （PMPS-OH） was synthesized and successfully used as a novel coating for solid phase microextraction （SPME）. PMPS-OH coated fiber was applied to the analysis of pesticides including α,β,γ,δ-BHC, p, p＇-DDD, p, p＇-DDE, o, p＇-DDT, p, p＇ DDT, bifenthrin, fenpropathrin, β-cyfluthrin, cyhalothrin, cypermethrin and fenvalerate by SPME-GC-ECD. The extraction effieieneies of the PMPS-OH coated fiber for selected pesticides were found to be higher than those of commercial fibers, such as PDMS, PA and PDMS/DVB. The SPME experimental conditions including stirring rate, extraction temperature and time, were studied, and the optimal conditions were established. The linearity for the target pesticides was from 0.01 to 2 ng/g, and the detection limits were between 0. 001 and 0. 05 ng/g. The proposed approach was applied to the determination of pesticides in vegetable samples, and the recovery for the pesticides spiked in vegetables at 4 ng/g ranged from 50.5% to 103%.

关 键 词：固相微萃取 农残检测 气相色谱 

分 类 号：O657.71[理学—分析化学]