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%.
出处
《分析科学学报》
CAS
CSCD
北大核心
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)
关键词
固相微萃取
农残检测
气相色谱
Solid-phase microextraction
Pesticides
Gas chromatography
Vegetables
