苯丙共聚物-聚硅氧烷复合固相微萃取涂层的制备及性能研究  

Preparation and Investigation of Solid Phase Microextraction Complex Coating of Phenylethylenethyl Acrylate Copolymer and Polymethylsiloxane

作　　者：申书昌[1] 付双[1] 王文波[1] 肖忠峰[1] 张维冰[2] 

机构地区：[1]齐齐哈尔大学化学化工学院,黑龙江齐齐哈尔161006 [2]中国科学院大连化学物理研究所,辽宁大连116011

出　　处：《分析测试学报》2006年第1期12-15,共4页Journal of Instrumental Analysis

基　　金：黑龙江省自然科学基金资助项目(B01-03)

摘　　要：合成了苯乙烯-丙烯酸乙酯共聚物，以此聚合物与甲基聚硅氧烷色谱固定液混合作为固相微萃取头涂层。通过热分析手段考察了该涂层的热稳定性，涂层使用温度可达280℃。使用微量进样器和不锈钢毛细管，自制了SPME装置。使用该涂层萃取分析了水中氯苯系化合物，各标准样品质量浓度在0—20μg／L内与色谱峰面积呈良好线性关系（r=0．9674—0．9934），检出限为0．28—0．64ng／L，相对标准偏差为5．4％-7．7％，加标回收率为91％-99％。将自制涂层与商品涂层（PDMS、PA）进行了比较，结果表明苯丙聚合物-甲基聚硅氧烷复合涂层对氯苯系化合物具有优良的吸附特性。在固相微萃取研究和应用中，提供了新的吸附物质和色谱固定液与石英纤维结合的新途径。Phenylethylene - ethyl acrylate copolymer was synthesized. The copolymer was combined with polymethylsiloxane to prepare SPME extraction coatings. The thermostability of the coating was investigated by thermal analysis, and the maximum sustainable temperature for the coating was as high as 280℃. The SPME equipment was custom-made using microinjector and stainless steel capillary columns. The coating was used to detect and analyze chlorobenzenes in water. In 0 -20μg/L, the linear relationship between the contents of the standard samples and their areas was good. The correlation coefficients（r） were in the range of 0. 967 4 -0. 993 4. The detection limits were in the range of 0.28 - 0. 64 ng/L, with relative standard deviations ranging from 5.4% to 7.7%. The average recoveries in spiking experiments were in the range of 91% -99%. In comparison of the complex coating with commercial coating（ PDMS and PA）, the experimental results indicated that the complex coating had superior sorption capacity for chlorobenzenes. The present study a new adsorbent and a procedure to combine GC stationary liquid with guartz fibre, which will be useful for further SPME research and applications.

关 键 词：固相微萃取 苯丙共聚物-甲基聚硅氧烷复合涂层 氯苯系物 色谱 

分 类 号：O657.71[理学—分析化学] O658.1[理学—化学]