The Preparation Of A Novel β-cyclodextrin Polymer Coating And Its Application In Solid Phase Microextraction

Solid phase microextraction(SPME)was first proposed by professor Pawliszyn in 1989,which is a novel sample pretreatment and enrichment technique.The development of SPME is based on solid phase extraction(SPE),which integrates sample collection,extraction and enrichment.It retains the advantages of SPE such as method efficient,reliable in results and less solvent consumption.SPME solves the problems of SPE,which need column filler and solvent desorption.SPME device can complete all the pretreatment and sampling work,become the sample pretreatment technology widely used in the method.Nowadays,it widely used in pretreatment technology.(3-cyclodextrin(β-CD)has a special structure of hydrophobic inwall and hydrophilic outwall.Its hydrophobic cavity is similar to the shape of flowerpot,which can be used as the subject to envelop the appropriate guest molecule formed host-guest inclusion complex,complete the recognition process of each other.Based on its unique structure,non-toxic and easy to be modified,β-CD and its polymers have been widely used in the field of sample pretreatment.However,the reports of various kinds ofβ-CD polymers have a lower surface area and adsorption performance than traditional activated carbon(AC).The porous β-CD-containing polymers(P-CDP)prepared by tetrafluoroterephthalonitrile as crosslinking agent is different from other polymers,which has a high surface area and adsorption properties;using decafluorobiphenyl as crosslinking agent prepared β-CD polymers(Decafluorobiphenyl P-CD-containing polymers,DFB-CDP)has a high affinity for perfluorooctanic acid,although it is no pores and has a low surface area.In this paper,two types of novel SPME coatings were prepared by sol-gel technology with P-CDP and DFB-CDP as the coating materials,coupled with gas chromatography-mass spectrometry(GC-MS)established a sensitive analysis method of micropollutants in environmental water samples.This thesis mainly inclueds the following three parts:(1)ReviewReview the development of SPME,including the preparation method of the coating and the type of coating materials.Summary and commentary on P-CD and its polymers application of micropollutants analysis in environmental water samples.(2)Preparation of novel P-CDP coating and its application in SPMEThe P-CDP was characterized by infrared spectrum(FT-IR)and N2 adsorption-desorption proved successfully synthesis.A newly P-CDP coating was prepared by sol-gel technology,characterized by thermogravimetry and environmental scanning electron microscopy(ESEM)to investigate the morphology and characteristics.The prepared coating coupled with GC-MS used to establish the analytical method of volatile organic compounds and odours substances in water samples.The method obtained a good linear in the range of 0.01-120 μg L-1(R2 ＝0.9946),the detection limit was 3 ng L-1.Repeated experiments demonstrated that the coating could extract 130 times the performance remained stable.Reproducibility experiment showed that the coating prepared by same batch and different batches relative standard deviation(RSD)was 1.7 and 1.9,respectively.(3)Preparation of novel DFB-CDP coating and its application in SPMEA newly DFB-CDP coating was prepared by sol-gel technology.The structure and morphology of the coating were investigated by FT-IR,N2 adsorption-desorption,thermo gravimetry and ESEM.The prepared coating coupled with GC-MS used to detect perfluorooctanoic acid in water samples,the method obtained a good linear in the range of 0.05-5 μg L-1(R2 = 0.9938).Application in real samples the method accored with the requirements.