Preparation Of A Novel Stir Bar Sorption Extraction Based On Hydroxyl Cucurbituril And Its Application In Determination Of Drugs In Biological Fluids

Solid-phase Micro-extraction(SPME) is a novel solvent-free sample preparation technique which combine sample extraction, detachment and injection. It has the advantages of convenient operation, high extraction efficiency, and high sensitivity.There had been various methods such as Fiber solid-phase micro-extraction(Fiber SPSE), tube solid-phase micro-extraction(In- tube SPSE), Stir Bar Sorption Extraction(SBSE), and so on. Because the Fiber SPSE stationary phase volume was small and easy to fracture, therefore, larger SBSE coating gradually began to develop in recent years. SBSE have the advantages of high enrichment factor, good reproducibility, but at present SBSE also was restricted by some factors including less species and expensive goods. What's more, the coating mostly was polydimethylsiloxane(PDMS). It is mainly used for extraction nonpolar or weak polar component, but its adsorption selectivity was poor. Thus, the coating which is of high extraction efficiency, wide selectivity, and suitable for analysis of the polar material have become the key to the development of the SBSE technology. In this thesis, through the sol-gel provided a novel PDMS/OH-Q[7]-SBSE coating material,uesd SBSE-HPLC to extraction different polar durgs in water and biological fluids.The main contents were as follows:1. Introduction of the three main forms of SPME technology: Fiber SPME?In-tube SPME ? SBSE. Their principle and device were illustrated and the applications of SBSE were introduced respectively.2.(HO)-Q[7],which was Synthetized by photochemical method, then it was separated and purified by silica gel column chromatography.Strucctural characterization of(HO)-Q[7] was determined by Infrared spectroscopy(IR), nuclear magnetic resonance techniques(1H-NMR) and mass spectrometry(MS). The results was indicated that(HO)-Q[7] purity can be reached over 95%.3. PDMS/(HO)-Q[7] coating was prepared by sol-gel technique.Optimized conditions of Preparation of PDMS/(HO)-Q[7] Coating; IR characterization proved that coatingstructure(HO)-Q[7] was involved in the reaction. SEM proved that the coating is relatively dense and there are no cracks. PDMS/(HO)-Q[7] coating have good solvent resistance, homogeneity and wear resistance.4. Established a analysis method of PDMS/(HO)-Q[7]-SBSE-HPLC for determination of different polar compounds(phenol, amine, ketones, polycyclic aromatic hydrocarbon) in the water.The linear range of analytical method was0.005-10?g/m L, detection limit was 2.12-34.5 ng/m L, enrichment factor was between2.6 and 22.1 times. In terms of the analysis of environmental water, the samples average recovery are between 92.2%-103.1%, RSD% between 5.6 %-7.8%.5. Used PDMS/(OH)-Q[7]-SBSE coating were critically compared with blank PDMS-SBSE coating for the extracion p-Nitroaniline, 2,6-Dimethyl phenol,Benzophenone, Fluorene,and the results showed that PDMS/(OH)-Q[7]-SBSE exhibited highest extraction efficiency;and discussed its extraction mechanism by Ultraviolet Specterphotometry.6. Establigshed a analysis method about PDMS/(HO)-Q[7]-SBSE-HPLC for determination of NSAIDs(ibuprofen, meiloxicam, naproxen, diclofenac) in urine. The linear range of analytical method was 0.001-10?g/m L,detection limit was0.4-22.6ng/m L,enrichment factor was between 4.01 and 61.13 times. Analysis of NSAIDs of average recovery between 91.0%-112% in urine, RSD between1.02%-8.69%.7. Used PDMS/(OH)-Q[7]-SBSE coating were critically compared with blank PDMS-SBSE coating for the extracion ketoprofen, diclofenac, ibuprofen,meloxicam,,and the results showed that PDMS/(OH)-Q[7]-SBSE exhibited highest extraction efficiency; Discussed its extraction mechanism by ITC.And used the establigshed method for detection of the actual urine samples,achieved satiafactory results.