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Molecularly Imprinted Solid-phase Extraction And Flow-injection Chemiluminescence For Trace Analysis Of Sulfanilamide

Posted on:2017-01-16Degree:MasterType:Thesis
Country:ChinaCandidate:L Y L ZhangFull Text:PDF
GTID:2271330485970572Subject:Nanophysics and Chemistry
Abstract/Summary:PDF Full Text Request
Sulfanilamide belongs toantimicrobial agents, for the variety of the typesand the low manufacturing cost, it was wildly used for the treatment of various bacterial diseases. But the abuse of sulfanilamides may cause harm, so monitor the concentration ofthose is important. At present, the main detection methods of the sulfanilamides are almost concentrate in the high performance liquid chromatography. The expensive equipment, difficult to operate, complicated pretreatment and requirement of seniortechnicalpersonnel make it slow to developed, especially in the villages and towns where the source of these pollution came out. So we need to figure out a more easily detction method to deal with this.Chemiluminescence was an analysis method with high sensitivity and short analysis time. It was widely used in environmental surveillance, pharmaceutical analytical and food detecting. But the characteristics of low slectivity limit it’s development. So figure out a method to compensate the selectivity is needed.Molecular imprinted polymer(MIP) is asynthetic materialwith desired recognition site. With those site it can specificity binding the target molecule and this made those material have the function of separation and enrichment. Combine this with the CL system, it can enrich our target molecule in the flow path and separate it from the complex sample which just compensate the method of chemiluminescence.In this paper, we established several systems of chemiluminescence to detect the sulfonamides and two of them were detcted with the molecular imprinted polymer. Themore details of this paper can be provided next:First we established a flow injection chemiluminescence method to detect the acrylamide. This new method was easy to operate with a lower request of instrument and suitable for daily monitoring. In hydrochloric acid medium, the acrylamide inhibited the chemiluminescence of vitamin C intermixed with potassium permanganate and methanal. Under the optimum condition, the chemiluminescence intensity was linear with the concentration of acrylamide over the range from 4.0×10-5g/L to 1.0×10-3g/L, and the limit of detection was 5.0×10-6g/L. The relative standard deviation(n=11) was 2.7% for acrylamide with concentration of 5.0×10-4g/L.Then we found that in hydrochloric acid medium, the sulfamerazine could increase the intensity of potassium permanganate-formaldehyde system. So we eatablished a new flow injection chemiluminescence method to detect it’s concentration. This method had some advantages like easy to operate, cheap reagent, high sensitivity and low detection limit. The chemiluminescence intensity was linear with the concentration of sulfamerazine in the range from 0.8×10-4mol/L to 1.5×10-3mol/L. The limit of detection was 1.0×10-5 mol/L. The RSD(n=11) was 3.8% for the concentration of 7.0×10-4mol/L.After that we used highly sensitive flow-injection chemiluminescence sysytem and combined it with the molecularly imprinted solid-phase extraction to analysis sulfamethoxazole(SMX). The molecularly imprinted polymer of sulfamethoxazole was made by diethylenetriamine(DETA), polyethylene glycol and epoxy resin. We choose diethylenetriamine as the monomer, polyethylene glycol as porogenic agent and epoxy resin as the cross-linker. The sulfamethoxazole was absorbed selectively by the MIP and the absorbed sulfamethoxazole was analysised on the chemiluminescence reaction of acidic potassium permanganate and formaldehyde. The CL intensity was linear in the range from 5.0×10-5mol/L to 1.2×10-3mol/L. The LOD(S/N=3) was 2.0×10-5mol/L, and the relative standard deviation(n=11) was 3.3% for the concentration of 5.0×10-4mol/L. This method had been successfully applied to detect the sulfamethoxazole content in a sulfamethoxazole tablet.At last we found that the sulfamethazine sodium can also increase the chemiluminescence intensity of potassium permanganate-formaldehyde system. So we used the diethylenetriamine(DETA), polyethylene glycol and epoxy resin together and made the sulfamethazine sodium moluecularly imprinted polymer. The intensity was linear with the concentration of sulfamerazine in the range from 0.7×10-4mol/L to 1.6×10-3mol/L. The limit of detection was 5.0×10-5 mol/L. The RSD(n=11) was 4.4% for the concentration of 8.0×10-4 mol/L.
Keywords/Search Tags:Molecular imprinting, Flow injection chemiluminescence, Sulfanilamide
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