Determination Of Commonly Used Antibiotics In Fishery Drugs By Chemiluminometry

Antibiotics is the general term for chemicals with the specific inhibition to somebiological activities of life in low concentration. In recent years, with the developmentof society, in order to meet the needs of life, the expansion of aquaculture was oncelarge-scale and centralized. Under the intensive mode of development, a variety ofdiseases caused by bacteria or micro-organisms has brought great losses to aquaculture.In order to control the diseases to make losses unnecessary reduce, frequency ofantibiotics using was increasing. Therefore, the establishment of the detection ofantibiotics in the water environment is undoubtedly an significance work.Chemiluminescence （CL） is a trace analysis method that is based on light radiation generated by chemical reaction （chemiluminescence） to determine the content of materials. The technology with low background, high sensitivity, wide linear range and simple instruments makes it a sensitive optical detection technology. So that CL technology has become an effective method for micro and trace analysis.The chemiluminescence reaction is divided into direct chemiluminescence andindirect chemiluminescence. In the chemiluminesce reaction, the luminescenceintensity is enhanced or weakening because of the foreign inorganic ions or organiccompounds joining into the CL system. Two detection methods of the enhancedchemiluminescence and inhibited chemiluminescence are established on this. Theinjection of chemiluminescence analysis is divided into two types: static-injection andflow-injection.In this study, the content of three kinds of aquaculture antibiotics（chlortetracycline,oxytetracycline, nitrofurazone） in fishery drugs have determined by the establishmentof the chemiluminescence reaction system.This thesis is divided into two main parts, the first part is the overview,and thesecond part is the research report.In the section of the review, it briefly introduced the usage of the aquaculture inthe global antibiotics with its consequences, and the principles, techniques onchemiluminescence analysis method. Then it summarizes the application of thechemiluminescence method used in the antibiotics detection.The research report consists of five parts:According to the principle that chlortetracycline can sensitize the chemiluminescence system of KMnO4‐Na2SO3, a method with static injection to determine chlortetracycline was set up. Under the best conditions, the chemiluminescence intensity was found to respond linearly to the concentration of chlortetracycline, ICL=220.31x+18.89, R2=.9794, with the detection limit of2.0×10-8mg/L. Precision of the method was tested at the concentration method level of1.0mg/L and the RSD′s （n=11） found was7.13％. The proposed was applied to the analysis of chlortetracycline hydrochloride ointment, giving values of recovery in the range96.9%¹02.5%, and the average recovery was993%.The results obtained were satisfactory.2) It was found that in the alkaline solution, chemiluminescence, produced by thereaction system of copper （II） ions-luminol-hydrogen peroxide, was remarkablyinhibited by the presence of oxytetracyline, and the magnitude of decrease ofchemiluminescence intensity was found to be directly proportional to the concentrationof oxytetracyline. Based on these facts, a method of static injection chemiluminescencedetermination of oxytetracyline was proposed. Linearity was kept in the range2.0×10-7mol/L¹.0×10-5mol/L with a detection limit of4.97×10-8mol/L. Precision of themethod was tested at the concentration method level of1.0×10-5mol/L and the RSD′s（n=11） found was2.20％. The proposed was applied to the analysis of oxytetracyclinehydrochloride soluble powder, giving values of recovery in the range97%¹03%, andthe average recovery was100.67%.The results obtained were satisfactory.3) According to the principle that nitrofurazone can sensitize the chemiluminescence system of H2SO4‐KMnO4, a method with static injection to determine nitrofurazone was set up. Under the best conditions, linearity was kept in the range2.5×10^‐6mol/L⁴.0×10^‐5mol/L （y=10.269x+5.6963, R²,=0.9887）with a detection limit of1.26×10^‐6mol/L. Precision of the method was tested at the concentration method level of2.0×10^‐5mol/L and the RSD′s （n=11） found was2.00％. The proposed was applied to the analysis of nitrofurazone powder, giving values of recovery in the range92%⁹6%, and the average recovery was93.67%.The results obtained were satisfactory.4) According to the principle that HCHO can sensitize the chemiluminescence system of OTC-KMnO4-HCl, a method with flow injection to determine oxytetracyline was set up. Under the best conditions, linearity was kept in the range0.4⁶0mg/L （y=12.86x‐2.13, R²=0.9906）with a detection limit of0.28mg/L. Precision of the method was tested at the concentration method level of10mg/L and the RSD′s （n=11） found was3.4%. The proposed was applied to the analysis of oxytetracycline hydrochloridesoluble powder, giving values of recovery in the range99.2%¹02.7%, and the average recovery was101.1%.The results obtained were satisfactory.5) According to the principle that Co2+can inhibit the chemiluminescencesystem of CTC-NaOH-Luminol-KIO4, a method with flow injection to determinechlortetracycline was set up. Under the best conditions, linearity was kept in the range1.0×10-7¹.0×10^-5g/L （y=12.86x-2.13, R²=0.9906）with a detection limit of2.0×10^-8g/L. Precision of the method was tested at the concentration method levelof10mg/L and the RSD′s （n=11） found was2.7%. The proposed was applied to theanalysis of chlortetracycline hydrochloride soluble powder, giving values of recoveryin the range98.5%¹01.2%, and the average recovery was100.2%.The resultsobtained were satisfactory.