Application Of A New Capillary Zone Electrophoresis-chemiluminescence Method In Determination Of Veterinary Drug Residues In Animal Derived Food

In alkaline medium, Ag(III) complex oxidant with luminol could be composed chemiluminescence system. Ag(III) complex can oxidize luminol to produce chemiluminescence, which is the baseline signal. Some substances can significantly enhance or inhibit Ag(III)- luminol chemiluminescence intensity, and the chemiluminescence relative intensities displayed a good linear relationship to the concentration in a certain range. The content of the drug can be measured according to the relationship between the degree of enhancement or inhibition of the Ag(III) complex-luminol system and the concentration of the drug. Capillary electrophoresis(CE) has high separation efficiency, decrease the dosage of solvent and sample, running lower costs, wide linear range, speed analysis and equipment is relatively simple, widely used in the fields of life science, environmental science and clinical medicine. The chemiluminescence has the advantages of high sensitivity, cost is low, easy assembly, no need of the light source to avoid the influence of stray light on the determination.In this paper, the Ag(III) complex-Luminol chemiluminescence system with capillary zone electrophoresis was combined, which is applied to the detection of the residues of the sulfonamides and tetracycline in animal foods.In this study, Ag(III)-luminol with high sensitive chemical chemiluminescence system,as efficient separation technology for capillary electrophoresis chemiluminescence detection system, for the detection of animal source food of residues veterinary drugs.Concentrated samples were purified by solid phase extraction technology, using capillary electrophoresis separation, and using chemiluminescence detection system detection, the new method of detection sulfonamides and tetracycline was established, the procedure is simple and fast, the results are sensitive and reliable. PART 1 Determination of sulfonamides residues in food by capillary Zone electrophoresis-chemiluminescence methodObjective: To establish a new Ag(III) complex and Luminol new chemiluminescence system in alkaline medium, combined with capillary electrophoresis, and a new method for the simultaneous separation and determination of 3 sulfonamides residues in animal foods.Methods: Pork, chicken, milk samples by SCX, HLB solid-phase extraction column purified and concentrated, by and by, using capillary electrophoresis electrochemical luminescence determination of the content of the sulfamethoxazole, sulfadimethoxine, sulfathiazole. The sulfonamides compounds by capillary electrophoresis separation, respectively with Ag(III)-luminol chemiluminescence system, and it has significant inhibitory effect in this chemical luminescence system, relative migration time qualitative relative chemiluminescence quantitative intensity, using standard curve method for the determination of samples of measured matter content. The conditions for the separation and chemiluminescence detection system were all optimized. Under the optimum conditions, the treated samples of pork, chicken, and milk processed were analyzed.Results: Under the optimized conditions, the linear ranges for the determination of SMZ, SDM, and ST are 2.0~200.0 ug/mL(r>0.9977), with detection limits(S/N=3) of 0.035, 0.20 and 0.35 ?g/mL, respectively. Relative standard deviation(RSD) values for the peak height are 1.3% to 1.9%(n=7), the recoveries of standard addition was in rang of 80.2%~102.9%.Conclusion: The method was applied to detection 3 sulfonamides residues in pork, chicken and milk samples. The operation is simple, rapid, accurate and reliable, and the result is satisfactory. PART 2 Determination of tetracycline residues in milk by capillary Zone electrophoresis-chemiluminescence methodObjective: To establish of Ag(III)-luminol new chemiluminescence system. In alkaline medium, a new analysis method was established of detection oxytetracycline and minocycline residual in milk by capillary electrophoresis separation.Methods: Oxytetracycline and minocycline followed by separation in capillary electrophoresis, respectively with Ag(III)-luminol chemiluminescence system role, oxytetracycline on the system have significant sensitizing effect, minocycline is of the system have significantly inhibited, and the chemiluminescence intensity and the concentration of the samples displayed a good linear relationship within a certain range. Milk samples by HLB solid phase extraction purification and concentration. By optimizing the condition of the method, the optimum condition: The concentration of Ag(III) complex is 8.0×10-5 mol/L(in 0.02 mol/L NaOH); buffer solution: 2.5×10-3 mol/L luminol, 1.4×10-2 mol/L sodium borate solution;16 kV Voltage;18 s sampling time.Results: Under the optimal separation and detection conditions, minocycline in 0.75~72.5 ?g/ml range good linearity(r>0.9976), oxytetracycline in 5.0~ 100.0 ?g/ml range with good linearity(r>0.9954), to minocycline and oxytetracycline parallel determination 7 times and the relative standard deviation(RSD) respectively 2.3%, 2.1%. Minocycline and oxytetracycline detection limits were 0.05 ?g/ml, 0.45 ?g/ml, respectively, of milk samples were spiked recovery rate determination, the result is 84.0% ~ 103.1%.Conclusion: To establish a new method for the simultaneous determination of minocycline and oxytetracycline content in milk by capillary zone electrophoresis chemiluminescence method. The method is accurate and reliable, and the method is accurate and reliable. It can be used for the analysis and detection of milk samples in the market.