| Salbutamol and Terbutaline, a selective β2-receptor agonist, can effectively inhibit the release of allergic substance such as histamine, bronchial spasm, and are applied clinically in bronchial asthma, bronchospasm, obstructive emphysema, chronic asthmatic bronchitis disease and so on. The addition of a trace of salbutamol and terbutaline in livestock feed can promote muscle growth, inhibit the growth of animal fat, significantly improve the lean meat rate, weight gain and increase the feed conversion rate. They have been used as the promoting agent of animal growth and feed additive. If people take in such animal food containing salbutamol and terbutaline, drugs will continue to accumulate in the body. When they reach a certain degree, they will produce toxic effects on the human body causing acute or chronic poisoning reactions. Normally the chances of drugs in food residues causing acute poisoning events are low. It is mostly the accumulation of chronic poisoning, which may also lead to carcinogenic, teratogenic, mutagenic effects and do great harm to human health. Therefore, the establishment of a simple, rapid and sensitive method for the detection of Salbutamol and Terbutaline residues has practical significance for the safety monitoring of food derived from animals.In alkaline medium, Ni(IV) complex with luminol produce a stable chemiluminescence(CL) signal. Salbutamol and terbutaline can significantly enhance the CL intensity, and substance concentration show a good linear relationship within a certain range. In this paper, Ni(IV) complex- Luminol chemiluminescence system coupled with flow-injection is developed for the determination of salbutamol and terbutaline. PART 1 Ni(IV)-Luminol chemiluminescence system coupled with flow injection for determination of salbutamol in Urine and feed samplesObjective: To establish a new method by Ni(IV)-Luminol chemiluminescence system coupled with flow injection for determination of salbutamol in sulfate tablets, urine and animal feed.Methods: Under alkaline conditions, Ni(IV) complex with Luminol produce a stable CL signal. Salbutamol can significantly enhance its base signal, and the concentration of sample show a good linear relationship within a certain range. Through optimizing the concentration of Luminol solution, Ni(IV) concentration, and alkalinity concentrations in luminol and Ni(IV) solution, a standard curve of salbutamol is drawed. At the best detection conditions, a new method by Ni(IV)-Luminol chemiluminescence system coupled with flow injection for determination of salbutamol in sulfate tablets, urine and animal feed is established.Results: Under the optimized experimental conditions, salbutamol detection limit is 1.0×10-11 mol/L, and there is a good linear relationship within a range of 1.0×10-9 mol/L ~ 5.0×10-7 mol/L. The limits of detection is 1.0×10-11 mol/L for salbutamol. Relative standard deviations(n= 13) is 1.72% for 5 ×10-8 mol/L salbutamol. Under optimum conditions, the proposed method has been applied to the analysis of tablets, urine and swine feed samples with satisfactory results.CL intensities are proportional to the SAL and TEB concentration in the range of 1.0 × 10-9 M to 5.0 × 10-7 M and 1.0 × 10-9 M to 1.0 × 10-7 M, respectively. The limits of detection(3σ) are both 1.0 × 10-11 M for SAL and TEB. Relative standard deviations(n = 11) are less than 2% for 5.0 × 10-8 M SAL and TEB. Possible reaction mechanisms for the CL system are suggested based on the CL system spectra, Ni(IV) complex oxidation characteristics, and free radical trapping experiment. The proposed method has been applied to the analysis of urine and swine feed samples with satisfactory results.Conclusion: A new Ni(IV)-Luminol CL system with flow injection, luminescent method is established, which is simple, sensitive, rapid, accurate and reliable, and can be used for the determination of salbutamol in albuterol sulfate tablets, urine and animal feed samples with satisfactory results PART 2 Ni(IV)-Luminol CL System with Flow injection for determination of TerbutalineObjective: To establish a flow injection-Ni(IV)-Luminol CL system for determination of Terbutaline in sulfate tablets, urine and animal feed.Methods: Under alkaline conditions, Ni(IV) complexes with Luminol produce a stable CL signal. Terbutaline can significantly enhance the base signal, and the concentration of sample show a good linear relationship within a certain range. Through optimizing the concentrations of luminol solution, Ni(IV) solution, alkalinity concentrations in luminol and Ni(IV) solution, a standard curve of terbutaline in the best detection conditions is drawed. A flow injection method for the determination of terbutaline based on Ni(IV)-Luminol CL system is established.Results: Under the optimized experimental conditions, The detection limit of terbutaline is 1.0×10-11 mol/L, and there is a good linear relationship within a range of 1.0×10-9 mol/L ~ 1.0×10-7 mol/L.Relative standard deviations(n= 13) is 1.76% for 5×10-8 mol/L terbutaline. Under optimum conditions, the proposed method has been applied to the analysis of tablets, urine and swine feed samples with satisfactory results.Conclusion: A new Ni(IV)- Luminol CL system with flow injection method is established, which is simple, sensitive, rapid, accurate and reliable, and can be used for the determination of terbutaline in terbutaline sulfate tablets, urine and animal feed with satisfactory results.PART 3 Proposed the Chemiluminescence reaction mechanism of Salbutamol and TerbutalineSalbutamol and terbutaline are β2- stimulant drugs with similar chemical structures. In the determination of Ni(IV)-Luminol CL system, two drugs both enhance the CL intensity of the system, so it is supposed that their reaction mechanisms should also be similar. The UV visible spectra, fluorescence spectra and CL spectra of Ni(IV)-luminol salbutamol/terbutaline CL system are studied by scanning or determination. Through the analysis of the spectra, the possible CL reaction mechanism of this system is inferred as follows:The reactions of Ni(IV), Luminol and salbutamol /terbutaline are free radical reactions. The reactions of salbutamol / terbutaline and Ni(IV) is much faster than that of Lumino with Ni(IV). And in the reaction process, free radicals generated by salbutamol or terbutaline partially transfer to luminol, so that the luminol free radicals increased. Thereby the luminescence species of luminol are increased, so that the CL intensity of the system enhanced. |
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