To Study Influencing Factors Of The Reaction Of Luminol-Ag(Ⅲ) Complex Chemiluminescence System And The Mechanism Of The Reaction And Detection Of Hexestrol In Milk By Capillary Electrophoresis With Chemiluminescence Contained Ag(Ⅲ) And Luminol Prepara

PART 1 Preparation of Nylon 6 Nanofibrous Membrane for Adsorption ofHexestrolObjective: To prepare nanofibrous membranes of Nylon 6 and study the adsorption properties of nylon 6 nanofibrous membranes for Hexestrol.To provide the basic theory for the process of food and biological sample spretreatment applied for the detection of Hexestrol milk.Methods: To obtain the concentration of 30% nylon 6 solution, at room temperature, the nylon 6 and the mixed solvent contained acid- cresol(6:4,V:V) are mixed for s12 hours. To take solution into the syringe with stainless steel needle(21). The main experimental conditions are as follows:the speed of injection is 0.02mm/min,the distance between collecting screen and the needle is 15 cm, 22 kv voltage is applied. The process of experiment last for 8~10hours. To detect the concentrations of hexestrol by high performance liquid chromatography(HPLC). Using static and dynamic adsorption method to stutied the adsorption properties of nylon 6 nanofibrous membranes for Hexestrol. The influences of adsorption time, initial concentration of Hexestrol and p H value of medium are investigated. The results indicated that when the initial concentration of Hexestrol was 2mg/L, the adsorption process of nylon 6 nanofibrous membranes obeyed the Pseudo-first-order kinetic model; and when the initial concentration was in the range of 5~20mg/L, the adsorption process accorded with the Pseudo-second-order kinetic model. The adsorption process of Hexestrol with nylon 6 nanofibrous membrane accorded with Freundlich isothermal adsorption model. Physical adsorption and chemical adsorption dominate the adsorption process, but physical adsorption play a more important role.The experiment are repeated 7 times, the result indicates that nylon 6 nanofibrous membranes is a new material which is characteristic of good efficiency and green can be cyclicly used.Conclusions: Nylon 6 nanofiber membranes that can achieve enriched Hexestrol of milk samples,is highly efficient adsorption material. Nylon 6 nanofiber membranes is also a new adsorption material which is characteristic of green can be cyclicly used. PART 2.To Study Influencing Factors of the Reaction of Luminol-Ag(III)Complex Chemiluminescence System And the Mechanism of the ReactionObjective: To study influencing factors of the reaction of Luminol-Ag(III) complex chemiluminescenceem system,and explicate more fundamental mechanism of the reaction.Methods: the reaction of Luminal,Ag(III) complex and sample is achieved by flow injection chemiluminescence apparatus. At the same time, we recorde the chemiluminescence intensity.Experiment makes use of nitrogen to eliminate air dissolved in each solution and sustainingly protect the environment of the reaction.In initial time,we recorde the chemiluminescence intensity.And after the reaction beginning, we recorde the chemiluminescence intensity every half hour until 7 hours.The same experiment was reapted one time per day last for three days.Set up contrast experiment that do not protect the environment of reaction by nitrogen.In order to explore a way how can ensure repeatability of the chemiluminescence intensity, we analyze the results of the experiment Under the condition of ensuring reproducibility, relations between tthe chemiluminescence intensity and different concentrations of Luminol,Ag(III) Complex,Sodium Formate,SDS,Na CO3,Nano Silver that take part in the reaction and the value of p H of the reactive environment were studied by single variable method.Results: The experimental results show that after making use of nitrogen to eliminate air dissolved in each solution and then to sustainingly protect the environment of the reaction last for 4 hours, the chemiluminescence intensity have a stable condition which last for 3 hours. In this stable period, the chemiluminescence intensity have a good reproducibility and a good linear relationship between intensities and concentrations of samples is showed. The chemiluminescence intensity of Luminol-Ag(III) complex chemiluminescenceem system is strikingly influenced by concentrations of Luminol,Ag(III) Complex which take part in the reaction and the value of p H of the reactive environment.The intensity is also influenced by air and some impurities which were dissolved in each solution have the ability to oxidize.The medium of the reaction have no influence to the intensity,but for the reaction rates.Conclusions: Our work show that carbon dioxide plays an important role to influence the intensity of Luminol-Ag(III) complex chemiluminescenceem system. We establish a new way that makes use of nitrogen to eliminate carbon dioxide dissolved in each solution and sustainingly protects the environment of the reaction to perfectly solve this puzzle to reproducibility. The chemiluminescence intensity has a closely connection with the concentrations of 3- amino acid phthalate two(3-AP) which be generated in the progress of the reaction be called for luminescent intermediate. The environment of the reaction has no influence to the intensity.PART 3 Detection of Hexestrol in Milk by Capillary Electrophoresis WithChemiluminescence Contained Ag(III) and LuminolObjective: To establish a new method for simultaneous determination of Hexestrol,Diethylstilbestrol and Dienestrol in milk by capillary electrophoresis with chemiluminescence.The new method has the characteristics of simple, fast,exact and low consumptionMethods: Based on the fact that Hexestrol,Diethylstilbestrol and Dienestrol can dramatically restrain the chemiluminescence intensity of Luminol-Ag(III) complex chemiluminescenceem system, and there is a good linear relationship between the chemiluminescence intensity and concentrations of samples. The experiment adopts the gravity sampling,and the process lasts for 12 s. An uncoated fused-silica capillary column(50 μm i.d.×80 cm) was used as separation channel. A constant voltage of 14 k V was applied for separation The running buffer contained 2×10-3M Luminol(in5×10-3Na OH+6×10-3Msodium borate). Under alkaline conditions, chemiluminescence is produced by the fast reaction between Luminol and sample that have been separated and Ag(III) complex led into by siphon action in the inspection window. Chemiluminescence is detected and then which’s intensity is boosted by photoelectric multiplier.To use retention time to qualitative and peak height to quantitative.Results: A good baseline separation of Hexestrol,Diethylstilbestrol and Dienestrol is obtained within 15 min. The calibration curves are linear in the range of 0.6~60μg/m L for Hexestrol and 0.5~40 μg/m L for Diethylstilbestrol and 1~60 μg/m L for Dienestrol. Regression equation are y=4.1754x+16.891,y=8.2234x+29.985 and y=2.9433x+13.085, with linear correlation coefficients of 0.9984,0.9934 and 0.9993, respectively. The limits of detection of Dexestrol,Diethylstilbestrol and Dienestrol were 0.57μg/m L,0.35μg/m L and 0.80μg/m L, respectively,with the relative standard deviation(RSD) of 2.38%,1.90% and 1.3%.Conclusions: The method that this paper establish can be applied for the separation and the detection of Dexestrol,Diethylstilbestrol and Dienestrol in milk. This new method is simple, fast,exact and have low consumption, and the result is perfect.