| Selenium has been considered a toxic substance since its discovery in 1817,and its role in animal growth was not discovered until it was used to treat Keshan disease in1979.With scientific progress and people’s increasing demands on the quantity and quality of food,the amount of selenium-rich feed used is also rising rapidly.Compared with the traditional selenium-rich feed,the selenium methionine has the advantages of low toxicity,high absorbability and stable chemical structure,so it has a large market space.However,it is difficult to popularize selenomethionine in the market because of its long synthetic route,expensive raw material price and many three wastes.It is necessary to optimize the synthesis process of selenomethionine in order to find a simple synthesis route,cheap and easy to obtain raw materials,less three wastes and mild process.In order to solve the above problems,this paper studied and designed the low cost methionine and benzyl chloride compounds as raw materials,through one-step reaction to prepare and purify the important intermediate of high serine lactone hydrochloride,the yield reached 66.17%.Then dimethyl diselenium ether,an important intermediate,was synthesized from selenium powder,hydrazine hydrate and dimethyl sulfate with a yield of85.72%.Finally,after the reduction reaction of dimethyl diselenium ether and the hyperserine lactone hydrochloride,the product was purified to obtain a crude selenomethionine with a purity of 22.70%,with a yield of 41.73% and a total synthetic yield of 23.67%.Orthogonal test was used to optimize the synthesis process of the hyperserine lactone hydrochloride and the synthesis process of selenomethionine.The synthetic route is simple,the raw materials are cheap and easy to be obtained,the three wastes are less,and the process is mild.In this paper,the methodological reliability evaluation of the HPLC method for the determination of selenomethionine was carried out.Using methanol: 0.6% potassium phosphate buffer = 5:95(V/V)as the mobile phase and PDA as the detector,the stability of se-methionine solution in this fluid system was investigated.In order to evaluate the accuracy of the method,we use the sample recovery rate to analyze the reliability of the method.The results showed that the se-methionine solution in the mobile phase system was stable and had a good linear relationship within the concentration range of 50-1000 PPM,with a linear coefficient of 0.99998 and a standard recovery of 98.11-102.11%,indicating that the se-methionine detection method had a good linear relationship and accuracy in the concentration region.This paper to explore itself’s ability to remove free radicals,containing selenium compounds for already on the market of traditional selenium-rich feed including yeast selenium and sodium selenite with selenomethionine hydroxyl radical and superoxide anion free radical scavenging ability with the research and experiment results show that the 0.10mg/m L selenium yeast on superoxide anion free radical and hydroxyl free radical clearance is 19.09 37.87% and 24.40 58.94% respectively;The scavenging rates of 0.10 mg/m L sodium selenite were 13.94% and 13.54% respectively.The scavenging rates of 0.10mg/m L selenomethionine were 16.77% and 18.97% respectively.The order of scavenging ability of two kinds of free radicals was yeast selenium > selenium methionine > sodium selenite.It provides basic data reference for the study of free radical scavenging capacity of selenium. |
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