Study On Synthesis Process Of Diosmin Under Ultrasonic Condition

Diosmin, named barosmin, was a kind of natural flavonoid glycosides compounds, the chemical name was 3’,5,7—trihydroxy—4’—methoxy flavones. It couldn’t satisfy the demand of modern medical treatment duing to the very low concentration of diosmin from natural plants, so now hesperidin was ulizied as raw material to synthesis medicinal diosmin through chemical process. Thus in this experiment ultrasound-assisted technology was applied in diosmin synthesis process, Through the response surface design of experiments to explore the optimum condition of ultrasonic-assisted synthesis of diosmin and to establish the polynomial quadratic equation model. And the synthetic product was validated with multiple spectrum methods. Also, the iodine-containing water could be disposed reasonably in this experiment. This provided important basis for a clean way of diosmin synthesis.⑴ According to single factor experiment and response surface methodology, it determined that the optimum synthesis conditions of diosmin were as follow: ultrasonic power 700 W, ultrasonic time 25 min, reaction time 5.6 h, reaction temperature 120 ℃. Four factors including ultrasonic power, ultrasonic time, reaction time and reaction temperature were optimized using central composite design and response surface methodology based on single factor investigations for achieving maximum the synthesis yield. With the help of Box-Benhnken central composite design and response surface analysis theory, the interaction of the respective variables and their influence on the yield was studied. Also the predictive model of polynomial quadratic equation was analyzed by Design Expert software. They were discussed for the key factors affecting ultrasonic synthesis and their interactions by the response surface and contour of the model, under these conditions, the average yield was 21.35%, compared to theoretical value, the respective relative error was 1.97%.⑵By applying various spectroscopic methods, such as infrared absorption spectrum, high performance liquid chromatography(HPLC), electrospray mass spectrometry, high resolution mass spectrometry and nuclear magnetic resonance spectrum,ect, and combined with the spectrum character information of diosmin standards, the product was identified as diosmin.⑶Cu SO4、Na2S2O3 were respectively used as the precipitator, reducer to settle down the iodine from the waste water that produced from the synthetic reaction process, cetrimonium bromide was used as flocculant to accelerate the precipitation, Fe Cl3 was used as the oxidant to oxidize Cu I to iodine, and then the obtained iodine was purified by the sublimation. Three factors including amount of Na2S2O3、Cu I reaction time and amount of Fe Cl3,the interaction of the respective variables and their influence on the rate were using orthogonal array design based on single factor factor investigations for achieving maximum the recovery rate of iodine. According to the range analysis, the result indicate that the optimum recovery conditions of iodine were as follow: 2.5 times theoretical value of Na2S2O3, Cu I reaction time 20 min, 1.4 times theoretical value of Fe Cl3. Under these conditions, the average recovery rate was 88.56%, the purity of obtained iodine was 95.86%.