Study On The Preparation, Characterization And Properties Of Rosin Starch Esters

This paper studied the preparation of rosin starch esters (RSE), which is synthesized with starch and rosin in the atmospheric pressure. The properties, structures, dynamics , mechanism and as carriers of Feinuoluofen calcium(FC)'s release effect, were also being researched. The results were as follows:1. Study on the purification method and alkaline of the rosinoyl chloride. The powder rosinoyl chloride is refined by benzene and petroleum instead of ether. The rosinoyl chloride can stay 4 months in the room temperature. The results showed that, compared with ethanol and DMF, the alkali resistance of rosinoyl chloride has better alkali resistance in ethanol than DMF.2. Preparation of the 4 different degrees of rosin starch esters (RSE). In the single factor experiments, the effects of some factors, which include the reaction time, reaction temperature, catalyst, activation time and solvent, on the degree of substitution were studied. According to these results of single factor experiments, analysised and optimizationed of reaction conditions on the degree of substitution by the response surface software. The most optimal process conditions were as follows:The most optimal process conditions of DS=0.0802: n(starch) : n(rosinoyl chloride) 2 : 1,reaction time 6 h, reaction temperature 98℃, catalyst 3.0 mL, activation time 42 min, solvent 23 mL, yield 69.91 %.The most optimal process conditions of DS=0.1252: n(starch) : n(rosinoyl chloride) 1 : 1,reaction time 6.5 h, reaction temperature 95℃, catalyst 3.5 mL, activation time 52 min, solvent 29 mL, yield 65.89 %.The most optimal process conditions of DS=0.4913: n(starch) : n(rosinoyl chloride) 1 : 2,reaction time 8 h, reaction temperature 90℃, catalyst 5.4 mL, activation time 50 min, solvent 40 mL, yield 57.05 %.The most optimal process conditions of DS=0.7518: n(starch) : n(rosinoyl chloride) 1 : 4,reaction time 9 h, reaction temperature 100℃, catalyst 3.5 mL, activation time 50 min, solvent 37 mL, yield 50.12 %. 3. The structure and morphology of rosin starch esters (RSE) were studied with modern instruments. It can be seen from the FT-IR spectrum that the weaking of the intensity of the intensity at the peak of 3382 cm-1, which due to the replacement of hysroxy. The intensity of the peak decreased with the increase of DS. There were a new carbonyl absorption peak aprrear in 1715 cm-1. The intensity of the peak increased with the increase of DS. The 13CNMR showed that starch and rosin was reactioned. The SEM photos showed that there were some dents and splits on rosin starch esters (RSE) surface. Some starch granules were no longer maintain the round shape, and there were layered structures. The crystalline structure of starch were destroyed. The X-ray spectra showed that the crystalline structure of starch were changed.4. After the starch was modified by rosin. The solubility of rosin starch esters (RSE) were bigged than starch in the organic solvents, and it increase with the increase of DS. The transparency of rosin starch esters (RSE) were smalled than starch, and it decreases with the increase of DS. The retrogradation of rosin starch esters (RSE) were smalled than starch, and it decreases with the increase of DS. The relative viscosity of rosin starch esters (RSE) were smalled than starch, and it decreases with the increase of DS and the decreases of concentration as well as the increase of temperature. The swelling ratio of rosin starch esters (RSE) were smalled than starch, and it decreases with the increase of DS. The hydrophobicity of starch was increased because the starch molecular chain was accessed by rosin acid. The products have"parents"nature with hydrophilic and lipophilic.5. The starch and rosin starch esters (RSE) were used as carriers of Feinuoluofen calcium (FC). They controlled release in artificial gastric juice. Mechanism and dynamics were studied respectively. The results showed that the controlled release of rosin starch esters (RSE) better than starch. The controlled release of rosin starch esters (RSE) was increased with the increase of DS. The release mechanism showed that the drug release meet fick diffusion and dissolution release mechanism. The drug release kinetics showed that the release patterns of Feinuoluofen calcium (FC) from the carriers of starch and rosin starch esters (RSE) fit first-order kinetics.