【摘要】：聚甘油脂肪酸酯作為一種新型乳化劑,因具有天然、安全性高、HLB值范圍寬,乳化穩(wěn)定性好等諸多優(yōu)點(diǎn),目前在食品、日化、醫(yī)藥等領(lǐng)域應(yīng)用廣泛。本論文主要以不同鏈長(zhǎng)的脂肪酸為原料,采用酶法綠色合成聚甘油脂肪酸酯產(chǎn)品,并研究其理化性質(zhì),以單甘酯作為對(duì)比,探討合成的聚甘油脂肪酸酯產(chǎn)品在乳液及藥物輸送體系中的應(yīng)用。本論文主要研究結(jié)果如下:第一,本論文研究并優(yōu)化了聚甘油的合成方法。采用氫氧化鈉作為催化劑,反應(yīng)體系置于高溫加熱條件下,甘油脫去水分子合成聚甘油,并通過(guò)單因素試驗(yàn)法和正交試驗(yàn)法優(yōu)化聚甘油的合成工藝,在最佳反應(yīng)條件下得到聚合度為3.61、無(wú)刺激性氣味的淺褐色聚甘油產(chǎn)品。經(jīng)過(guò)分子蒸餾設(shè)備提純后,最終可以得到純度為86.33%的聚甘油,其中二聚甘油含量為68.30%,三聚甘油含量為13.13%,四聚甘油含量為3.18%。第二,本文采用固定化435脂肪酶在無(wú)溶劑體系下分別催化米糠油、樟樹(shù)籽油、乙酸合成不同鏈長(zhǎng)脂肪酸聚甘油酯。利用單因素試驗(yàn)和響應(yīng)面試驗(yàn)優(yōu)化反應(yīng)條件,在最佳反應(yīng)條件下,得到三種原料合成反應(yīng)的平均酯化率分別為69.37%,67.34%和71.68%,并通過(guò)FTIR、HPLC/ESI/MS等方法鑒定了聚甘油酯產(chǎn)品的組成。第三,本文采用Griffin提出的方法,計(jì)算出自制聚甘油酯的HLB值皆大于7,為親水性的乳化劑類(lèi)型。以目前使用最為廣泛的乳化劑單甘酯作為對(duì)照,研究自制聚甘油酯產(chǎn)品的乳化性、起泡性等。研究結(jié)果為:在長(zhǎng)碳鏈脂肪酸聚甘油酯乳液制備的乳液中,使其靜置穩(wěn)定性、離心穩(wěn)定性以及耐熱穩(wěn)定性表現(xiàn)最優(yōu)的情況下,乳化劑的最小添加量分別為0.1%、0.1%、0.3%;在中碳鏈脂肪酸聚甘油酯制備的乳液中,使其靜置穩(wěn)定性、離心穩(wěn)定性、耐熱穩(wěn)定性表現(xiàn)最優(yōu)的情況下,乳化劑的最小添加量分別為0.3%、0.3%、0.3%。而短碳鏈脂肪酸聚甘油酯及單甘酯的乳化效果較差,乳液極不穩(wěn)定,容易發(fā)生油滴聚結(jié)、油水分離的現(xiàn)象。在乳化劑添加量為0.3%時(shí),由米糠油合成的聚甘油酯制備的乳液最穩(wěn)定,粒徑只有16.8nm;由樟樹(shù)籽油合成的聚甘油酯制備的乳液起泡性和泡沫穩(wěn)定性表現(xiàn)最佳,分別達(dá)到76.34%和92.96%。最后,本文選取在體內(nèi)吸收效率低的姜黃素作為包埋對(duì)象,采用前體注入法制備姜黃素乳液包埋體系,利用單因素試驗(yàn),考察原料用量、穩(wěn)定劑用量、姜黃素用量對(duì)乳液包埋體系包埋率的影響。結(jié)果顯示以上三個(gè)因素的最佳添加量分別為20%、0.1g、7%,在此條件下長(zhǎng)、中、短碳鏈脂肪酸聚甘油酯及單甘酯的制備的姜黃素乳液包埋體系包埋率分別達(dá)到51.31%、43.01%、5.12%、58.96%。
[Abstract]:As a new emulsifier, polyglycerol fatty acid ester is widely used in food, daily chemistry, medicine and other fields because of its many advantages, such as natural, high safety, wide range of HLB value, good emulsification stability and so on. In this paper, polyglycerol fatty acid ester was synthesized by enzymatic green synthesis with different chain length fatty acids as raw materials, and its physical and chemical properties were studied, compared with monoglyceride. The application of synthetic polyglycerol fatty acid ester in emulsion and drug delivery system was discussed. The main results of this thesis are as follows: first, the synthesis method of polyglycerol is studied and optimized. Polyglycerol was synthesized by using sodium hydroxide as catalyst and the reaction system was heated at high temperature. The synthesis process of polyglycerol was optimized by single factor test and orthogonal test. A light brown polyglycerol product with polymerization degree 3.61 and no irritant odor was obtained under the optimum reaction conditions. After purification by molecular distillation equipment, the purity of polyglycerol was 86.33%, in which the content of dipolyglycerol was 68.30, the content of tripolyglycerol was 13.13 and the content of tetrapolyglycerol was 3.18. Secondly, the immobilized 435 lipase was used to catalyze rice bran oil, camphor seed oil and acetic acid to synthesize different chain length fatty acid polyglycerides in solvent free system. The reaction conditions were optimized by single factor test and response surface test. Under the optimum reaction conditions, the average esterification rates of the three synthetic reactions were 69.37% 67.34% and 71.68%, respectively, and the average esterification rates were 69.37% and 71.68%, respectively, by FTIR,. The composition of polyglycerol ester was identified by HPLC/ESI/MS and other methods. Thirdly, by using the method proposed by Griffin, the HLB values of self-made polyglycerides are all greater than 7, which is a hydrophilic emulsifier type. The emulsifying and foaming properties of polyglycerol products were studied by using the most widely used emulsifier monoglyceride. The results are as follows: in the emulsion prepared by long chain fatty acid polyglyceride emulsion, when the stability, centrifugal stability and heat stability of the emulsion are optimal, the minimum amount of emulsifier is 0.1% and 0.1%, respectively. 0.3; In the emulsion prepared by medium carbon chain fatty acid polyglyceride, the stability of the emulsion is stable, the stability of centrifugation and heat resistance is the best, and the minimum amount of emulsifier is 0.3% and 0.3%, respectively. The emulsification effect of short carbon chain fatty acid polyglycerides and monoglycerides is poor, the emulsion is very unstable, oil droplet coalescence and oil-water separation are easy to occur. When the amount of emulsifier was 0.3, the emulsion prepared by polyglycerol from rice bran oil was the most stable, and the particle size was only 16.8 nm. The foaming property and foam stability of the emulsion prepared from camphor seed oil were 76.34% and 92.96% respectively. Finally, curcumin with low absorption efficiency was selected as the entrapment object, and the curcumin emulsion embedding system was prepared by precursor injection method. The amount of raw material and stabilizer was investigated by single factor test. The effect of curcumin dosage on the entrapment rate of emulsion embedding system. The results showed that the optimum addition amount of the above three factors was 200.1g / 7.The entrapment rate of curcumin emulsion was 51.31, respectively, for the preparation of long, medium and short carbon chain fatty acid polyglycerides and monoglycerides under this condition, and the results showed that the entrapment efficiency of curcumin emulsion was 51.31%, respectively. 43.01 and 5.12, about 58.96.
【學(xué)位授予單位】：南昌大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類(lèi)號(hào)】：O647.2

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本文編號(hào)：2326104