本文選題：甘油二酯 + 單甘酯�。� 參考：《華南理工大學》2012年碩士論文

【摘要】：本論文研究了富含α-亞麻酸的偏甘油酯的檢測、制備、分離純化及其理化性質(zhì)，為富含多不飽和脂肪酸的甘油二酯及單甘酯的開發(fā)與應用提供依據(jù)。通過HPLC-RID方法檢測甘油酯混合樣品中的甘油三酯、甘油二酯及單甘酯的質(zhì)量濃度并計算百分含量；通過單因素和響應面優(yōu)化實驗設計獲得了采用酶制劑Lipozyme435催化亞麻籽油甘油解制備甘油二酯和單甘酯的最優(yōu)工藝條件；對最優(yōu)反應條件下獲得的甘油二酯和單甘酯反應產(chǎn)物采用分子蒸餾進行了分離純化，獲得了富含α-亞麻酸的高純度甘油二酯與單甘酯產(chǎn)品，并對產(chǎn)品進行了理化指標檢測與儲存穩(wěn)定性研究。 1.研究了甘油酯混合樣品中各酯類組分的HPLC-RID檢測及百分含量計算方法，并對方法的準確度和精密度進行了考察。獲得了甘油三酯，α-亞麻酸甘油二酯和α-亞麻酸單甘酯的標準曲線線性回歸方程，依次分別為y1=1.3423x1、y2=1.5722x2和y3=1.4055x3、相關系數(shù)R1、R2與R3依次分別為0.999、0.998和0.999。精密度與回收率研究結果表明：在適宜的濃度范圍內(nèi)，采用HPLC-RID檢測混合甘油酯樣品中甘油三酯、甘油二酯和單甘酯的質(zhì)量濃度，依照質(zhì)量濃度計算各酯類成分的百分含量的方法精密度與準確度良好。在計算混合甘油酯產(chǎn)品中的酯類成分百分含量時，采用質(zhì)量濃度計算百分含量與直接采用峰面積計算百分含量相比，甘油三酯與單甘酯百分含量分別高0.81%和1.73%，甘油二酯百分含量低2.54%，兩種計算方法獲得的數(shù)據(jù)較為接近。 2.研究了無溶劑體系下采用酶制劑Lipozyme435催化亞麻籽油甘油解制備甘油二酯的工藝。在采用單因素實驗設計考察了底物摩爾比、反應時間、加酶量和反應溫度4個因素對反應產(chǎn)物中甘油二酯含量影響的基礎上，運用響應面實驗設計優(yōu)化得到了甘油二酯制備的最佳工藝條件，即底物摩爾比亞麻籽油：甘油（mol/mol）5：3，加酶量880PLU/g亞麻籽油，反應溫度58.3℃，反應時間9.1h。在此條件下反應所得產(chǎn)物中的甘油二酯含量為50.21%，理論純度可達60.12%，亞麻酸含量為46.22%。 3.研究了叔丁醇溶劑體系下采用酶制劑Lipozyme435催化亞麻籽油甘油解制備單甘酯的工藝。在采用單因素實驗設計考察了底物摩爾比、反應時間、加酶量、油醇比和反應溫度5個因素對反應產(chǎn)物中單甘酯含量影響的基礎上，運用響應面實驗設計優(yōu)化了單甘酯制備的最佳工藝條件，即底物摩爾比亞麻籽油：甘油（mol/mol）為1：3，加酶量為601PLU/g亞麻籽油，反應溫度為56.1℃，油醇比為亞麻籽油占叔丁醇（m/v）的39.7%，反應時間10.5h。在此條件下反應所得產(chǎn)物中單甘酯含量為71.1%，α-亞麻酸的含量達51.36%。 4.研究確定了甘油二酯與單甘酯反應產(chǎn)物采用分子蒸餾分離純化的溫度條件，其中一級分子蒸餾溫度應在120℃，二級分子蒸餾溫度應在220℃，在此條件下對產(chǎn)物進行純化后獲得了純度分別為56.5%的甘油二酯產(chǎn)品和82.3%的單甘酯產(chǎn)品。所得甘油二酯產(chǎn)品在25℃下澄清、透明；水分及揮發(fā)物含量為0.13%；游離甘油含量為0.17%；酸價和皂化值分別為2.10mg KOH/g和182.60mg KOH/g；過氧化值為2.76mmol KOH/g；色澤為Red值4.0Yellow值8.3（25.4mm）。所得單甘酯產(chǎn)品在25℃下呈乳白色膏狀；水分及揮發(fā)物含量為0.10%；游離甘油含量為2.08%；酸價和皂化值分別為3.20mg KOH/g和168.21mg KOH/g；過氧化值為0.50mmol KOH/g；色澤為Red值0.1Yellow值10.0（25.4mm），甘油二酯與單甘酯產(chǎn)品分別符合亞麻籽油標準GBT8235-2008和食品添加劑單、雙硬脂酸甘油酯標準GB1986-2007。產(chǎn)品的氧化穩(wěn)定性研究結果表明：甘油二酯產(chǎn)品儲藏穩(wěn)定性略優(yōu)于亞麻籽油，低于大豆油，單甘酯產(chǎn)品的儲存穩(wěn)定性較差，，甘油二酯和單甘酯產(chǎn)品在添加抗氧化劑后儲藏穩(wěn)定性明顯增強。
[Abstract]:In this paper, the determination, preparation, purification and physicochemical properties of the partial glycerol rich in alpha linolenic acid were studied, and the basis for the development and application of diesters and monoglycerides rich in polyunsaturated fatty acids was provided. The mass concentration of glycerol three ester, diester and monoglyceride in the mixed glyceride samples was detected by HPLC-RID method. The optimum technological conditions for the preparation of glycerol diester and monoglyceride with Lipozyme435 catalyzed glycerol in linseed oil were obtained by single factor and response surface optimization. Molecular distillation was used to obtain the product of diester and monoglyceride obtained under the optimal reaction conditions. High purity diacylglycerol and monoglyceride products, which are rich in alpha linolenic acid, have been studied, and physicochemical indexes and storage stability of the products have been studied.
1. the HPLC-RID detection and percentage calculation method of each component of glyceride mixed samples were studied, and the accuracy and accuracy of the method were investigated. The standard curve regression equation of triglyceride, alpha linolenic acid diester and alpha linolenic monoglyceride was obtained, which were respectively y1=1.3423x1, y2=1.5722x2 and y3=1.40, respectively. 55X3, the correlation coefficient R1, R2 and R3 are respectively the results of 0.999,0.998 and 0.999. precision and recovery respectively. In the suitable concentration range, HPLC-RID is used to detect the quality concentration of triglyceride, diester and monoglyceride in the samples of mixed glyceride, and the method of calculating the percentage of each component according to the quality concentration is precise. When calculating the percentage content of the ester components in the mixed glyceride, the content of the content calculated by the mass concentration is 0.81% and 1.73% higher in the content of the triglyceride and the monoglyceride, and the content of the diester of the triglyceride is 2.54%, and the data obtained by the two methods are compared. To be close.
2. the preparation of glycerol diester from linseed oil catalyzed by Lipozyme435 in solvent free system was studied. On the basis of 4 factors, such as substrate molar ratio, reaction time, enzyme amount and reaction temperature, the response surface experiment was designed on the basis of the response surface experiment. The optimum process conditions for the preparation of diacylglycerol were obtained, namely the substrate mole ratio flax seed oil: glycerol (mol/mol) 5:3, and the amount of 880PLU/g linseed oil added to the enzyme, the reaction temperature was 58.3 C, the reaction time was 9.1h., the content of the diester in the product was 50.21%, the physical purity was 60.12%, the linolenic acid content was 46.22%.
3. the process of preparing monoglyceride in linseed oil catalyzed by enzyme preparation Lipozyme435 under the solvent system of tert butyl alcohol was studied. On the basis of the effect of 5 factors on the content of monoglyceride in the product, the effect of the ratio of substrate molar ratio, reaction time, enzyme amount, oil alcohol ratio and reaction temperature on the content of monoglyceride in the reaction products, the response surface experiment was used. The optimum process conditions for the preparation of monoglyceride, namely, the substrate mole ratio flax seed oil: glycerol (mol/mol) was 1:3, and the amount of enzyme was 601PLU/g flax seed oil, the reaction temperature was 56.1, and the oil and alcohol ratio was 39.7% of the linseed oil (m/v), and the reaction time 10.5h. was 71.1%, alpha subtermate. The content of hemp acid reached 51.36%.
4. the temperature conditions for the separation and purification of diacylglycerol and monoglyceride reaction products by molecular distillation are determined, in which the first order molecular distillation temperature should be 120, and the two stage molecular distillation temperature should be at 220. Under this condition, the product is purified and the purity of the product is 56.5%, and the product of 82.3% monoglyceride, respectively, is obtained. The diacylglycerol products were clarified and transparent at 25 C; the content of water and volatiles was 0.13%, the content of free glycerol was 0.17%; the acid value and saponification value were 2.10mg KOH/g and 182.60mg KOH/g, the peroxide value was 2.76mmol KOH/g; the color was Red value 4.0Yellow value 8.3 (25.4mm). The monoglyceride products were milk white paste at 25 degrees C; water The content and volatiles content are 0.10%, free glycerol content is 2.08%, acid value and saponification value are 3.20mg KOH/g and 168.21mg KOH/g, peroxidation value is 0.50mmol KOH/g, Red value 0.1Yellow value 10 (25.4mm), and glycerol diester and monoglyceride products are in line with linseed oil standard GBT8235-2008 and food additive list, distearic acid, respectively. The results of the oxidation stability of the glyceryl ester standard GB1986-2007. product show that the storage stability of the diester product is slightly better than the linseed oil. The storage stability of the product is lower than that of the soybean oil. The stability of the diester and monoglyceride products is obviously enhanced after the addition of antioxidants.
【學位授予單位】：華南理工大學
【學位級別】：碩士
【學位授予年份】：2012
【分類號】：R151

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