花生四烯酸甘油酯双重微胶囊化及性质表征
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摘要
花生四烯酸是一种n-6系列多不饱和脂肪酸,对人体具有重要的生理功能作用,其主要以花生四烯酸甘油酯形式存在,花生四烯酸甘油酯在体外易受环境因素影响,在体内易受胃液影响,产生氧化酸败现象,变质的花生四烯酸甘油酯对人体有害并且气味难闻,影响摄入体验；另一方面,花生四烯酸甘油酯常温下为粘稠状液态,运输、储存不便。而且油溶性花生四烯酸甘油酯难与水溶性物质混合,限制了花生四烯酸在食品工业上的应用,论文的主要目的是寻找-种工艺技术来解决花生四烯酸面临的这些问题。
论文以糊精以及实验室自制的变性淀粉MSF-231为壁材,对花生四烯酸甘油酯进行喷雾干燥处理,得到花生四烯酸甘油酯一次微胶囊产品；应用一次微胶囊产品,以羟丙基甲基纤维素邻苯二甲酸酯(?)(HPMCP)为肠溶性壁材进行二次微胶囊化,得到耐酸性的肠溶微胶囊产品。研究微胶囊化的工艺配方,检验对比所得两种微胶囊产品的常规性质,考察产品的耐酸碱能力,得到以下主要结论：
1、一次微胶囊制备的最佳工艺配方为：30%花生四烯酸甘油酯,15%自制变形淀粉MSF-231、54%糊精,自制复合乳化剂P0281用量为0.7%、P0299-2用量为0.3%,乳化温度75℃,30MPa高压均质2次,该工艺得到的乳状液稳定性高达99.89%；最佳喷雾干燥工艺为：进风温度180℃、出风温度95℃,固液比1：1,对乳状液进行喷雾干燥,得到的花生四烯酸甘油酯一次微胶囊产品性质稳定,包埋效果好。二次微胶囊制备的最佳工艺配方为：80%花生四烯酸甘油酯一次微胶囊,20%HPMCP,溶剂组成为乙醇/二氯甲烷,比例为3：1,壁材溶液浓度为7%；喷雾干燥条件为：进风温度135℃,出风温度75℃；所得产品油脂释放率低,干燥完全。
2、两种微胶囊产品的结构均接近于球形,一次、二次微胶囊产品的挥发物含量分别为2.77%和2.18%,含油率分别为29.86%和23.83%,均接近于原始含油率,包埋率分别为96.21%和97.36%,初始表面含油率分别为1.13%和0.63%,120天内增量分别为0.41%和0.32%,说明两种微胶囊产品干燥完全,微胶囊化工艺较完善,芯壁材混合均匀,包埋率高,表面含油率低、表面油增加缓慢。并且二次微胶囊化没有破坏一次微胶囊产品原有性质。
3、一次微胶囊产品和二次微胶囊产品的初始PV值分别为2.57meq/kg和2.44meq/kg,120天内增量分别为2.00meq/kg和1.71meq/kg,两种微胶囊产品初始酸价分别为0.61 mg KOH/g和0.57 mg KOH/g,在250天内酸价变化均比较缓慢,增量分别为2.75 mg KOH/g和2.36 mg KOH/g,在250-350天共100天贮存期内,一次微胶囊产品酸价上升速度加快,增量为3.57 mg KOH/g,而二次微胶囊产品酸价变化依然缓慢,增量为0.18 mg KOH/g, PV值低,变化缓慢,说明两种壁材都能够有效隔离氧气,达到保护芯材的目的；酸价变化情况说明二次微胶囊化能增加花生四烯酸甘油酯微胶囊的贮藏时间。
4、一次微胶囊产品经人工胃液30分钟处理后,油脂释放率为18.63%,经4小时处理后,油脂释放率为92.38%,二次微胶囊产品经人工胃液4小时处理,油脂释放率仅为5.81%,说明二次包埋有效地控制了花生四烯酸甘油酯在胃部的释放,减少了花生四烯酸甘油酯的体内变质。
5、二次微胶囊产品经人工肠液10分钟处理后,油脂释放率为85.95%,在60分钟时,释放率为98.67%,说明二次微胶囊化壁材用量合理,实验选用的肠溶包衣壁材HPMCP在肠道内能快速崩解,对芯材花生四烯酸甘油酯的肠道吸收影响很小。
Arachidonic acid is one of n-6 series polyunsaturated fatty acids, its physiological functions are important for human body and the main existence form is glyceryl arachidonate, oxidation and acidification of glyceryl arachidonate is incidental by environmental factors out of body or gastric juice in body, the intake experience is bad that metamorphic products are Harmful and the odor is unpleasant. On the other hand, glyceryl arachidonate is viscous liquid at room temperature, transport and storage is difficult. Mixing of oil-soluble glyceryl arachidonate and water-soluble substances is difficult; the application of arachidonic acid in the food industry is limited. The main objective of this thesis is finding a technology that can resolve these problems.
Take dextrin and MSF-231 (modified starch that lab-made) as wall material, and glyceryl arachidonate as core material, one-walled microcapsules was prepared by spray drying; Hydroxypropyl methyleellulose phathalate and parts of one-walled microcapsules were microcapsulated second time and formed into enteric-soluble microcapsules by the same method. Based on research of process and formulation of microencapsulation, test and compare the general properties of two types of microencapsulated products, examine their ability on acid tolerance, the main conclusions are the following:
1. The best process and formulation of preparation of one-walled glyceryl arachidonate microcapsules by spray drying:30% glyceryl arachidonate,15% MSF-231,54% dextrin,0.7% P0281 (lab-made emulsifier),0.3% P0299-2(lab-made emulsifier), mix and emulsify in 75℃, then homogenize twice times under 30 MPa, the stability of the emulsion made by this process has been as high as 99.89%; The best process of spray drying:180℃inlet air,95℃discharge air, half solid and half liquid, the products made in these conditions have a higher embedding rate and stable performance. The best process and formulation of preparation of double-walled glyceryl arachidonate microcapsules by spray drying:80% one-walled microcapsules, 20% HPMCP, solvent consist of ethanol and dichloromethane, and the ratio is 3:1, the concentration of wall material solution is 7%; the best process of spray drying:135℃inlet air,75℃discharge air, the release rate of oil of double-walled glyceryl arachidonate microcapsules is low, the product is dry completely.
2. The structures of two types of microencapsulated products were close to spherical, the moisture content of one-walled microcapsules and double-walled microcapsules were 2.77% and 2.18%, oil rates were 23.83% and 29.86% and close to the original oil content, microencapsulation efficiencies were 96.21% and 97.36%, the initial surface oil content were 1.13% and 0.63%, the increments of surface oil content were 0.41% and 0.32% in 120 days, indicating that two types of products were dried completely, the process of microencapsulation was complete, the mixture of core material and wall material was well-proportioned, the products had a higher embedding rate and a lower percentage of surface oil and surface oil increased slowly, Important was that the original natures of one-walled microcapsules had not been destroyed by second time microcapsulated.
3. The initial peroxide values of one-walled microcapsules and double-walled microcapsules were 2.57 meq/kg and 2.44 meq/kg, the increments of peroxide values were 0.41% and 0.32% in 120 days, and acid numbers were 0.61 mg KOH/g and 0.57 mg KOH/g and increased slowly, the increments were 2.75 mg KOH/g and 2.36 mg KOH/g in 250 days, but in the next 100 days storage period, acid number of one-walled microcapsules increased faster and the increment was 3.57 mg KOH/g, acid number of double-walled microcapsules increased still slowly and the increment was 0.18 mg KOH/g, low peroxide value and increased slowly indicated that two kinds of wall materials can isolate the oxygen effectively and to protect the core material; Changes of acid numbers indicated that second time microcapsulated can increase storage time of microcapsules of glyceryl arachidonate.
4. After dealing with artificial gastric juice for 30 minutes, the release rate of oil of one-walled microcapsules was 18.63%, after 4 hours treatment, the release rate of oil was 92.38%, but the release rate of oil of double-walled microcapsules was 5.81% after 4 hours treatment, the different of the release rate of oil between two types microcapsulated products indicated that the second time microcapsulated can control the release of glyceryl arachidonate in the stomach effectively and reduce the deterioration in body.
5. After dealing with artificial intestinal juice for 10 minutes, the release rate of oil of double-walled microcapsules was 85.95%, in 60 minutes, the release rate was 98.67%,it indicated that the wall material content of the second time microencapsulation was reasonable and HPMCP, which is a type of enteric coating wall material, can disintegrate quickly in the intestine, the second time microencapsulation has little effect on the absorption of glyceryl arachidonate in the intestine.
论文以糊精以及实验室自制的变性淀粉MSF-231为壁材,对花生四烯酸甘油酯进行喷雾干燥处理,得到花生四烯酸甘油酯一次微胶囊产品；应用一次微胶囊产品,以羟丙基甲基纤维素邻苯二甲酸酯(?)(HPMCP)为肠溶性壁材进行二次微胶囊化,得到耐酸性的肠溶微胶囊产品。研究微胶囊化的工艺配方,检验对比所得两种微胶囊产品的常规性质,考察产品的耐酸碱能力,得到以下主要结论：
1、一次微胶囊制备的最佳工艺配方为：30%花生四烯酸甘油酯,15%自制变形淀粉MSF-231、54%糊精,自制复合乳化剂P0281用量为0.7%、P0299-2用量为0.3%,乳化温度75℃,30MPa高压均质2次,该工艺得到的乳状液稳定性高达99.89%；最佳喷雾干燥工艺为：进风温度180℃、出风温度95℃,固液比1：1,对乳状液进行喷雾干燥,得到的花生四烯酸甘油酯一次微胶囊产品性质稳定,包埋效果好。二次微胶囊制备的最佳工艺配方为：80%花生四烯酸甘油酯一次微胶囊,20%HPMCP,溶剂组成为乙醇/二氯甲烷,比例为3：1,壁材溶液浓度为7%；喷雾干燥条件为：进风温度135℃,出风温度75℃；所得产品油脂释放率低,干燥完全。
2、两种微胶囊产品的结构均接近于球形,一次、二次微胶囊产品的挥发物含量分别为2.77%和2.18%,含油率分别为29.86%和23.83%,均接近于原始含油率,包埋率分别为96.21%和97.36%,初始表面含油率分别为1.13%和0.63%,120天内增量分别为0.41%和0.32%,说明两种微胶囊产品干燥完全,微胶囊化工艺较完善,芯壁材混合均匀,包埋率高,表面含油率低、表面油增加缓慢。并且二次微胶囊化没有破坏一次微胶囊产品原有性质。
3、一次微胶囊产品和二次微胶囊产品的初始PV值分别为2.57meq/kg和2.44meq/kg,120天内增量分别为2.00meq/kg和1.71meq/kg,两种微胶囊产品初始酸价分别为0.61 mg KOH/g和0.57 mg KOH/g,在250天内酸价变化均比较缓慢,增量分别为2.75 mg KOH/g和2.36 mg KOH/g,在250-350天共100天贮存期内,一次微胶囊产品酸价上升速度加快,增量为3.57 mg KOH/g,而二次微胶囊产品酸价变化依然缓慢,增量为0.18 mg KOH/g, PV值低,变化缓慢,说明两种壁材都能够有效隔离氧气,达到保护芯材的目的；酸价变化情况说明二次微胶囊化能增加花生四烯酸甘油酯微胶囊的贮藏时间。
4、一次微胶囊产品经人工胃液30分钟处理后,油脂释放率为18.63%,经4小时处理后,油脂释放率为92.38%,二次微胶囊产品经人工胃液4小时处理,油脂释放率仅为5.81%,说明二次包埋有效地控制了花生四烯酸甘油酯在胃部的释放,减少了花生四烯酸甘油酯的体内变质。
5、二次微胶囊产品经人工肠液10分钟处理后,油脂释放率为85.95%,在60分钟时,释放率为98.67%,说明二次微胶囊化壁材用量合理,实验选用的肠溶包衣壁材HPMCP在肠道内能快速崩解,对芯材花生四烯酸甘油酯的肠道吸收影响很小。
Arachidonic acid is one of n-6 series polyunsaturated fatty acids, its physiological functions are important for human body and the main existence form is glyceryl arachidonate, oxidation and acidification of glyceryl arachidonate is incidental by environmental factors out of body or gastric juice in body, the intake experience is bad that metamorphic products are Harmful and the odor is unpleasant. On the other hand, glyceryl arachidonate is viscous liquid at room temperature, transport and storage is difficult. Mixing of oil-soluble glyceryl arachidonate and water-soluble substances is difficult; the application of arachidonic acid in the food industry is limited. The main objective of this thesis is finding a technology that can resolve these problems.
Take dextrin and MSF-231 (modified starch that lab-made) as wall material, and glyceryl arachidonate as core material, one-walled microcapsules was prepared by spray drying; Hydroxypropyl methyleellulose phathalate and parts of one-walled microcapsules were microcapsulated second time and formed into enteric-soluble microcapsules by the same method. Based on research of process and formulation of microencapsulation, test and compare the general properties of two types of microencapsulated products, examine their ability on acid tolerance, the main conclusions are the following:
1. The best process and formulation of preparation of one-walled glyceryl arachidonate microcapsules by spray drying:30% glyceryl arachidonate,15% MSF-231,54% dextrin,0.7% P0281 (lab-made emulsifier),0.3% P0299-2(lab-made emulsifier), mix and emulsify in 75℃, then homogenize twice times under 30 MPa, the stability of the emulsion made by this process has been as high as 99.89%; The best process of spray drying:180℃inlet air,95℃discharge air, half solid and half liquid, the products made in these conditions have a higher embedding rate and stable performance. The best process and formulation of preparation of double-walled glyceryl arachidonate microcapsules by spray drying:80% one-walled microcapsules, 20% HPMCP, solvent consist of ethanol and dichloromethane, and the ratio is 3:1, the concentration of wall material solution is 7%; the best process of spray drying:135℃inlet air,75℃discharge air, the release rate of oil of double-walled glyceryl arachidonate microcapsules is low, the product is dry completely.
2. The structures of two types of microencapsulated products were close to spherical, the moisture content of one-walled microcapsules and double-walled microcapsules were 2.77% and 2.18%, oil rates were 23.83% and 29.86% and close to the original oil content, microencapsulation efficiencies were 96.21% and 97.36%, the initial surface oil content were 1.13% and 0.63%, the increments of surface oil content were 0.41% and 0.32% in 120 days, indicating that two types of products were dried completely, the process of microencapsulation was complete, the mixture of core material and wall material was well-proportioned, the products had a higher embedding rate and a lower percentage of surface oil and surface oil increased slowly, Important was that the original natures of one-walled microcapsules had not been destroyed by second time microcapsulated.
3. The initial peroxide values of one-walled microcapsules and double-walled microcapsules were 2.57 meq/kg and 2.44 meq/kg, the increments of peroxide values were 0.41% and 0.32% in 120 days, and acid numbers were 0.61 mg KOH/g and 0.57 mg KOH/g and increased slowly, the increments were 2.75 mg KOH/g and 2.36 mg KOH/g in 250 days, but in the next 100 days storage period, acid number of one-walled microcapsules increased faster and the increment was 3.57 mg KOH/g, acid number of double-walled microcapsules increased still slowly and the increment was 0.18 mg KOH/g, low peroxide value and increased slowly indicated that two kinds of wall materials can isolate the oxygen effectively and to protect the core material; Changes of acid numbers indicated that second time microcapsulated can increase storage time of microcapsules of glyceryl arachidonate.
4. After dealing with artificial gastric juice for 30 minutes, the release rate of oil of one-walled microcapsules was 18.63%, after 4 hours treatment, the release rate of oil was 92.38%, but the release rate of oil of double-walled microcapsules was 5.81% after 4 hours treatment, the different of the release rate of oil between two types microcapsulated products indicated that the second time microcapsulated can control the release of glyceryl arachidonate in the stomach effectively and reduce the deterioration in body.
5. After dealing with artificial intestinal juice for 10 minutes, the release rate of oil of double-walled microcapsules was 85.95%, in 60 minutes, the release rate was 98.67%,it indicated that the wall material content of the second time microencapsulation was reasonable and HPMCP, which is a type of enteric coating wall material, can disintegrate quickly in the intestine, the second time microencapsulation has little effect on the absorption of glyceryl arachidonate in the intestine.
引文
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