复合凝聚反应制备茉莉香精微/纳米胶囊及其机理研究
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摘要
复合凝聚反应（Complex coacervation）是发生于两种或两种以上大分子之间的基于静电相互作用的自聚集现象。利用不同反应程度的产物，可获得一系列具有不同尺度、特殊表面性能或优异乳化性质的复合凝聚物。它们在食品、化工、医药及纺织领域都有潜在的应用价值。然而，由于该反应原料间差异性较大，可控因素多且可调范围窄，致使其工业化进程缓慢。
本论文所研究的对象为复合凝聚反应应用领域的一个极重要分支——胶囊化包埋。通过对不同尺度的复合凝聚物形成机理的研究，发现适用于纳米胶囊及微胶囊制备的不同反应阶段，以茉莉精油作为芯材，较为简便地获得相应胶囊化产品的制备工艺，并对其胶囊性质进行了一定的探索。具体研究内容及结果如下：
选取明胶-阿拉伯胶体系作为反应的原料组合，在不同的混合比例（2:1，1:1，1:2，w/w）下，测量逐滴添加醋酸后600nm的吸光值变化，得到浊度滴定曲线。通过对曲线不同阶段的分析，发现该体系可通过pH条件控制，形成可溶性复合物及不可溶性复合物阶段，即它们具备了形成纳米胶囊与微胶囊的可能性。
研究1:1混合比例下，相同pH值的明胶-阿拉伯胶体系的复聚物及以茉莉精油为芯材的微胶囊之间的关联性，具体为显微图像、产率及内部特性（抗机械外力-耐热性）。结果表明，二者之间具有极高的一致性，可借此简化微胶囊的工艺优化过程，概括如下：通过电位分析确定壁材之间可能的混合比例；浊度滴定曲线被用作选择最适混合比例及相应的pH条件；所得出的最适条件即可应用于微胶囊的制备。据此工艺优化过程，研究发现了一种新型多糖类壁材——羧甲基纤维素钠，显微图像结果表明其所形成的微胶囊结构与明胶-阿拉伯胶体系相似。
通过动态温度流变分析模拟两种产自不同树种的阿拉伯胶（A. Senegal：AA；A. Seyal：BA）与明胶发生复合凝聚反应包裹茉莉精油后的冷却过程。结果发现对于流变曲线中弹性模量大于粘性模量的阶段，明胶-BA体系较明胶-AA体系具有更低的温度，即意味着要达到同样的弹性模量值时，明胶-BA体系需使温度降至更低。由于弹性模量体现了体系的类固体性质，因此可通过二者流变曲线的差异来指导微胶囊制备过程中的冷却步骤，达到使价格较低的BA型阿拉伯胶与价格较高的AA型接近的显微形态效果。具体的冷却条件为：AA，20-10°C；BA，5-0°C。
选取三组混合比例（2:1，1:1，1:2）下的明胶-阿拉伯胶体系，利用多种手段研究其分子水平的复聚物形成机理。首先，通过显微图像及粒径分布分析发现，随pH的降低，1:1及1:2混合比例下的复聚物粒径逐渐增大，而2:1的复聚物粒径则逐渐减小。其次，原料转化率分析结果显示，复聚物的粒径转变趋势与阿拉伯胶的转化率变化相一致，即阿拉伯胶参与反应的数量越多，则复聚物粒径越大。最后，通过圆二光谱技术揭示了2:1混合比例下明胶、阿拉伯胶大分子的构象转变过程。在复聚物的形成中，明胶分子由无规卷曲结构转向了有序的PPII螺旋；阿拉伯胶分子则由部分有序的PPII螺旋转向了结构紧凑的PPI螺旋。该构象转变规律也体现于1:1与1:2的混合比例中。据此，推测复聚物粒径的改变是受分子水平的结构转变与参与反应的阿拉伯胶数量二者共同的影响。
利用等温滴定量热技术对复合凝聚反应中的结合等温线进行分析，进一步佐证了明胶-阿拉伯胶体系中存在可溶性复合物及不可溶性复合物的两阶段产物。通过不同温度下的曲线发现氢键作用对反应影响较大，低温促使更多氢键的生成。考虑到可溶性复合物的形成中静电相互作用极其有限，因此在以下纳米胶囊的制备中只需要常温条件（25~30°C）反应即可。
原位酸化剂——葡萄糖酸-δ-内酯被用于自发地缓慢改变体系的pH值，从而获得低水平下的浊度滴定曲线，探寻可溶性复合物的形成pH范围。结果表明，随明胶-阿拉伯胶混合比例的降低，相应的pH范围逐渐扩大。同时，通过NaCl及脲的添加发现大分子间的相互作用不仅包含起主导作用的静电相互作用，也与疏水相互作用有关。在确定可溶性复合物形成pH范围后，利用粒径分布分析获得适于纳米胶囊制备的最适pH条件及壁材比例（1:1，pH4.80）。其后，以平均粒径、多分散指数、电位及载量为指标，采用单因素优化，获得茉莉香精纳米胶囊的制备条件：明胶、阿拉伯胶比例1:1，总浓度0.5%；茉莉精油浓度0.5%；乳化剂（Span80: Tween80=1:1）浓度0.5%；固化剂转谷氨酰胺酶添加量0.25%。该条件下所制得的茉莉精油纳米胶囊平均粒径（r）为69.56nm，PDI值为0.135，带电量为-14.80mV。透射电镜结果与粒径测量结果相似，且充分证明了纳米胶囊对茉莉精油的包埋特性。
为获得具耐高温性的茉莉香精纳米胶囊，特对其固化过程进行研究。对不同pH条件（pH4.80，6.0，7.0，8.0）下固化的茉莉香精纳米胶囊进行80°C的水浴加热，结果表明中性或弱碱性条件下的固化能显著提高粒子所带电荷的绝对值，增加体系的稳定性。在pH7条件下固化的纳米胶囊，经过7h的加热后，粒径为101.89nm，多分散指数为0.106，电位为-9.45mV，它的稳定性仍优于未固化纳米胶囊的初始值（电位-8.67mV）。基于纳米胶囊在形成与热作用下的粒径转变现象，发现大分子吸附、固化交联、热展开等是导致其粒径变化的主要因素。
pH7固化条件下的茉莉香精纳米胶囊于加热不同时间下的挥发性物质分析结果发现，五种茉莉香精的特征性风味（芳樟醇，氨茴酸甲酯，顺-茉莉酮，二氢月桂烯醇，乙酸苄酯，乙酸苯乙酯，肉桂酸甲酯和吲哚）随加热时间的延长含量均下降。根据它们的下降趋势分析该纳米胶囊能耐受80°C、5h以内的加热条件。采用热重分析，对不同固化条件的茉莉香精纳米胶囊进行研究，以表征它们抵抗干热的能力。结果表明pH7、8条件下固化的纳米胶囊耐热性显著优于pH6的条件，它们经过200°C下15min的加热，体系的整体失重率仅为约20%。
Complex coacervation reaction is a self-assembled phenomenon that always happened among two orabove two kinds of macromolecules driven by electrostatic interactions. Through the application ofdifferent extents of reaction products, we could obtain series of complex coacervates with variable size,special surface capability or excellent emulsification. Such complex coacervates will confer great potentialsin industries like food, chemical engineering, pharmaceutical and textile. However, due to the largedifference among raw materials and big difficult in controlling the parameters, its process ofindustrialization is always slow.
The current paper was focused on an important application field of complex coacervation-microencapsulation. The formation mechanism of complex coacervates was been investigated to disclosethe variable reaction phases suitable for preparation of nano-capsule and microcapsule. Furthermore, thecorresponding capsule type products were specifically fabricated with jasmine essence as core material;also their capsules’ characteristics were explored. The main contents are as follows:
The gelatin-gum arabic system was chosen as raw materials of the reaction. Firstly, the turbidity titrationcurve at variable mixing ratios (2:1，1:1，1:2，w/w) for gelatin-gum arabic was obtained via drop-wise additionof acetic acid and then tested the absorbance values at600nm. Through analysis of the curve, it was found thatthis system could form soluble complexes and insoluble complexes by pH adjustment. In correspondence, thiscurve had the possibility to form nano-capsule and microcapsule.
The complex coacervates and corresponding microcapsules at the mixing ratio of1:1and the same pHrange were investigated to find their relationship in each other, for the purpose of simplifying microcapsulepreparation optimization processing. Comparisons on morphology, yield and internal characteristic(anti-mechanical force capability-heat-resistance) were performed. Finally, a simplified method was proposed,in which the zeta-potential measurement helps to establish the approximate mixing ratios of wall materials; theturbidity analysis facilitates the finding of suitable pH corresponded to the highest turbidity to make the perfectmicrocapsule. According to this method, a new combination of wall materials named gelatin and sodiumcarboxymethyl cellulose was provided and verified by morphology.
The dynamic-temperature rheological analysis was applied to investigate the cooling process ofcomplex coacervation happened between gelatin and two variety of gum arabic from different types of tree(A. Senegal: AA; A. Seyal: BA). It was found that the systems composed of different gum arabic conferredgreat variance on the property of viscoelasticity. In particular, the transition temperature from viscosity toelasticity was much higher for AA type complexes than BA type complexes. As the elasticity representedthe solid-like capability, such rheological curve could be applied to guide the preparation of microcapsuleby adjusting the cooling conditions. Therefore, the cheaper BA type gum arabic could own a similarmorphology with AA type. The specific cooling conditions are20-10°C for AA and5-0°C for BA。
The coacervates of gelatin and gum arabic with three mixing ratios (2:1,1:1and1:2, w/w) wereprepared in order to elucidate their pH-dependent complexation mechanism. Firstly, the analysis ofmorphology and size distribution showed that with pH decline, the coacervates became larger for themixing ratio of1:1and1:2; whereas, the trend went oppositely as to the mixing ratio of2:1. Through thecomposition analysis of coacervates, such transition pattern was found to be consistent with the conversionrate of gum arabic. Coacervates prepared by the mixing ratio of2:1were chosen to further investigate theformation mechanism at the molecular level. During the complexation process with pH decrease, gelatinmolecules experienced a conformational change from a flexible pattern to an ordered PPII helix. On theother hand, gum arabic went through a transition from partly ordered PPII helix to a more compactstructure, called PPI helix. Such characteristics of conformational transition were also similar for thesystems with mixing ratios of1:1and1:2. Therefore, it was presumed that the change of coacervates size was due to the combined reasons including the conformational transition and the reacted amount of gumarabic.
The isothermal titration calorimetry was used to analyze the binding isotherm for complexcoacervation. The curve verified again the existence of two phase products, including soluble complexesand insoluble complexes. Also, the curves at different temperatures showed that hydrogen bond played animportant role for structure formation. Specifically, the low temperature facilitated more hydrogen bondproduced. Considering the limit electrostatic interactions existed for soluble complexes, the correspondingnano-capsules could be strengthened by hydrogen bond through reacting just at room temperature, withoutthe need of heating.
The colloidal behavior of soluble complexes was investigated using turbidity titration (600nm) withthe help of an in situ acidification-glucono-δ-lactone. The results showed that, with the decrease of mixingratio, the corresponding pH range for soluble complexes became a little larger. Furthermore, the addition ofNaCl and urea indicated the interactions between macromolecules were not only electrostatic interactions,but also hydrophobic interactions. Through the analysis of particle distribution, pH4.80under the mixingratio of1:1was chosen as the favorable condition for the nano-particles preparation. Subsequently,corresponding nano-capsules with jasmine essential oil entrapped were prepared. Based on the parametersof general size, polydispersity index (PDI), zeta potential and load, the best nano-capsules weresuccessfully prepared (r=69.56nm, PDI=0.135and zeta potial=-14.80mV) The optimized conditions wereselected as follows: total concentration0.5%, jasmine essence concentration0.5%, emulsifier concentration0.5%, emulsifier composition Span80and Tween80(1:1), cross-linker transglutaminase (0.25%). Theresults of transmission electron morphology were consistent with the particle size distribution, furtherverifying the encapsulation capability of nano-capsules.
In order to obtain heat-resistant jasmine essence nano-capsules, the hardening process via cross-linkertransglutaminase was investigated. Their heat-resistance capability against80°C water bath was evaluated bysize, PDI and zeta potential. The results showed that the nanocapsules cross-linked at alkaline conditionsconferred a better stability. Specifically, the nano-capsules processed at pH7for hardening process could endurethe incubation at80°C for7h. The final characteristics are as follows: size=101.89nm, PDI=0.106, zetapotential=-9.45mV. Such particles stability were still better than the original value of un-hardenednano-capsules (zeta potentiall=-8.67mV). Based on the particle size transition rules among nano-capsules’formation and heat effect, it signified the macromolecules’ absorption, cross-linkage and heat-unfolding were themain reasons for size variation.
During the analysis of volatile compounds for jasmine essence nano-capsules hardened at pH7undervariable heating time, five characteristic flavor compounds (linalool, methyl anthranilate, cis-jasmone,dihydromyrcenol, benzyl acetate, acetic acid phenethyl ester, cinnamic acid methyl ester and indole) for jasmineessence were found gradually decreased along the extension of time. According to these results, it could beconcluded that the nano-capsules containing jasmine essence were able to resist the heat processing (80°C)below5hours. Furthermore, the thermal analysis was applied to explore the capability of jasmine essencenano-capsules against dry heating effect. The results found the nano-capsules processed at pH7,8displayed abetter heat-resistant capability than pH6. After15min heating at200°C, their total weight lose was only lessthan20%.
本论文所研究的对象为复合凝聚反应应用领域的一个极重要分支——胶囊化包埋。通过对不同尺度的复合凝聚物形成机理的研究，发现适用于纳米胶囊及微胶囊制备的不同反应阶段，以茉莉精油作为芯材，较为简便地获得相应胶囊化产品的制备工艺，并对其胶囊性质进行了一定的探索。具体研究内容及结果如下：
选取明胶-阿拉伯胶体系作为反应的原料组合，在不同的混合比例（2:1，1:1，1:2，w/w）下，测量逐滴添加醋酸后600nm的吸光值变化，得到浊度滴定曲线。通过对曲线不同阶段的分析，发现该体系可通过pH条件控制，形成可溶性复合物及不可溶性复合物阶段，即它们具备了形成纳米胶囊与微胶囊的可能性。
研究1:1混合比例下，相同pH值的明胶-阿拉伯胶体系的复聚物及以茉莉精油为芯材的微胶囊之间的关联性，具体为显微图像、产率及内部特性（抗机械外力-耐热性）。结果表明，二者之间具有极高的一致性，可借此简化微胶囊的工艺优化过程，概括如下：通过电位分析确定壁材之间可能的混合比例；浊度滴定曲线被用作选择最适混合比例及相应的pH条件；所得出的最适条件即可应用于微胶囊的制备。据此工艺优化过程，研究发现了一种新型多糖类壁材——羧甲基纤维素钠，显微图像结果表明其所形成的微胶囊结构与明胶-阿拉伯胶体系相似。
通过动态温度流变分析模拟两种产自不同树种的阿拉伯胶（A. Senegal：AA；A. Seyal：BA）与明胶发生复合凝聚反应包裹茉莉精油后的冷却过程。结果发现对于流变曲线中弹性模量大于粘性模量的阶段，明胶-BA体系较明胶-AA体系具有更低的温度，即意味着要达到同样的弹性模量值时，明胶-BA体系需使温度降至更低。由于弹性模量体现了体系的类固体性质，因此可通过二者流变曲线的差异来指导微胶囊制备过程中的冷却步骤，达到使价格较低的BA型阿拉伯胶与价格较高的AA型接近的显微形态效果。具体的冷却条件为：AA，20-10°C；BA，5-0°C。
选取三组混合比例（2:1，1:1，1:2）下的明胶-阿拉伯胶体系，利用多种手段研究其分子水平的复聚物形成机理。首先，通过显微图像及粒径分布分析发现，随pH的降低，1:1及1:2混合比例下的复聚物粒径逐渐增大，而2:1的复聚物粒径则逐渐减小。其次，原料转化率分析结果显示，复聚物的粒径转变趋势与阿拉伯胶的转化率变化相一致，即阿拉伯胶参与反应的数量越多，则复聚物粒径越大。最后，通过圆二光谱技术揭示了2:1混合比例下明胶、阿拉伯胶大分子的构象转变过程。在复聚物的形成中，明胶分子由无规卷曲结构转向了有序的PPII螺旋；阿拉伯胶分子则由部分有序的PPII螺旋转向了结构紧凑的PPI螺旋。该构象转变规律也体现于1:1与1:2的混合比例中。据此，推测复聚物粒径的改变是受分子水平的结构转变与参与反应的阿拉伯胶数量二者共同的影响。
利用等温滴定量热技术对复合凝聚反应中的结合等温线进行分析，进一步佐证了明胶-阿拉伯胶体系中存在可溶性复合物及不可溶性复合物的两阶段产物。通过不同温度下的曲线发现氢键作用对反应影响较大，低温促使更多氢键的生成。考虑到可溶性复合物的形成中静电相互作用极其有限，因此在以下纳米胶囊的制备中只需要常温条件（25~30°C）反应即可。
原位酸化剂——葡萄糖酸-δ-内酯被用于自发地缓慢改变体系的pH值，从而获得低水平下的浊度滴定曲线，探寻可溶性复合物的形成pH范围。结果表明，随明胶-阿拉伯胶混合比例的降低，相应的pH范围逐渐扩大。同时，通过NaCl及脲的添加发现大分子间的相互作用不仅包含起主导作用的静电相互作用，也与疏水相互作用有关。在确定可溶性复合物形成pH范围后，利用粒径分布分析获得适于纳米胶囊制备的最适pH条件及壁材比例（1:1，pH4.80）。其后，以平均粒径、多分散指数、电位及载量为指标，采用单因素优化，获得茉莉香精纳米胶囊的制备条件：明胶、阿拉伯胶比例1:1，总浓度0.5%；茉莉精油浓度0.5%；乳化剂（Span80: Tween80=1:1）浓度0.5%；固化剂转谷氨酰胺酶添加量0.25%。该条件下所制得的茉莉精油纳米胶囊平均粒径（r）为69.56nm，PDI值为0.135，带电量为-14.80mV。透射电镜结果与粒径测量结果相似，且充分证明了纳米胶囊对茉莉精油的包埋特性。
为获得具耐高温性的茉莉香精纳米胶囊，特对其固化过程进行研究。对不同pH条件（pH4.80，6.0，7.0，8.0）下固化的茉莉香精纳米胶囊进行80°C的水浴加热，结果表明中性或弱碱性条件下的固化能显著提高粒子所带电荷的绝对值，增加体系的稳定性。在pH7条件下固化的纳米胶囊，经过7h的加热后，粒径为101.89nm，多分散指数为0.106，电位为-9.45mV，它的稳定性仍优于未固化纳米胶囊的初始值（电位-8.67mV）。基于纳米胶囊在形成与热作用下的粒径转变现象，发现大分子吸附、固化交联、热展开等是导致其粒径变化的主要因素。
pH7固化条件下的茉莉香精纳米胶囊于加热不同时间下的挥发性物质分析结果发现，五种茉莉香精的特征性风味（芳樟醇，氨茴酸甲酯，顺-茉莉酮，二氢月桂烯醇，乙酸苄酯，乙酸苯乙酯，肉桂酸甲酯和吲哚）随加热时间的延长含量均下降。根据它们的下降趋势分析该纳米胶囊能耐受80°C、5h以内的加热条件。采用热重分析，对不同固化条件的茉莉香精纳米胶囊进行研究，以表征它们抵抗干热的能力。结果表明pH7、8条件下固化的纳米胶囊耐热性显著优于pH6的条件，它们经过200°C下15min的加热，体系的整体失重率仅为约20%。
Complex coacervation reaction is a self-assembled phenomenon that always happened among two orabove two kinds of macromolecules driven by electrostatic interactions. Through the application ofdifferent extents of reaction products, we could obtain series of complex coacervates with variable size,special surface capability or excellent emulsification. Such complex coacervates will confer great potentialsin industries like food, chemical engineering, pharmaceutical and textile. However, due to the largedifference among raw materials and big difficult in controlling the parameters, its process ofindustrialization is always slow.
The current paper was focused on an important application field of complex coacervation-microencapsulation. The formation mechanism of complex coacervates was been investigated to disclosethe variable reaction phases suitable for preparation of nano-capsule and microcapsule. Furthermore, thecorresponding capsule type products were specifically fabricated with jasmine essence as core material;also their capsules’ characteristics were explored. The main contents are as follows:
The gelatin-gum arabic system was chosen as raw materials of the reaction. Firstly, the turbidity titrationcurve at variable mixing ratios (2:1，1:1，1:2，w/w) for gelatin-gum arabic was obtained via drop-wise additionof acetic acid and then tested the absorbance values at600nm. Through analysis of the curve, it was found thatthis system could form soluble complexes and insoluble complexes by pH adjustment. In correspondence, thiscurve had the possibility to form nano-capsule and microcapsule.
The complex coacervates and corresponding microcapsules at the mixing ratio of1:1and the same pHrange were investigated to find their relationship in each other, for the purpose of simplifying microcapsulepreparation optimization processing. Comparisons on morphology, yield and internal characteristic(anti-mechanical force capability-heat-resistance) were performed. Finally, a simplified method was proposed,in which the zeta-potential measurement helps to establish the approximate mixing ratios of wall materials; theturbidity analysis facilitates the finding of suitable pH corresponded to the highest turbidity to make the perfectmicrocapsule. According to this method, a new combination of wall materials named gelatin and sodiumcarboxymethyl cellulose was provided and verified by morphology.
The dynamic-temperature rheological analysis was applied to investigate the cooling process ofcomplex coacervation happened between gelatin and two variety of gum arabic from different types of tree(A. Senegal: AA; A. Seyal: BA). It was found that the systems composed of different gum arabic conferredgreat variance on the property of viscoelasticity. In particular, the transition temperature from viscosity toelasticity was much higher for AA type complexes than BA type complexes. As the elasticity representedthe solid-like capability, such rheological curve could be applied to guide the preparation of microcapsuleby adjusting the cooling conditions. Therefore, the cheaper BA type gum arabic could own a similarmorphology with AA type. The specific cooling conditions are20-10°C for AA and5-0°C for BA。
The coacervates of gelatin and gum arabic with three mixing ratios (2:1,1:1and1:2, w/w) wereprepared in order to elucidate their pH-dependent complexation mechanism. Firstly, the analysis ofmorphology and size distribution showed that with pH decline, the coacervates became larger for themixing ratio of1:1and1:2; whereas, the trend went oppositely as to the mixing ratio of2:1. Through thecomposition analysis of coacervates, such transition pattern was found to be consistent with the conversionrate of gum arabic. Coacervates prepared by the mixing ratio of2:1were chosen to further investigate theformation mechanism at the molecular level. During the complexation process with pH decrease, gelatinmolecules experienced a conformational change from a flexible pattern to an ordered PPII helix. On theother hand, gum arabic went through a transition from partly ordered PPII helix to a more compactstructure, called PPI helix. Such characteristics of conformational transition were also similar for thesystems with mixing ratios of1:1and1:2. Therefore, it was presumed that the change of coacervates size was due to the combined reasons including the conformational transition and the reacted amount of gumarabic.
The isothermal titration calorimetry was used to analyze the binding isotherm for complexcoacervation. The curve verified again the existence of two phase products, including soluble complexesand insoluble complexes. Also, the curves at different temperatures showed that hydrogen bond played animportant role for structure formation. Specifically, the low temperature facilitated more hydrogen bondproduced. Considering the limit electrostatic interactions existed for soluble complexes, the correspondingnano-capsules could be strengthened by hydrogen bond through reacting just at room temperature, withoutthe need of heating.
The colloidal behavior of soluble complexes was investigated using turbidity titration (600nm) withthe help of an in situ acidification-glucono-δ-lactone. The results showed that, with the decrease of mixingratio, the corresponding pH range for soluble complexes became a little larger. Furthermore, the addition ofNaCl and urea indicated the interactions between macromolecules were not only electrostatic interactions,but also hydrophobic interactions. Through the analysis of particle distribution, pH4.80under the mixingratio of1:1was chosen as the favorable condition for the nano-particles preparation. Subsequently,corresponding nano-capsules with jasmine essential oil entrapped were prepared. Based on the parametersof general size, polydispersity index (PDI), zeta potential and load, the best nano-capsules weresuccessfully prepared (r=69.56nm, PDI=0.135and zeta potial=-14.80mV) The optimized conditions wereselected as follows: total concentration0.5%, jasmine essence concentration0.5%, emulsifier concentration0.5%, emulsifier composition Span80and Tween80(1:1), cross-linker transglutaminase (0.25%). Theresults of transmission electron morphology were consistent with the particle size distribution, furtherverifying the encapsulation capability of nano-capsules.
In order to obtain heat-resistant jasmine essence nano-capsules, the hardening process via cross-linkertransglutaminase was investigated. Their heat-resistance capability against80°C water bath was evaluated bysize, PDI and zeta potential. The results showed that the nanocapsules cross-linked at alkaline conditionsconferred a better stability. Specifically, the nano-capsules processed at pH7for hardening process could endurethe incubation at80°C for7h. The final characteristics are as follows: size=101.89nm, PDI=0.106, zetapotential=-9.45mV. Such particles stability were still better than the original value of un-hardenednano-capsules (zeta potentiall=-8.67mV). Based on the particle size transition rules among nano-capsules’formation and heat effect, it signified the macromolecules’ absorption, cross-linkage and heat-unfolding were themain reasons for size variation.
During the analysis of volatile compounds for jasmine essence nano-capsules hardened at pH7undervariable heating time, five characteristic flavor compounds (linalool, methyl anthranilate, cis-jasmone,dihydromyrcenol, benzyl acetate, acetic acid phenethyl ester, cinnamic acid methyl ester and indole) for jasmineessence were found gradually decreased along the extension of time. According to these results, it could beconcluded that the nano-capsules containing jasmine essence were able to resist the heat processing (80°C)below5hours. Furthermore, the thermal analysis was applied to explore the capability of jasmine essencenano-capsules against dry heating effect. The results found the nano-capsules processed at pH7,8displayed abetter heat-resistant capability than pH6. After15min heating at200°C, their total weight lose was only lessthan20%.
引文
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