浓缩诱导含钙离子的海藻酸钠与高酯果胶体系胶凝及其应用的研究
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摘要
海藻酸钠与高酯果胶是来源广泛的天然水溶性多糖，因其具有独特的胶凝特性而被广泛应用于食品和医药领域。海藻酸钠凝胶通常用钙离子胶凝方法制备，而高酯果胶的胶凝作用也受钙离子影响。然而，海藻酸钠的遇钙胶凝机理还有待完善，而钙离子对高酯果胶胶凝过程的作用机理还不清楚，并且常用的钙离子胶凝方法存在难以控制胶凝过程或需引入研究对象以外的化学物质的弊端，因此不适用于研究海藻酸钠与高酯果胶的涉钙胶凝过程。本文首先建立了一种新的钙离子胶凝方法；其次在此基础上，从有利于实际生产应用的角度出发，研究了海藻酸钠与高酯果胶的涉钙胶凝过程，以期进一步完善其涉钙胶凝机理；最后，探究了此钙离子胶凝方法在保健食品中的应用前景，以期拓宽海藻酸钠与高酯果胶的应用范围。
首先，以相同来源但粘度等级不同的海藻酸钠（分别用LA和MA指代低等粘度和中等粘度的海藻酸钠）为研究对象，通过流变学方法构建了海藻酸钠的浓缩诱导型钙离子胶凝体系，并研究了海藻酸钠分子链在含钙离子体系浓缩过程中的相互作用。凝胶渗透色谱和1H核磁共振光谱分析结果表明，LA和MA的结构差异主要在于其分子量分布不同。流变学研究结果表明，1%（w/v）海藻酸钠与4μmol/mL CaCl2是构建LA和MA的浓缩诱导型钙离子胶凝体系的较适初始条件，该体系在水分蒸发过程中由具有良好流动特性的溶液状态转变成了具有均一网状结构的凝胶状态。另外，LA和MA分别按照重量比0:4、1:3、2:2、3:1和4:0复配而成的含钙离子水溶性体系在流动特性和胶凝行为方面呈现出显著差异，说明海藻酸钠的分子量分布对以钙离子为媒介的海藻酸钠分子链相互作用具有重要的影响。
其次，以海藻酸钠的浓缩诱导型钙离子胶凝过程和“蛋盒”结构胶凝机理为参考，用浓缩诱导型钙离子胶凝方法研究了钙离子在高酯果胶胶凝过程中的作用。结果表明，在水分蒸发过程中，含有2.72μmol/mL CaCl2的浓度为1%（w/v）的高酯果胶（甲酯化度为75.6%）水溶性体系所形成凝胶的强度（储存模量G′约为1140000Pa）高于海藻酸钠参照体系，证明钙离子参与了高酯果胶的胶凝过程，同时说明可能还存在其它因素导致高酯果胶形成凝胶；与海藻酸钠水溶性体系相比，相同的钙离子添加量对高酯果胶水溶性体系的流体行为具有更强的削弱作用：其流动指数n降低了29%、粘稠指数k升高了1226%、损耗角δ减小了30°，说明钙离子很可能通过非结合性方式与高酯果胶分子相互作用而参与了高酯果胶的胶凝过程；不含钙离子的高酯果胶水溶性体系在单独水分蒸发作用下，δ角减小了33.7%，但该体系不能在水分蒸发过程中形成凝胶，并且钙离子的存在使其δ角从62°减小到29°，说明钙离子对高酯果胶的胶凝过程具有引发和加速的作用；高酯果胶分子与钙离子之间不存在明显的最适相互作用比例，而高酯果胶含钙离子水溶性体系需要蒸发大量水分后才能形成凝胶，并且所形成的凝胶具有明显高于海藻酸钠参照体系的游离钙离子含量，这些研究结果表明，钙离子通过与其在海藻酸钠胶凝过程中不同的作用方式引发和加速了高酯果胶的胶凝过程。
再次，在明确海藻酸钠与高酯果胶的浓缩诱导型钙离子胶凝作用的基础上，将海藻酸钠与高酯果胶分别以3:1、2:2和1:3重量比复配成水溶性体系（分别用A3P1、A2P2和A1P3表示），研究了钙离子对该体系流动特性（用流动指数n和粘稠指数k来表征）、物理状态特性（用损耗角δ来表征）和浓缩诱导型钙离子胶凝特性（用储存模量G′和损耗模量G″来表征）的影响。结果表明，钙离子的存在改变了A/P（指代海藻酸钠与高酯果胶复配）水溶性体系的n值、k值和δ值与其A/P配比之间的线性关系，使得A1P3、A3P1和A2P2体系的n值依次降低、k值依次升高，而A2P2和A1P3体系的δ值因钙离子的存在而减小至45°以下；在水分蒸发过程中，A3P1和A1P3的含钙离子水溶性体系（分别用CaA3P1与CaA1P3表示）呈现了浓缩诱导型钙离子胶凝过程，而A2P2的含钙离子水溶性体系（CaA2P2）始终保持非凝胶状态。这些研究结果表明，钙离子的存在使A/P体系具有与海藻酸钠/高酯果胶单一体系所不同的流变学性质。
最后，将浓缩诱导型钙离子胶凝方法与喷雾干燥法结合制备出海藻酸钠/高酯果胶的浓缩诱导型钙离子凝胶，并将其用作原淀粉的生味掩盖剂和共轭亚油酸（CLA）的抗氧化控释载体。首先研究了该凝胶作为淀粉生味掩盖剂的应用效果：用扫描电子显微镜观察淀粉-海藻酸钠凝胶微球发现，海藻酸钠凝胶包覆于淀粉颗粒表面；与原料蜡质玉米淀粉相比，淀粉-海藻酸钠凝胶微球在牛奶中的淀粉生味、粗糙口感和入喉异感都明显减小，使得牛奶依然保持原来的风味和光滑的口感，因此，该凝胶可用作淀粉生味掩盖剂促进禾谷类原淀粉作为慢消化淀粉的直接应用。然后，研究了浓缩诱导型钙离子凝胶作为CLA载体的应用效果：CaA3P1形成的浓缩诱导型钙离子凝胶在模拟胃和小肠消化试验中显示出相对适用于构建小肠定位释放载体的消化稳定性；25mL1%（w/v）辛烯基琥珀酸淀粉酯（OSA淀粉）糊液能与1mL CLA形成稳定性较好的乳状液，并且OSA淀粉糊液中的游离直链淀粉在乳化操作过程中能与CLA相互作用形成稳定的复合物，因而，利用OSA淀粉的乳化稳定作用能将CLA引至海藻酸钠/高酯果胶的水溶性体系中；钙离子的存在使CaA3P1与OSA淀粉-CLA乳状液的混合物（以4:1体积比混合）经过喷雾干燥后能形成CLA载体；经过同等条件的加速氧化处理后，无载体保护的CLA的过氧化值（POV）是原来的10.3倍，而受载体保护的CLA的POV是原来的1.6倍，说明浓缩诱导型钙离子凝胶载体对CLA具有较好的抗氧化保护作用；该载体在模拟胃和小肠消化条件下对CLA的释放率分别为44(±1.8)%和50(±2.9)%，说明该载体对CLA的小肠定位释放性能还有待进一步提高。
从上述研究内容与结果可以看出：1.浓缩诱导型钙离子胶凝方法是一种简单且便于控制的钙离子胶凝方法；2.可以通过调整粘度等级不同的普通海藻酸钠商品的复配比例来调控海藻酸钠与钙离子的相互作用，以获得具有理想应用性能的海藻酸钠产品；3.高酯果胶在含钙离子水溶性体系浓缩过程中所展现的胶凝特性可应用于生产新的钙离子类果胶凝胶；4. CaA2P2具有最弱流动特性和最强固体状态特性，并且在水分蒸发过程中不能形成凝胶，使其可作为热稳定型增稠剂应用于食品工业，而CaA3P1和CaA1P3具有较好的流动特性和浓缩诱导型钙离子胶凝特性，使其可作为胶凝剂应用于食品和医药工业；5.海藻酸钠与高酯果胶的浓缩诱导型钙离子胶凝过程及其与喷雾干燥法相结合的胶凝方法在食品和医药领域具有较好的实际应用前景。
Sodium alginate (SA) and high methoxy pectin (HMP) are water-soluble polysaccharides with naturaland abundant sources, and they are widely applied in the food and pharmaceutical industries due to theirgel-forming properties. SA gels are usually produced by Ca~(2+)gelling methods (CGMs), and the gelation ofHMP is also affected by Ca~(2+). However, the gelling mechanism of SA with Ca~(2+)still needs to be improved,and the acting mechanism of Ca~(2+)in the gelation of HMP is still unclear. Furthermore, the commonly usedCGMs are not appropriate for the investigation of the Ca~(2+)-involved gelling processes (CIGPes) of SA andHMP as the methods either fail to control the gelling process or introduce other materials besides thesubjects into the investigated systems. Therefore, in order to better understand the Ca~(2+)-involved gellingmechanisms of SA and HMP as well as to broaden their application range, a new method namedconcentration-induced Ca~(2+)gelling method (CICGM) was developed in the study, and the CIGPes of SAand HMP were investigated using the gelling method from the aspects beneficial to practical applications.
Firstly, a concentration-induced Ca~(2+)gelling system (CICGS) of SA was developed using two SAshaving different viscosity (low-viscosity alginate (LA) and medium-viscosity alginate (MA)) obtained fromthe same brown algae, and their chain interactions during the concentration-induced Ca~(2+)gelling process(CICGP) were investigated rheologically. The main structural differences between LA and MA were foundto be their molecular weight distributions according to the analysis results of gel permeationchromatography and1H nuclear magnetic resonance. As shown by the rheological investigation results,1%(w/v) of SA and4μmol/mL of CaCl2were the appropriate initial conditions for preparing a SA CICGSwhich can be converted from a solution state with good flow properties to a gel state of uniform meshstructure during water evaporation. Furthermore, the Ca~(2+)-containing aqueous systems composed of LAand MA mixed at ratios of0:4,1:3,2:2,3:1and4:0(weight basis) showed significantly different flowproperties and concentration-induced Ca~(2+)gelling behavior, indicating that the molecular weightdistributions of SAs have important influence on their molecular chain interactions mediated by Ca~(2+).
Secondly, using the CICGP of SA and its “egg-box” gelling mechanism as references, the effect ofCa~(2+)on the gelation of HMP was investigated by the CICGM. The aqueous system composed of1%(w/v)of HMP (75.6%of degree of methyl esterification) and4μmol/mL of CaCl2formed a gel whose strength(storage modulus G′≈1140000Pa) was higher than that of the referenced SA system during waterevaporation. This result confirms that Ca~(2+)participates in the gelation of HMP, and also suggests that thegelation of HMP likely involves other factors besides the participation of Ca~(2+). Compared with the SAaqueous system, the flow behavior of the HMP aqueous system was weakened in a greater extent by thesame amount of Ca~(2+)addition (flow index n decreased by29%, consistency index k increased by1226%,and loss angle δ reduced by30°), indicating that the Ca~(2+)likely participates in the gelling process of HMPthrough a non-binding interaction with the HMP molecules. Furthermore, the Ca~(2+)-free aqueous system ofHMP could not form gels in the water evaporation although33.7%of its δ value was reduced by the waterevaporation. However, the δ value of the HMP aqueous system was reduced from62°to29°due to theexistence of Ca~(2+). These results indicate that Ca~(2+)plays a role of triggering and accelerating in the gelationof HMP, and the function of Ca~(2+)was achieved through an acting way different from its acting way in thegelation of SA as supported by the absence of an optimal ratio of HMP-Ca~(2+)interactions and the high freeCa~(2+)content in the HMP gel formed after large amount of water was evaporated in comparison with the SAsystem.
Thirdly, the effect of Ca~(2+)on the flow properties (charactered by n and k), physical state properties(charactered by δ) and concentration-induced Ca~(2+)gelling properties (charactered by storage modulus G′and loss modulus G″) of the aqueous systems composed of mixed SA and HMP (A/P) at weight-basis ratios of3:1,2:2and1:3(labelled as A3P1, A2P2and A1P3, respectively) were investigated basingunderstanding the gelation of Ca~(2+)-containing aqueous systems of SA and HMP during water evaporation.The existence of Ca~(2+)changed the linear relationship between the n, k and δ values of the A/P systems andtheir A/P ratios. Specifically, due to the existence of Ca~(2+), the n values of the A1P3, A3P1and A2P2decreased orderly while their k values increase orderly, and the δ values of the A2P2and A1P3werereduced below45°. During water evaporation, the Ca~(2+)-containing aqueous systems of both A3P1andA1P3(labelled as CaA3P1and CaA1P3, respectively) showed a CICGP while the Ca~(2+)-containing aqueoussystem of A2P2(CaA2P2) kept in a non-gel state all the time. These results manifest that the rheologicalproperties of the A/P aqueous systems are distinctly different from those of the aqueous systems of SA orHMP alone due to the existence of Ca~(2+).
Finally, the CICGM was combined with spray drying method to prepare a concentration-induced Ca~(2+)gel (CICG), and the gels were applied as a masked agent of raw taste for starch and an antioxidative andcontrol-release carrier for conjugated linoleic acid (CLA). The CICG of SA in the starch-SA gel microbeadswas observed to be coating on the surface of the starch granules using scanning electron microscopy.Compared with the raw material waxy corn starch, the starch-SA gel microbeads showed much weaker rawtaste, rough feeling and unpleasant throat feeling in milk, and kept the original flavor and smoothmouthfeel of the milk. This comparison result indicates that the CICGP of SA can be applied as a maskedagent of raw taste for starch to facilitate the direct application of cereal raw starch as slowly digestiblestarch. In addition, the CICG formed by the CaA3P1showed digestion stability relatively appropriate fordeveloping small intestine-target release carriers. Octenyl succinic anhydride modified starch (OSA starch)paste (1%, w/v) and CLA mixed at a volume ratio of25:1could form a stable emulsion, and the freeamylose in the paste could form stable complexes with CLA during the emulsifying operation, so CLA canbe introduced into the aqueous systems of SA and HMP through the emulsifying and stabilizing effects ofthe OSA starch on it. CaA3P1and OSA starch-CLA emuolsion mixed at a volume ratio of4:1could formCLA carriers through spray drying due to the existence of Ca~(2+). After the same accelerated oxidationtreatment, the peroxide value (POV) of the CLA without carrier protection was10.3times of its originalPOV while the POV of the CLA in the carriers was1.6times of its original POV, indicating that the CICGcarriers have a good antioxidative protection effect on CLA. Besides, the CICG carriers released44(±1.8)%and50(±2.9)%of CLA in simulated stomach and small intestine conditions, repectively, suggesting thatthe small intestine-target release properties of the carriers for CLA need to be improved.
Briefly, the following conclusions can be drawn based on the above investigated contents and results:1. CICGM is simple and easy for controlling the gelling process;2. the SA-Ca~(2+)interactions can beregulated through adjusting the mixing ratios of the commercial SAs of different viscosity to produce SAproducts with desirable application properties;3. the gelling properties of HMP shown in the concentratingprocess of its Ca~(2+)-containing aqueous systems can be used to produce new Ca~(2+)-related pectin gels;4. theCaA2P2, which can not form gels in water evaporation but has the weakest flow properties and thestrongest solid state properties, can be applied as a heat-stable thickener in the food industry, and theCaA3P1and CaA1P3having good flow properties and concentration-induced Ca~(2+)gelling properties canbe applied as gelling agents in the food and pharmaceutical industries;5. the CICGM combined with spraydrying, and the CICGPs of SA and HMP have good practical application prospects in the field of food andmedicine.
首先，以相同来源但粘度等级不同的海藻酸钠（分别用LA和MA指代低等粘度和中等粘度的海藻酸钠）为研究对象，通过流变学方法构建了海藻酸钠的浓缩诱导型钙离子胶凝体系，并研究了海藻酸钠分子链在含钙离子体系浓缩过程中的相互作用。凝胶渗透色谱和1H核磁共振光谱分析结果表明，LA和MA的结构差异主要在于其分子量分布不同。流变学研究结果表明，1%（w/v）海藻酸钠与4μmol/mL CaCl2是构建LA和MA的浓缩诱导型钙离子胶凝体系的较适初始条件，该体系在水分蒸发过程中由具有良好流动特性的溶液状态转变成了具有均一网状结构的凝胶状态。另外，LA和MA分别按照重量比0:4、1:3、2:2、3:1和4:0复配而成的含钙离子水溶性体系在流动特性和胶凝行为方面呈现出显著差异，说明海藻酸钠的分子量分布对以钙离子为媒介的海藻酸钠分子链相互作用具有重要的影响。
其次，以海藻酸钠的浓缩诱导型钙离子胶凝过程和“蛋盒”结构胶凝机理为参考，用浓缩诱导型钙离子胶凝方法研究了钙离子在高酯果胶胶凝过程中的作用。结果表明，在水分蒸发过程中，含有2.72μmol/mL CaCl2的浓度为1%（w/v）的高酯果胶（甲酯化度为75.6%）水溶性体系所形成凝胶的强度（储存模量G′约为1140000Pa）高于海藻酸钠参照体系，证明钙离子参与了高酯果胶的胶凝过程，同时说明可能还存在其它因素导致高酯果胶形成凝胶；与海藻酸钠水溶性体系相比，相同的钙离子添加量对高酯果胶水溶性体系的流体行为具有更强的削弱作用：其流动指数n降低了29%、粘稠指数k升高了1226%、损耗角δ减小了30°，说明钙离子很可能通过非结合性方式与高酯果胶分子相互作用而参与了高酯果胶的胶凝过程；不含钙离子的高酯果胶水溶性体系在单独水分蒸发作用下，δ角减小了33.7%，但该体系不能在水分蒸发过程中形成凝胶，并且钙离子的存在使其δ角从62°减小到29°，说明钙离子对高酯果胶的胶凝过程具有引发和加速的作用；高酯果胶分子与钙离子之间不存在明显的最适相互作用比例，而高酯果胶含钙离子水溶性体系需要蒸发大量水分后才能形成凝胶，并且所形成的凝胶具有明显高于海藻酸钠参照体系的游离钙离子含量，这些研究结果表明，钙离子通过与其在海藻酸钠胶凝过程中不同的作用方式引发和加速了高酯果胶的胶凝过程。
再次，在明确海藻酸钠与高酯果胶的浓缩诱导型钙离子胶凝作用的基础上，将海藻酸钠与高酯果胶分别以3:1、2:2和1:3重量比复配成水溶性体系（分别用A3P1、A2P2和A1P3表示），研究了钙离子对该体系流动特性（用流动指数n和粘稠指数k来表征）、物理状态特性（用损耗角δ来表征）和浓缩诱导型钙离子胶凝特性（用储存模量G′和损耗模量G″来表征）的影响。结果表明，钙离子的存在改变了A/P（指代海藻酸钠与高酯果胶复配）水溶性体系的n值、k值和δ值与其A/P配比之间的线性关系，使得A1P3、A3P1和A2P2体系的n值依次降低、k值依次升高，而A2P2和A1P3体系的δ值因钙离子的存在而减小至45°以下；在水分蒸发过程中，A3P1和A1P3的含钙离子水溶性体系（分别用CaA3P1与CaA1P3表示）呈现了浓缩诱导型钙离子胶凝过程，而A2P2的含钙离子水溶性体系（CaA2P2）始终保持非凝胶状态。这些研究结果表明，钙离子的存在使A/P体系具有与海藻酸钠/高酯果胶单一体系所不同的流变学性质。
最后，将浓缩诱导型钙离子胶凝方法与喷雾干燥法结合制备出海藻酸钠/高酯果胶的浓缩诱导型钙离子凝胶，并将其用作原淀粉的生味掩盖剂和共轭亚油酸（CLA）的抗氧化控释载体。首先研究了该凝胶作为淀粉生味掩盖剂的应用效果：用扫描电子显微镜观察淀粉-海藻酸钠凝胶微球发现，海藻酸钠凝胶包覆于淀粉颗粒表面；与原料蜡质玉米淀粉相比，淀粉-海藻酸钠凝胶微球在牛奶中的淀粉生味、粗糙口感和入喉异感都明显减小，使得牛奶依然保持原来的风味和光滑的口感，因此，该凝胶可用作淀粉生味掩盖剂促进禾谷类原淀粉作为慢消化淀粉的直接应用。然后，研究了浓缩诱导型钙离子凝胶作为CLA载体的应用效果：CaA3P1形成的浓缩诱导型钙离子凝胶在模拟胃和小肠消化试验中显示出相对适用于构建小肠定位释放载体的消化稳定性；25mL1%（w/v）辛烯基琥珀酸淀粉酯（OSA淀粉）糊液能与1mL CLA形成稳定性较好的乳状液，并且OSA淀粉糊液中的游离直链淀粉在乳化操作过程中能与CLA相互作用形成稳定的复合物，因而，利用OSA淀粉的乳化稳定作用能将CLA引至海藻酸钠/高酯果胶的水溶性体系中；钙离子的存在使CaA3P1与OSA淀粉-CLA乳状液的混合物（以4:1体积比混合）经过喷雾干燥后能形成CLA载体；经过同等条件的加速氧化处理后，无载体保护的CLA的过氧化值（POV）是原来的10.3倍，而受载体保护的CLA的POV是原来的1.6倍，说明浓缩诱导型钙离子凝胶载体对CLA具有较好的抗氧化保护作用；该载体在模拟胃和小肠消化条件下对CLA的释放率分别为44(±1.8)%和50(±2.9)%，说明该载体对CLA的小肠定位释放性能还有待进一步提高。
从上述研究内容与结果可以看出：1.浓缩诱导型钙离子胶凝方法是一种简单且便于控制的钙离子胶凝方法；2.可以通过调整粘度等级不同的普通海藻酸钠商品的复配比例来调控海藻酸钠与钙离子的相互作用，以获得具有理想应用性能的海藻酸钠产品；3.高酯果胶在含钙离子水溶性体系浓缩过程中所展现的胶凝特性可应用于生产新的钙离子类果胶凝胶；4. CaA2P2具有最弱流动特性和最强固体状态特性，并且在水分蒸发过程中不能形成凝胶，使其可作为热稳定型增稠剂应用于食品工业，而CaA3P1和CaA1P3具有较好的流动特性和浓缩诱导型钙离子胶凝特性，使其可作为胶凝剂应用于食品和医药工业；5.海藻酸钠与高酯果胶的浓缩诱导型钙离子胶凝过程及其与喷雾干燥法相结合的胶凝方法在食品和医药领域具有较好的实际应用前景。
Sodium alginate (SA) and high methoxy pectin (HMP) are water-soluble polysaccharides with naturaland abundant sources, and they are widely applied in the food and pharmaceutical industries due to theirgel-forming properties. SA gels are usually produced by Ca~(2+)gelling methods (CGMs), and the gelation ofHMP is also affected by Ca~(2+). However, the gelling mechanism of SA with Ca~(2+)still needs to be improved,and the acting mechanism of Ca~(2+)in the gelation of HMP is still unclear. Furthermore, the commonly usedCGMs are not appropriate for the investigation of the Ca~(2+)-involved gelling processes (CIGPes) of SA andHMP as the methods either fail to control the gelling process or introduce other materials besides thesubjects into the investigated systems. Therefore, in order to better understand the Ca~(2+)-involved gellingmechanisms of SA and HMP as well as to broaden their application range, a new method namedconcentration-induced Ca~(2+)gelling method (CICGM) was developed in the study, and the CIGPes of SAand HMP were investigated using the gelling method from the aspects beneficial to practical applications.
Firstly, a concentration-induced Ca~(2+)gelling system (CICGS) of SA was developed using two SAshaving different viscosity (low-viscosity alginate (LA) and medium-viscosity alginate (MA)) obtained fromthe same brown algae, and their chain interactions during the concentration-induced Ca~(2+)gelling process(CICGP) were investigated rheologically. The main structural differences between LA and MA were foundto be their molecular weight distributions according to the analysis results of gel permeationchromatography and1H nuclear magnetic resonance. As shown by the rheological investigation results,1%(w/v) of SA and4μmol/mL of CaCl2were the appropriate initial conditions for preparing a SA CICGSwhich can be converted from a solution state with good flow properties to a gel state of uniform meshstructure during water evaporation. Furthermore, the Ca~(2+)-containing aqueous systems composed of LAand MA mixed at ratios of0:4,1:3,2:2,3:1and4:0(weight basis) showed significantly different flowproperties and concentration-induced Ca~(2+)gelling behavior, indicating that the molecular weightdistributions of SAs have important influence on their molecular chain interactions mediated by Ca~(2+).
Secondly, using the CICGP of SA and its “egg-box” gelling mechanism as references, the effect ofCa~(2+)on the gelation of HMP was investigated by the CICGM. The aqueous system composed of1%(w/v)of HMP (75.6%of degree of methyl esterification) and4μmol/mL of CaCl2formed a gel whose strength(storage modulus G′≈1140000Pa) was higher than that of the referenced SA system during waterevaporation. This result confirms that Ca~(2+)participates in the gelation of HMP, and also suggests that thegelation of HMP likely involves other factors besides the participation of Ca~(2+). Compared with the SAaqueous system, the flow behavior of the HMP aqueous system was weakened in a greater extent by thesame amount of Ca~(2+)addition (flow index n decreased by29%, consistency index k increased by1226%,and loss angle δ reduced by30°), indicating that the Ca~(2+)likely participates in the gelling process of HMPthrough a non-binding interaction with the HMP molecules. Furthermore, the Ca~(2+)-free aqueous system ofHMP could not form gels in the water evaporation although33.7%of its δ value was reduced by the waterevaporation. However, the δ value of the HMP aqueous system was reduced from62°to29°due to theexistence of Ca~(2+). These results indicate that Ca~(2+)plays a role of triggering and accelerating in the gelationof HMP, and the function of Ca~(2+)was achieved through an acting way different from its acting way in thegelation of SA as supported by the absence of an optimal ratio of HMP-Ca~(2+)interactions and the high freeCa~(2+)content in the HMP gel formed after large amount of water was evaporated in comparison with the SAsystem.
Thirdly, the effect of Ca~(2+)on the flow properties (charactered by n and k), physical state properties(charactered by δ) and concentration-induced Ca~(2+)gelling properties (charactered by storage modulus G′and loss modulus G″) of the aqueous systems composed of mixed SA and HMP (A/P) at weight-basis ratios of3:1,2:2and1:3(labelled as A3P1, A2P2and A1P3, respectively) were investigated basingunderstanding the gelation of Ca~(2+)-containing aqueous systems of SA and HMP during water evaporation.The existence of Ca~(2+)changed the linear relationship between the n, k and δ values of the A/P systems andtheir A/P ratios. Specifically, due to the existence of Ca~(2+), the n values of the A1P3, A3P1and A2P2decreased orderly while their k values increase orderly, and the δ values of the A2P2and A1P3werereduced below45°. During water evaporation, the Ca~(2+)-containing aqueous systems of both A3P1andA1P3(labelled as CaA3P1and CaA1P3, respectively) showed a CICGP while the Ca~(2+)-containing aqueoussystem of A2P2(CaA2P2) kept in a non-gel state all the time. These results manifest that the rheologicalproperties of the A/P aqueous systems are distinctly different from those of the aqueous systems of SA orHMP alone due to the existence of Ca~(2+).
Finally, the CICGM was combined with spray drying method to prepare a concentration-induced Ca~(2+)gel (CICG), and the gels were applied as a masked agent of raw taste for starch and an antioxidative andcontrol-release carrier for conjugated linoleic acid (CLA). The CICG of SA in the starch-SA gel microbeadswas observed to be coating on the surface of the starch granules using scanning electron microscopy.Compared with the raw material waxy corn starch, the starch-SA gel microbeads showed much weaker rawtaste, rough feeling and unpleasant throat feeling in milk, and kept the original flavor and smoothmouthfeel of the milk. This comparison result indicates that the CICGP of SA can be applied as a maskedagent of raw taste for starch to facilitate the direct application of cereal raw starch as slowly digestiblestarch. In addition, the CICG formed by the CaA3P1showed digestion stability relatively appropriate fordeveloping small intestine-target release carriers. Octenyl succinic anhydride modified starch (OSA starch)paste (1%, w/v) and CLA mixed at a volume ratio of25:1could form a stable emulsion, and the freeamylose in the paste could form stable complexes with CLA during the emulsifying operation, so CLA canbe introduced into the aqueous systems of SA and HMP through the emulsifying and stabilizing effects ofthe OSA starch on it. CaA3P1and OSA starch-CLA emuolsion mixed at a volume ratio of4:1could formCLA carriers through spray drying due to the existence of Ca~(2+). After the same accelerated oxidationtreatment, the peroxide value (POV) of the CLA without carrier protection was10.3times of its originalPOV while the POV of the CLA in the carriers was1.6times of its original POV, indicating that the CICGcarriers have a good antioxidative protection effect on CLA. Besides, the CICG carriers released44(±1.8)%and50(±2.9)%of CLA in simulated stomach and small intestine conditions, repectively, suggesting thatthe small intestine-target release properties of the carriers for CLA need to be improved.
Briefly, the following conclusions can be drawn based on the above investigated contents and results:1. CICGM is simple and easy for controlling the gelling process;2. the SA-Ca~(2+)interactions can beregulated through adjusting the mixing ratios of the commercial SAs of different viscosity to produce SAproducts with desirable application properties;3. the gelling properties of HMP shown in the concentratingprocess of its Ca~(2+)-containing aqueous systems can be used to produce new Ca~(2+)-related pectin gels;4. theCaA2P2, which can not form gels in water evaporation but has the weakest flow properties and thestrongest solid state properties, can be applied as a heat-stable thickener in the food industry, and theCaA3P1and CaA1P3having good flow properties and concentration-induced Ca~(2+)gelling properties canbe applied as gelling agents in the food and pharmaceutical industries;5. the CICGM combined with spraydrying, and the CICGPs of SA and HMP have good practical application prospects in the field of food andmedicine.
引文
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