挤压法糖玻璃化包埋维生素的研究
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摘要
L-抗坏血酸(AA)通常称为维生素C,是一种重要的具有生理生化功能的水溶性化合物,是维持人体正常调节功能所必须的功能活性成分。AA除了在人体内具有营养作用外,也作为一种抗氧化剂成分被广泛应用于各种食品配料中。AA有助于无机铁的吸收并且能抑制体内致癌化合物的生成,也可作为辅酶因子参与肉碱的合成、促进胶原蛋白合成,同时可以调节神经系统及提高免疫力。AA在降低严重疾病如心脏病、癌症等方面的潜在作用也受到关注。随着对这种重要食品成分功能性质认识的提高,人们越来越多的将其加入各种食品体系中。但是AA的高反应活性不但使其易失活还会使得整个食品体系不稳定,因此在应用前需要进行稳定化。
本论文研究了利用挤压法制备水溶性维生素(AA为代表)的糖玻璃化胶囊的方法,同时也对油溶性维生素(维生素E为代表)的挤压糖玻璃化技术进行了研究。以便建立既可用于包埋水溶性功能因子又能包埋油溶性功能因子的挤压糖玻璃化共性包埋技术。系统研究了挤压糖玻璃化胶囊的制备工艺和配方的选择并对产品性质进行了深入的分析。
主要研究内容如下：
1.以低DE值的麦芽糊精作为基质,利用挤压法将AA包埋于玻璃化基质中。主要研究了配方参数如芯壁比和水分添加量(增塑剂)对挤压产品玻璃化转变温度(Tg)的影响。对不同配方产品中AA的产率、含量和水分含量以及挤压参数进行了测定和比较。结果如下：水分含量和芯壁比对产品Tg影响较大,水分含量从7.860%提高到10.430%时,挤压产品的Tg值从43.17℃降低到27.48℃；芯壁比从1：4变化到1：8时,Tg值从35.79-C上升到41.46℃。挤压产品的AA产率高于96%,随着产品中水分含量的增加,AA产率略有下降。提高水分添加量和芯壁比可以减少挤压的特定机械能和模头压力。通过X-射线衍射分析,AA可能以分子分散的形式分散于麦芽糊精基质中。
2.以高DE值的麦芽糊精作为基质,采用挤压法制备糖玻璃化AA胶囊。考察了挤压腔温度、螺杆转速和喂料速度对挤压过程中电机扭拒(扭矩百分比)、模头压力的影响。分析了挤压产品的AA含量、产率和挤压产品Tg等理化指标。结果表明：提高挤压腔温度、增加螺杆转速和降低喂料速度可以减小电机扭矩及模头压力。确定的挤压腔温度、螺杆转速和进料速度分别为中温(85℃—105℃—120℃—105℃)、60 rpm和1.1 kg/h。在优化的挤压工艺基础上,以高DE值的麦芽糊精作为主要基质,在配方中添加阿拉伯胶和海藻糖,采用优化后的挤压工艺将AA包埋于低水分含量／固态／玻璃态的混合碳水化合物基质中。对产品的理化指标进行了分析,得到挤压产品中AA载量高于15.67g/100g的挤压产品,AA的产率大于97%,产品的Tg高于40℃。添加海藻糖会使产品的Tg降低,而添加阿拉伯胶可减小产品的膨胀率。扫描电子显微镜、X-射线衍射和傅里叶变换红外光谱分析表明AA分散于碳水化合物基质中形成了玻璃态的固溶体。20-40目挤压产品的溶解实验表明其具有较快的溶解速率,其中的AA可以在10min内完全溶解释放,且溶解速率由碳水化合物基质控制。将挤压产品应用于配方奶粉中,AA的损失明显减小,表明将AA包埋于糖玻璃化基质中可以降低AA与食品体系中其他成分的反应,从而更好的保护AA。
3.采用挤压法制备了低聚异麦芽糖为基质的AA无糖玻璃化胶囊。选择了10%和16%两种AA含量的配方,在螺杆转速60 rpm,喂料速度1 kg/h的条件下,研究了三种挤压腔温度时的挤压工艺。探讨了挤压过程中电机扭拒、模头压力等的变化规律。采用差式扫描量热法、X-射线衍射对产品性质进行了表征。对挤压产品中AA的产率和载量等理化指标进行了分析。结果表明：提高挤压腔温度可以减小电机扭矩和模头压力,AA含量对三种温度条件下的电机扭矩影响较小。当挤压腔为中温和低温时,AA含量的增加可以使模头压力减小。两种含量下的AA均得到了很好的包埋,挤压产物的Tg随着AA含量增加而降低。X-射线分析表明AA以分子形式分散于基质中,形成了固溶体。将挤压产品应用于配方奶粉中,AA的保留率得到较大提高。
4.利用挤压法将维生素E(VE)包埋于碳水化合物基质中。选择了四种典型的配方,其中配方中分别含有5%和8%的VE,配方中添加了20%和30%的变性淀粉于麦芽糊精中作为基质。四种配方中都添加1%的大豆卵磷脂作为乳化剂。挤压中喂料速度设定为1.2 kg/h,挤压腔的温度设定分别为T1(65℃),T2(950C),T3(115℃)和T4(105℃),螺杆转速保持60 rpm。对挤压过程中电机扭矩、特定机械能和模头压力等指标进行了测定和分析,对挤压产品的理化性质进行了研究。结果表明：提高VE含量或者减少变性淀粉含量可以使得电机扭矩、特定机械能和模头压力减小。使用具有乳化作用的变性淀粉对于油溶性物质的包埋具有重要作用。挤压后VE的保留率高于93%。变性淀粉和高HLB值乳化剂的使用使VE以小液滴形态分散于基质中,并且液滴大小和分布比较均匀。在贮藏期间,VE略有损失,但保留率显著高于未包埋的VE,VE得到了很好的包埋。得到的挤压产品的Tg高于30℃,并且Tg可以作为温度提高时产品结块性的良好预测指标。
L-Ascorbic acid (AA) commonly known as Vitamin C is a physiologically and biochemically essential water soluble bioactive compound required for the normal regulatory functions. AA has been extensively used in variety of food formulations and acts as an antioxidant agent besides its nutritional role in the human body. It is established that AA helps in the absorption of inorganic Fe and inhibits the formulation of carcinogenic compounds in the body. It also acts as co-factor for enzymes, involves in the biosynthesis of carnitine, stimulates collagen synthesis, modulates neurotransmitter systems and offers improved immunity against diseases. Its possible role in minimizing the risk of serious diseases such as heart diseases and cancer is very interesting. With the improved knowledge of functional properties of this vital food ingredient, the trend to incorporate it into different food systems is increasing. Due to the highly unstable nature, AA is prone to be degradation and also destabilize the whole food system. Therefore, it is important to stabilize AA prior to its application.
The technique of the encapsulation of vitamins (AA and vitamin E) in glassy carbohydrates employing extrusion was investigated. The processes and formulations of the technique were studied. And the characteristics of the extrudated products were analysised. Major contents of this paper are as following:
1. AA was encapsulated in glassy low dextrose equivalent (DE) maltodextrin (DE 8-10) matrix by extrusion. The effects of formulation parameters i.e., core-matrix ratio and moisture content were mainly investigated on glass transition temperature (Tg) of extrudates. The AA yield, AA content and moisture of the products together with extrusion parameters were also measured and compared for different formulations. Both the water content and AA content have a great effect on Tg. The Tg of extrudates containing water content from 7.860% to 10.430% decreased from 43.17℃to 27.48℃and The Tg of extrudates which core to matrix from 1:4 to 1:8 increased from 35.79℃to 41.64℃. AA yield of all samples is above 96% and with increasing water content there was a small decrease in the AA yield. The increased water level and core-matrix ratio reduce specific mechanical energy and die head pressure. From X-ray diffraction result, AA was most likely molecularly dispersed within the maltodextrin matrix.
2. Extrusion was used to produce capsules of AA in a glassy high DE maltodextrin (DE 10-15) matrix. Barrel temperature, screw speed and feed speed were selected as variables and motor torque (motor torque percent) and die head pressure during extrusion were studied. The AA loading capacity, yield and Tg of the extruded products were also investigated. The results showed that high barrel temperature, high screw speed or low feed speed could make motor torque and die head pressure decrease. The optimum barrel temperature, screw speed and feed speed were middle temperature (85℃-105℃-120℃-105℃),60 rpm and 1.1 kg h-1. Encapsulation of AA in the low water content/solid/glassy-state carbohydrate matrix was developed according on the optimum condition. Maltodextrin (DE 10-15), trehalose and gum arabic were used in the formulation as film forming materials. Glass phase characteristics of AA in the encapsulating matrix were assessed. The method could allow the AA content in final extrudates (payload) of three formulations more than 15.67 g/100 g extrudates while the AA yield were above 97%. The Tg of the extrudates were above 40℃. The incorporation of trehalose and gum arabic reduced the Tg and the expansion ratio of the extrudates, respectively. The results of scanning electron microscopy, X-ray diffraction, and Fourier-transform infrared spectroscopy indicated that the formulated feed materials became a glassy solid solution, where the AA were dispersed in the matrix of carbohydrates. Milled extrudates (20～40 mesh) of three formulations showed a fast dissolution rate, and AA in milled extrudates were completely dissolved within 10 minutes. The rate was controlled by the carbohydrates matrix. The extruded products were applied to the formula milk powder and the AA loss decreased obviously which indicated that the encapsulated AA in the glassy carbohydrates matrix may decrease the reactions between AA and other ingredients in the food system. AA could be well protected.
3. AA was encapsulated in the glassy isomalto-oligosaccharides by extrusion. Two formulations which had 10% and 16% AA content were prepared. The measuring feeder was set to obtain a flow rate of 1 kg h-1 of premixed material and screw speed was maintained at 60 rpm for all the experimental runs. Three barrel temperatures were studied. The parameters such as torque and die head pressure during extrusion were investigated. X-ray diffraction and differential scanning calorimeter were used to investigate the characteristics of products. The AA yield, loading capacity and moisture content of the products were also measured. The results showed that high barrel temperature could make motor torque and die head pressure decrease. At middle and low barrel temperature, torque decreased with increased AA. AA could be encapsulated successfully. The Tg was decreased with increased AA.The result of X-ray diffraction indicated that the formulation was a glassy solid solution. The extrudated products were applied to the formula milk powder and the AA retention rate were improved greatly.
4. Vitamin E (VE) was encapsulated in glassy carbohydrates by extrusion. Four typical formulations were prepared in order to have 5% and 8% VE added to each 20% and 30% modified starch containing feed material, all four formulations contained soya lecithin at 1% level as an emulsifier. The measuring feeder was set to obtain a flow rate of 1.2 kg h-1 of premixed material, the barrel temperatures were set to T1 (65℃), T2 (95℃), T3 (115℃), T4 (105℃) and screw speed was maintained at 60 rpm for all the experimental runs.The parameters such as torque, specific mechanical energy and die head pressure during extrusion were monitored. The physico-chemical properties of glassy extruded products were investigated. The results showed that high VE content and low modified starch could make motor torque, SME and die head pressure decrease. It is very important to use the modified stach with the emulsification properties for encapsulating the oil soluble materials. The VE retention rates were above 93% after extrusion. The VE oil could be dispersed as the small oil droplets throughout the carbohydrate matrix by using the high HLB emulsifier and modified starch. The size and distribution of the VE oil droplets were uniform. There was a slight loss for VE during the storage, while the VE retention rate of encapsulated VE was much higher than unencapsulated VE significantly. The VE could be encapsulated successfully. The Tg of the extrudates were above 30℃and Tg could be a good predictor of caking properties at elevated temperatures.
本论文研究了利用挤压法制备水溶性维生素(AA为代表)的糖玻璃化胶囊的方法,同时也对油溶性维生素(维生素E为代表)的挤压糖玻璃化技术进行了研究。以便建立既可用于包埋水溶性功能因子又能包埋油溶性功能因子的挤压糖玻璃化共性包埋技术。系统研究了挤压糖玻璃化胶囊的制备工艺和配方的选择并对产品性质进行了深入的分析。
主要研究内容如下：
1.以低DE值的麦芽糊精作为基质,利用挤压法将AA包埋于玻璃化基质中。主要研究了配方参数如芯壁比和水分添加量(增塑剂)对挤压产品玻璃化转变温度(Tg)的影响。对不同配方产品中AA的产率、含量和水分含量以及挤压参数进行了测定和比较。结果如下：水分含量和芯壁比对产品Tg影响较大,水分含量从7.860%提高到10.430%时,挤压产品的Tg值从43.17℃降低到27.48℃；芯壁比从1：4变化到1：8时,Tg值从35.79-C上升到41.46℃。挤压产品的AA产率高于96%,随着产品中水分含量的增加,AA产率略有下降。提高水分添加量和芯壁比可以减少挤压的特定机械能和模头压力。通过X-射线衍射分析,AA可能以分子分散的形式分散于麦芽糊精基质中。
2.以高DE值的麦芽糊精作为基质,采用挤压法制备糖玻璃化AA胶囊。考察了挤压腔温度、螺杆转速和喂料速度对挤压过程中电机扭拒(扭矩百分比)、模头压力的影响。分析了挤压产品的AA含量、产率和挤压产品Tg等理化指标。结果表明：提高挤压腔温度、增加螺杆转速和降低喂料速度可以减小电机扭矩及模头压力。确定的挤压腔温度、螺杆转速和进料速度分别为中温(85℃—105℃—120℃—105℃)、60 rpm和1.1 kg/h。在优化的挤压工艺基础上,以高DE值的麦芽糊精作为主要基质,在配方中添加阿拉伯胶和海藻糖,采用优化后的挤压工艺将AA包埋于低水分含量／固态／玻璃态的混合碳水化合物基质中。对产品的理化指标进行了分析,得到挤压产品中AA载量高于15.67g/100g的挤压产品,AA的产率大于97%,产品的Tg高于40℃。添加海藻糖会使产品的Tg降低,而添加阿拉伯胶可减小产品的膨胀率。扫描电子显微镜、X-射线衍射和傅里叶变换红外光谱分析表明AA分散于碳水化合物基质中形成了玻璃态的固溶体。20-40目挤压产品的溶解实验表明其具有较快的溶解速率,其中的AA可以在10min内完全溶解释放,且溶解速率由碳水化合物基质控制。将挤压产品应用于配方奶粉中,AA的损失明显减小,表明将AA包埋于糖玻璃化基质中可以降低AA与食品体系中其他成分的反应,从而更好的保护AA。
3.采用挤压法制备了低聚异麦芽糖为基质的AA无糖玻璃化胶囊。选择了10%和16%两种AA含量的配方,在螺杆转速60 rpm,喂料速度1 kg/h的条件下,研究了三种挤压腔温度时的挤压工艺。探讨了挤压过程中电机扭拒、模头压力等的变化规律。采用差式扫描量热法、X-射线衍射对产品性质进行了表征。对挤压产品中AA的产率和载量等理化指标进行了分析。结果表明：提高挤压腔温度可以减小电机扭矩和模头压力,AA含量对三种温度条件下的电机扭矩影响较小。当挤压腔为中温和低温时,AA含量的增加可以使模头压力减小。两种含量下的AA均得到了很好的包埋,挤压产物的Tg随着AA含量增加而降低。X-射线分析表明AA以分子形式分散于基质中,形成了固溶体。将挤压产品应用于配方奶粉中,AA的保留率得到较大提高。
4.利用挤压法将维生素E(VE)包埋于碳水化合物基质中。选择了四种典型的配方,其中配方中分别含有5%和8%的VE,配方中添加了20%和30%的变性淀粉于麦芽糊精中作为基质。四种配方中都添加1%的大豆卵磷脂作为乳化剂。挤压中喂料速度设定为1.2 kg/h,挤压腔的温度设定分别为T1(65℃),T2(950C),T3(115℃)和T4(105℃),螺杆转速保持60 rpm。对挤压过程中电机扭矩、特定机械能和模头压力等指标进行了测定和分析,对挤压产品的理化性质进行了研究。结果表明：提高VE含量或者减少变性淀粉含量可以使得电机扭矩、特定机械能和模头压力减小。使用具有乳化作用的变性淀粉对于油溶性物质的包埋具有重要作用。挤压后VE的保留率高于93%。变性淀粉和高HLB值乳化剂的使用使VE以小液滴形态分散于基质中,并且液滴大小和分布比较均匀。在贮藏期间,VE略有损失,但保留率显著高于未包埋的VE,VE得到了很好的包埋。得到的挤压产品的Tg高于30℃,并且Tg可以作为温度提高时产品结块性的良好预测指标。
L-Ascorbic acid (AA) commonly known as Vitamin C is a physiologically and biochemically essential water soluble bioactive compound required for the normal regulatory functions. AA has been extensively used in variety of food formulations and acts as an antioxidant agent besides its nutritional role in the human body. It is established that AA helps in the absorption of inorganic Fe and inhibits the formulation of carcinogenic compounds in the body. It also acts as co-factor for enzymes, involves in the biosynthesis of carnitine, stimulates collagen synthesis, modulates neurotransmitter systems and offers improved immunity against diseases. Its possible role in minimizing the risk of serious diseases such as heart diseases and cancer is very interesting. With the improved knowledge of functional properties of this vital food ingredient, the trend to incorporate it into different food systems is increasing. Due to the highly unstable nature, AA is prone to be degradation and also destabilize the whole food system. Therefore, it is important to stabilize AA prior to its application.
The technique of the encapsulation of vitamins (AA and vitamin E) in glassy carbohydrates employing extrusion was investigated. The processes and formulations of the technique were studied. And the characteristics of the extrudated products were analysised. Major contents of this paper are as following:
1. AA was encapsulated in glassy low dextrose equivalent (DE) maltodextrin (DE 8-10) matrix by extrusion. The effects of formulation parameters i.e., core-matrix ratio and moisture content were mainly investigated on glass transition temperature (Tg) of extrudates. The AA yield, AA content and moisture of the products together with extrusion parameters were also measured and compared for different formulations. Both the water content and AA content have a great effect on Tg. The Tg of extrudates containing water content from 7.860% to 10.430% decreased from 43.17℃to 27.48℃and The Tg of extrudates which core to matrix from 1:4 to 1:8 increased from 35.79℃to 41.64℃. AA yield of all samples is above 96% and with increasing water content there was a small decrease in the AA yield. The increased water level and core-matrix ratio reduce specific mechanical energy and die head pressure. From X-ray diffraction result, AA was most likely molecularly dispersed within the maltodextrin matrix.
2. Extrusion was used to produce capsules of AA in a glassy high DE maltodextrin (DE 10-15) matrix. Barrel temperature, screw speed and feed speed were selected as variables and motor torque (motor torque percent) and die head pressure during extrusion were studied. The AA loading capacity, yield and Tg of the extruded products were also investigated. The results showed that high barrel temperature, high screw speed or low feed speed could make motor torque and die head pressure decrease. The optimum barrel temperature, screw speed and feed speed were middle temperature (85℃-105℃-120℃-105℃),60 rpm and 1.1 kg h-1. Encapsulation of AA in the low water content/solid/glassy-state carbohydrate matrix was developed according on the optimum condition. Maltodextrin (DE 10-15), trehalose and gum arabic were used in the formulation as film forming materials. Glass phase characteristics of AA in the encapsulating matrix were assessed. The method could allow the AA content in final extrudates (payload) of three formulations more than 15.67 g/100 g extrudates while the AA yield were above 97%. The Tg of the extrudates were above 40℃. The incorporation of trehalose and gum arabic reduced the Tg and the expansion ratio of the extrudates, respectively. The results of scanning electron microscopy, X-ray diffraction, and Fourier-transform infrared spectroscopy indicated that the formulated feed materials became a glassy solid solution, where the AA were dispersed in the matrix of carbohydrates. Milled extrudates (20～40 mesh) of three formulations showed a fast dissolution rate, and AA in milled extrudates were completely dissolved within 10 minutes. The rate was controlled by the carbohydrates matrix. The extruded products were applied to the formula milk powder and the AA loss decreased obviously which indicated that the encapsulated AA in the glassy carbohydrates matrix may decrease the reactions between AA and other ingredients in the food system. AA could be well protected.
3. AA was encapsulated in the glassy isomalto-oligosaccharides by extrusion. Two formulations which had 10% and 16% AA content were prepared. The measuring feeder was set to obtain a flow rate of 1 kg h-1 of premixed material and screw speed was maintained at 60 rpm for all the experimental runs. Three barrel temperatures were studied. The parameters such as torque and die head pressure during extrusion were investigated. X-ray diffraction and differential scanning calorimeter were used to investigate the characteristics of products. The AA yield, loading capacity and moisture content of the products were also measured. The results showed that high barrel temperature could make motor torque and die head pressure decrease. At middle and low barrel temperature, torque decreased with increased AA. AA could be encapsulated successfully. The Tg was decreased with increased AA.The result of X-ray diffraction indicated that the formulation was a glassy solid solution. The extrudated products were applied to the formula milk powder and the AA retention rate were improved greatly.
4. Vitamin E (VE) was encapsulated in glassy carbohydrates by extrusion. Four typical formulations were prepared in order to have 5% and 8% VE added to each 20% and 30% modified starch containing feed material, all four formulations contained soya lecithin at 1% level as an emulsifier. The measuring feeder was set to obtain a flow rate of 1.2 kg h-1 of premixed material, the barrel temperatures were set to T1 (65℃), T2 (95℃), T3 (115℃), T4 (105℃) and screw speed was maintained at 60 rpm for all the experimental runs.The parameters such as torque, specific mechanical energy and die head pressure during extrusion were monitored. The physico-chemical properties of glassy extruded products were investigated. The results showed that high VE content and low modified starch could make motor torque, SME and die head pressure decrease. It is very important to use the modified stach with the emulsification properties for encapsulating the oil soluble materials. The VE retention rates were above 93% after extrusion. The VE oil could be dispersed as the small oil droplets throughout the carbohydrate matrix by using the high HLB emulsifier and modified starch. The size and distribution of the VE oil droplets were uniform. There was a slight loss for VE during the storage, while the VE retention rate of encapsulated VE was much higher than unencapsulated VE significantly. The VE could be encapsulated successfully. The Tg of the extrudates were above 30℃and Tg could be a good predictor of caking properties at elevated temperatures.
引文
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