蕨根淀粉理化性质及抗性淀粉制备工艺的研究
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摘要
蕨根中含淀粉20%～35%,是蕨根的主要组成物质。研究证明蕨根淀粉制品具有强身、健体、防癌、抗癌之功效,因此,开发前景十分广阔。本文以蕨根淀粉为原料,系统地研究了蕨根淀粉的基本理化性质和分子结构,并得出了压热法制备蕨根抗性淀粉的最佳工艺。主要结论如下:
1.蕨根淀粉理化性质的研究
运用扫描电镜、X-射线衍射仪、分光光度计、Brabender粘度计、差示扫描量热仪等仪器,对蕨根淀粉的颗粒形态、晶体类型、老化特性、流变学特性、糊化特性等进行了研究,并以玉米淀粉和马铃薯淀粉作对照。
蕨根淀粉水分含量较低,灰分、蛋白质和粗脂肪含量均介于玉米淀粉和马铃薯淀粉之间,其组成成分为水分10.29%±0.17%、灰分0.31%±0.03%、蛋白质0.09%±0.01%、粗脂肪0.22%±0.02%。蕨根淀粉颗粒多数为卵圆形,部分为圆形和多边形,表面光滑无裂纹,平均粒径为14μm,粒径分布在7～28μm。蕨根淀粉颗粒的偏光十字接近于中心位置,且比较明显,多数呈十字型,部分呈“X”型,晶体结构属C型。
蕨根淀粉糊的持水性和冻融稳定性较马铃薯淀粉差,但优于玉米淀粉,溶解度介于玉米淀粉和马铃薯淀粉之间。透光率为13.3%,较玉米淀粉和马铃薯淀粉差。蕨根淀粉糊放置7小时后澄清液体积百分比小,淀粉糊的凝沉性较弱。蕨根淀粉的老化值大于马铃薯淀粉小于玉米淀粉,且老化值受浓度的影响较大。
蕨根淀粉糊的表观粘度随着温度的升高而降低;在一定的剪切力作用下,蕨根淀粉、玉米淀粉和马铃薯淀粉糊的表观粘度均随着剪切时间的增加而下降,表现为假塑性流体,属于剪切稀化体系,蕨根淀粉糊的剪切稀化现象较玉米淀粉和马铃薯淀粉弱。淀粉糊的Brabender粘度曲线表明:蕨根淀粉的峰值粘度明显高于玉米淀粉,略低与马铃薯淀粉,热稳定性和冷稳定性好。DSC图谱分析得出:蕨根淀粉的糊化温度较低,为58.94℃～71.73℃,其热焓值低于玉米淀粉和马铃薯淀粉,为12.86 J/g。
蕨根淀粉凝胶表面脆性一般,不易破裂;内部的硬度不大,弹性很好,粘度大,在受到外力作用后,容易回复原有形状。
2.蕨根淀粉分子结构的研究
蕨根淀粉和玉米淀粉的直链淀粉含量分别为25.38%和20.33%,蕨根淀粉的直链淀粉含量较玉米淀粉高。
碱液分散淀粉时的搅拌速度、直链淀粉从盐溶液中分离出来的速度、纯化时正丁醇和水的用量、离心速度和离心时的温度对直链淀粉和支链淀粉的分离及纯度有影响。
用正丁醇重结晶法重结晶8次和5次可以得到纯度较高的蕨根直链淀粉和支链淀粉;蕨根直链淀粉和支链淀粉的分子量均小于玉米直链淀粉和支链淀粉。
蕨根直链淀粉和支链淀粉与碘络合物的最大吸收波长分别为640nm和547nm;蕨根直链淀粉和支链淀粉的蓝值分别为0.91和0.13,均处于相应的分布范围内,表明纯化后的蕨根直链淀粉和支链淀粉的纯度较高。
3.蕨根抗性淀粉制备工艺的研究
压热法制备蕨根抗性淀粉的过程中,淀粉乳浓度、压热温度、pH值、压热时间和老化时间对蕨根抗性淀粉得率有不同程度的影响。通过三因素二次正交旋转组合设计,得出淀粉乳浓度、pH值、压热时间对蕨根抗性淀粉得率的影响大小次序为:淀粉乳浓度＞pH值＞压热时间。压热法制备蕨根抗性淀粉的最佳工艺条件为:淀粉乳浓度28.7%,pn值7.8,121℃压热处理38min,4℃老化24h,得到的蕨根抗性淀粉得率为10.94%。
在淀粉乳浓度27.05%～28.02%,pH值7.48～8.00,压热时间29.68min～36.27min的优化参数条件下,蕨根抗性淀粉得率达8.5%以上的可能性有95%。
Occupying the proportion of about 35% in fern root, the starch is its main composition. Some researches have shown that fern root starch not only can strengthen our bodies, but also it has the function of preventing and killing cancers. Therefore, there is a vast range of prospects for exploiting fern root starch. With a view to that, the paper makes a systematic investigation of the physicochemical properties and the molecular structure of fern root starch, and deeply illustrates the best technology of making fern root resistant starch through autoclaving. The main results are as follows:
1. Physicochemical properties of fern root starch
Comparing with corn and potato starches, the granule shape, crystal type, retrogradation properties, rheological properties and gelatinization properties of fern root starch were studied by scanning electron microscope, X-ray diffraction, spectral photometer, Brabender viscosimeter and differential scanning calorimetry.
Fern root starch contained little water, and the contents of its ashes, proteins, and fats were between those of com and potato starches. It consisted of 10.29%±0.17% of water, 0.31 %±0.03% of ashes, 0.09%±0.01% of crude protein and 0.22%±0.02% of fat. Most of fern root starch granules were oval, and a few of them were round and polygon in shape, which were smooth and of no cracks. The granules were around 7～28μm in diameter, and their average diameter was 14μm. The granules had a clear malte cross, most of which appeared cross-shaped, but some of which appeared X-shaped in the center. The crystalline pattern of fern root starch was C type.
Comparing with corn and potato starches, fern root starch was less transparent. Its freeze-thaw stability and solubility were between them. Deposited for seven hours, fern root starch paste had little sedimentation. The degree of retrogradation value was greater than that of potato starch, and smaller than that of corn starch. The starch concentration of the paste had great influence on its retrogradation value.
The higher the temperature was, the lower the apparent viscosity of fern root starch paste becomed. Affected by certain shearing force, the apparent viscosity of fern root, corn and potato starch pastes would decrease as the shearing time increases. Appearing a kind of pseudoplastic fluid, they belong to shearing dilution system. Shearing dilution of fern root starch paste was weaker than that of corn and potato starches. The Brabender viscosity analyses of starch pastes indicated that the peak viscosity of fern root starch was obviously higher than that of corn starch, and a little lower than that of potato statch. Moreover, it had the property of good heat and cold paste stability. DSC thermograms of fern root starch showed that the gelatinization temperature, being from 58.94℃to 71.73℃, was slow ,and enthalpy, being 12.86 J/g, was lower than those of potato and corn starches.
Being not easy to break, the surface of fern root starch gelatinization was not very brittle. Its inside was not very hard, but was elastic and of high viscosity. Affected by outside forces, fern root starch gelatinization was easy to return the original form.
2. Molecular structure of fern root starch
Being in the proportion of 25.38 %, the amylose content of fern root was more than that of corn starch, which was in the proportion of 20.33 %.
The fractionation of amylose and amylopection, and their purity were affected by the blending speed of dispering starch in base solution, the velocity of separating amylose from saline solution, centrifugal speed and temperature.
Highly pure amylose and amylopectin can be successfully separated from fern root starch by means of 1-butanol and re-crystallization for 8 times and 5 times. The molecular weights of fern root amylose and amylopectin is smaller than those of corn starch.
Theλ_(max) of starch-iodine complexes of fern root amylose and amylopectin were 640nm and 547nm respectively. Being 0.91 and 0.13 respectively, the blue values were in the corresponding range, which indicated that fern root amylose and amylopectin were of high-purity.
3. Preparation technology of fern root resistant starch
In resistant preparation, the yield of fern root resistant starch was somewhat influenced by starch concentration, autoclaving temperature, pH value, autoclaving time and retrogradation time. The results of three-factor and two-dimensional revolving orthogonal combinatorial design showed that the subsequence of influence was like this: starch concentration>pH values >autoclaving time. The optimum of preparation process for fern root resistant starch was as follows: starch concentration being 28.7%, its pH being 7.8, the starch had been heated for 38minutes at 121℃,then retrograded for 24 hours at 4℃, and the yield was 10.94%.
On the optimized conditions, starch concentration being 27.05 %～28.02%, pH being 7.48～8.00, autoclaving time being 29.68min～36.27min, the possibility reached above 8.5% of the fern root resistant starch's yield was 95 %.
1.蕨根淀粉理化性质的研究
运用扫描电镜、X-射线衍射仪、分光光度计、Brabender粘度计、差示扫描量热仪等仪器,对蕨根淀粉的颗粒形态、晶体类型、老化特性、流变学特性、糊化特性等进行了研究,并以玉米淀粉和马铃薯淀粉作对照。
蕨根淀粉水分含量较低,灰分、蛋白质和粗脂肪含量均介于玉米淀粉和马铃薯淀粉之间,其组成成分为水分10.29%±0.17%、灰分0.31%±0.03%、蛋白质0.09%±0.01%、粗脂肪0.22%±0.02%。蕨根淀粉颗粒多数为卵圆形,部分为圆形和多边形,表面光滑无裂纹,平均粒径为14μm,粒径分布在7～28μm。蕨根淀粉颗粒的偏光十字接近于中心位置,且比较明显,多数呈十字型,部分呈“X”型,晶体结构属C型。
蕨根淀粉糊的持水性和冻融稳定性较马铃薯淀粉差,但优于玉米淀粉,溶解度介于玉米淀粉和马铃薯淀粉之间。透光率为13.3%,较玉米淀粉和马铃薯淀粉差。蕨根淀粉糊放置7小时后澄清液体积百分比小,淀粉糊的凝沉性较弱。蕨根淀粉的老化值大于马铃薯淀粉小于玉米淀粉,且老化值受浓度的影响较大。
蕨根淀粉糊的表观粘度随着温度的升高而降低;在一定的剪切力作用下,蕨根淀粉、玉米淀粉和马铃薯淀粉糊的表观粘度均随着剪切时间的增加而下降,表现为假塑性流体,属于剪切稀化体系,蕨根淀粉糊的剪切稀化现象较玉米淀粉和马铃薯淀粉弱。淀粉糊的Brabender粘度曲线表明:蕨根淀粉的峰值粘度明显高于玉米淀粉,略低与马铃薯淀粉,热稳定性和冷稳定性好。DSC图谱分析得出:蕨根淀粉的糊化温度较低,为58.94℃～71.73℃,其热焓值低于玉米淀粉和马铃薯淀粉,为12.86 J/g。
蕨根淀粉凝胶表面脆性一般,不易破裂;内部的硬度不大,弹性很好,粘度大,在受到外力作用后,容易回复原有形状。
2.蕨根淀粉分子结构的研究
蕨根淀粉和玉米淀粉的直链淀粉含量分别为25.38%和20.33%,蕨根淀粉的直链淀粉含量较玉米淀粉高。
碱液分散淀粉时的搅拌速度、直链淀粉从盐溶液中分离出来的速度、纯化时正丁醇和水的用量、离心速度和离心时的温度对直链淀粉和支链淀粉的分离及纯度有影响。
用正丁醇重结晶法重结晶8次和5次可以得到纯度较高的蕨根直链淀粉和支链淀粉;蕨根直链淀粉和支链淀粉的分子量均小于玉米直链淀粉和支链淀粉。
蕨根直链淀粉和支链淀粉与碘络合物的最大吸收波长分别为640nm和547nm;蕨根直链淀粉和支链淀粉的蓝值分别为0.91和0.13,均处于相应的分布范围内,表明纯化后的蕨根直链淀粉和支链淀粉的纯度较高。
3.蕨根抗性淀粉制备工艺的研究
压热法制备蕨根抗性淀粉的过程中,淀粉乳浓度、压热温度、pH值、压热时间和老化时间对蕨根抗性淀粉得率有不同程度的影响。通过三因素二次正交旋转组合设计,得出淀粉乳浓度、pH值、压热时间对蕨根抗性淀粉得率的影响大小次序为:淀粉乳浓度＞pH值＞压热时间。压热法制备蕨根抗性淀粉的最佳工艺条件为:淀粉乳浓度28.7%,pn值7.8,121℃压热处理38min,4℃老化24h,得到的蕨根抗性淀粉得率为10.94%。
在淀粉乳浓度27.05%～28.02%,pH值7.48～8.00,压热时间29.68min～36.27min的优化参数条件下,蕨根抗性淀粉得率达8.5%以上的可能性有95%。
Occupying the proportion of about 35% in fern root, the starch is its main composition. Some researches have shown that fern root starch not only can strengthen our bodies, but also it has the function of preventing and killing cancers. Therefore, there is a vast range of prospects for exploiting fern root starch. With a view to that, the paper makes a systematic investigation of the physicochemical properties and the molecular structure of fern root starch, and deeply illustrates the best technology of making fern root resistant starch through autoclaving. The main results are as follows:
1. Physicochemical properties of fern root starch
Comparing with corn and potato starches, the granule shape, crystal type, retrogradation properties, rheological properties and gelatinization properties of fern root starch were studied by scanning electron microscope, X-ray diffraction, spectral photometer, Brabender viscosimeter and differential scanning calorimetry.
Fern root starch contained little water, and the contents of its ashes, proteins, and fats were between those of com and potato starches. It consisted of 10.29%±0.17% of water, 0.31 %±0.03% of ashes, 0.09%±0.01% of crude protein and 0.22%±0.02% of fat. Most of fern root starch granules were oval, and a few of them were round and polygon in shape, which were smooth and of no cracks. The granules were around 7～28μm in diameter, and their average diameter was 14μm. The granules had a clear malte cross, most of which appeared cross-shaped, but some of which appeared X-shaped in the center. The crystalline pattern of fern root starch was C type.
Comparing with corn and potato starches, fern root starch was less transparent. Its freeze-thaw stability and solubility were between them. Deposited for seven hours, fern root starch paste had little sedimentation. The degree of retrogradation value was greater than that of potato starch, and smaller than that of corn starch. The starch concentration of the paste had great influence on its retrogradation value.
The higher the temperature was, the lower the apparent viscosity of fern root starch paste becomed. Affected by certain shearing force, the apparent viscosity of fern root, corn and potato starch pastes would decrease as the shearing time increases. Appearing a kind of pseudoplastic fluid, they belong to shearing dilution system. Shearing dilution of fern root starch paste was weaker than that of corn and potato starches. The Brabender viscosity analyses of starch pastes indicated that the peak viscosity of fern root starch was obviously higher than that of corn starch, and a little lower than that of potato statch. Moreover, it had the property of good heat and cold paste stability. DSC thermograms of fern root starch showed that the gelatinization temperature, being from 58.94℃to 71.73℃, was slow ,and enthalpy, being 12.86 J/g, was lower than those of potato and corn starches.
Being not easy to break, the surface of fern root starch gelatinization was not very brittle. Its inside was not very hard, but was elastic and of high viscosity. Affected by outside forces, fern root starch gelatinization was easy to return the original form.
2. Molecular structure of fern root starch
Being in the proportion of 25.38 %, the amylose content of fern root was more than that of corn starch, which was in the proportion of 20.33 %.
The fractionation of amylose and amylopection, and their purity were affected by the blending speed of dispering starch in base solution, the velocity of separating amylose from saline solution, centrifugal speed and temperature.
Highly pure amylose and amylopectin can be successfully separated from fern root starch by means of 1-butanol and re-crystallization for 8 times and 5 times. The molecular weights of fern root amylose and amylopectin is smaller than those of corn starch.
Theλ_(max) of starch-iodine complexes of fern root amylose and amylopectin were 640nm and 547nm respectively. Being 0.91 and 0.13 respectively, the blue values were in the corresponding range, which indicated that fern root amylose and amylopectin were of high-purity.
3. Preparation technology of fern root resistant starch
In resistant preparation, the yield of fern root resistant starch was somewhat influenced by starch concentration, autoclaving temperature, pH value, autoclaving time and retrogradation time. The results of three-factor and two-dimensional revolving orthogonal combinatorial design showed that the subsequence of influence was like this: starch concentration>pH values >autoclaving time. The optimum of preparation process for fern root resistant starch was as follows: starch concentration being 28.7%, its pH being 7.8, the starch had been heated for 38minutes at 121℃,then retrograded for 24 hours at 4℃, and the yield was 10.94%.
On the optimized conditions, starch concentration being 27.05 %～28.02%, pH being 7.48～8.00, autoclaving time being 29.68min～36.27min, the possibility reached above 8.5% of the fern root resistant starch's yield was 95 %.
引文
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