稻米淀粉物性研究
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摘要
在商业淀粉中,发现稻米淀粉具有特殊的应用,这是由于稻米淀粉是谷物中颗粒最小的淀粉以及稻米淀粉中剩余的蛋白的低过敏性,进而在世界范围内形成了对稻米淀粉进行有效开发利用的研究热点,因而为了开发出附加值较高的稻米淀粉产品,就需要对稻米淀粉的物性进行系统研究。本研究首先利用碱法、表面活性剂(SDS)、碱性蛋白酶和中性蛋白酶与超声波结合去除米粉中的蛋白质,获得较纯的稻米淀粉;随后研究了直链淀粉含量不同的稻米样品之间的黏滞性差别,以及稻米淀粉黏滞性和质构性的相关性;蛋白质作为稻米中的第二大成分,测定其对稻米淀粉黏滞性的影响;研究稻米淀粉中直链淀粉与脂肪酸形成的复合物对稻米淀粉复合指数、水溶性、碘吸收和流变性的影响;用DSC分析了米粉和稻米淀粉在热力学上的差异;碱在食品中是一个很重要的添加剂,测定了其对稻米淀粉黏滞性的影响,以及单糖和双糖对稻米淀粉黏滞性的影响;最后建立了用近红外透射光谱测定稻米淀粉RVA特征值的定标模型。主要结论如下:
(1)用四种方法分别去除稻米中的蛋白质,结果表明,碱法能很好的去除稻米中的蛋白质,所得稻米淀粉中蛋白质含量最低,不过在清洗过程中要消耗大量的水;SDS也能去除稻米中一定量的蛋白质,但是所得稻米淀粉中剩余蛋白质含量较高,不能达到商业淀粉的要求;碱性蛋白酶酶解蛋白质达到降低蛋白质含量的目的,但是在酶解的过程中,酶解时间较长;中性蛋白酶与超声波结合去除稻米中的蛋白质,所得淀粉中蛋白质含量基本能达到应用要求,并且破损淀粉少。
(2)用快速粘度仪测定不同直链淀粉含量(AC)的稻米淀粉的黏滞谱,结果显示根据RVA谱的主要特征值消减值和崩解值,可以区分出稻米样品的的AC高低,就是AC相仿的品种之间的粘滞特性的差异也可区分开,并且这种差异与稻米食用品质有密切的关系,因而可根据RVA谱黏滞特性判断稻米样品食用品质的优劣。按测定稻米淀粉黏滞谱的过程制作稻米淀粉凝胶,用质构仪测定淀粉凝胶的质构性,相关性分析表明稻米淀粉中直链淀粉含量与黏滞性和质构性指标之间的相关性均达到极显著水平。淀粉凝胶的硬度和粘性的下降和上升趋势与RVA谱中的崩解值和消减值的变化趋势相似,消减值越大,凝胶就越硬,粘性就越小。
(3)选择六个稻米样品用RVA测定了稻米中蛋白质对稻米淀粉黏滞谱特征值的影响。结果显示糙米和精米在去除蛋白质前后黏滞谱的差别基本是一致的,蛋白质去除后稻米淀粉黏滞谱下降;用还原剂二硫苏糖醇打破蛋白质中的二硫键,测定其对精米及储藏精米淀粉黏滞性的影响,结果显示精米的谱线总体是下降的,而储藏样品中低直链淀粉含量的两个样品的谱线是下降,高直链淀粉含量的两个样品谱线是上升的。用丙醇优化能很好的提取出稻米中的醇溶蛋白,测定其对淀粉黏滞性和质构性的影响,醇溶蛋白能使RVA特征值中的峰值粘度、最终粘度和消减值降低,崩解值升高,能使硬度、粘性、粘附性降低。另外还选择两个稻米样品研究施氮量对稻米淀粉黏滞性的影响,随着施氮量的增加稻米中蛋白质含量增加,而稻米淀粉的RVA谱线下降越低,在糙米和精米中结果表现一致。
(4)选择四种饱和脂肪酸添加到稻米淀粉中,测定四种饱和脂肪酸对淀粉糊化性质的影响。结果显示,随着脂肪酸量的增加复合指数增加,并且月桂酸使复合指数增加的最多;直链淀粉-脂肪酸复合物使碘光谱最大吸收值下降,相比月桂酸使碘光谱最大吸收值下降的最多;由于月桂酸与直链淀粉形成复合物的能力强,使吸收比率下降的也最显著。
选择两个稻米样品在淀粉悬浊液中加入月桂酸和棕榈酸,测定脂肪酸对稻米淀粉流变性的影响。结果显示,两种脂肪酸与直链淀粉结合限制了稻米淀粉颗粒的膨胀,使得淀粉TG′增加,淀粉峰值G′降低,月桂酸使两个样品淀粉的峰值G′下降比较大;淀粉凝胶在4℃下冷藏,两个稻米淀粉凝胶脱水随着冷藏时间的延长而增加,添加脂肪酸,淀粉脱水增加,并且月桂酸使两种淀粉糊脱水比棕榈酸增加。(5)用DSC测定了六个直链淀粉含量不同的稻米样品的米粉和淀粉在热力学上的差异,以及水与米粉和淀粉按不同比例混合后,稻米淀粉热力学性质的差别。结果显示,随着六个样品中直链淀粉含量的增加,米粉和淀粉的起始温度和凝胶温度增加,热焓降低。米粉和淀粉的热焓都随着水分含量增加而增加,在不同水分含量下淀粉的热焓总体比米粉的热焓高,二者都表现出糯米的热焓高于其它非蜡质淀粉,并且在米粉中糯米比其它样品热焓达到恒定值要早;同样米粉和淀粉的起始温度随水分含量的增加而增加,凝胶温度随着水分含量的增加而降低。
(6)选择六个直链淀粉含量不同的稻米淀粉样品,测定分别在稻米淀粉中加入1.00% Na2CO3和NaOH,比较二者对淀粉RVA谱的影响,以及加入不同量的Na2CO3对稻米淀粉的影响;在稻米淀粉中加入单糖和双糖对稻米淀粉黏滞谱的影响,以及阴离子使稻米淀粉糊化的温度和浓度。结果显示,与原淀粉相比加入Na2CO3和NaOH后淀粉黏滞谱线显著下降,并且NaOH使谱线的下降更大,都达到了显著水平;在六个稻米样品淀粉中添加不同浓度的Na2CO3,结果显示随着Na2CO3浓度的增加,也就是随着pH值的增加,黏滞谱线逐渐下降。在Na2CO3达到一定浓度后,pH值的增加缓慢,在对RVA特征值影响上也趋于稳定,对六个样品的影响基本是一致的;选择的单糖和双糖添加到淀粉中,都使淀粉的特征值有所下降;阴离子使稻米淀粉糊化的规律是:根据阴离子碱性的强弱而显示出使稻米淀粉糊化的快慢,使淀粉糊化的顺序是:OH—>HOC6H4COO—>SCN—>I—>Br—>CL—>SO62—。
(7)收集164份稻米样品建立了精米直链淀粉含量、胶稠度和淀粉黏滞谱特征值的近红外透射光谱定标模型。结果显示直链淀粉含量数学模型在测定精米直链淀粉含量是可行的;胶稠度近红外定标模型能达到间接测定胶稠度的要求;所建立的稻米淀粉黏滞谱特征值定标模型都能达到测定精米淀粉峰值粘度、热浆粘度、崩解值、消减值、最终粘度和回复值的要求。这为稻米品质测定提供了一个快速无损的检测技术。
Among commercial starches, rice starch finds special application because it has a small granule size and its residual protein is non-allergenic,so exploitation and utilization of rice starch have become the hot topic in the world.In order to exploit rice starch production with high value, there is a great urgency to study the physical property of rice starch. Firstly rice starch is isolated by alkalin steeping, alkaline protease, sodium dodecyl sulfate,combination of neutral protease and high-intensity ultrasound, respectively. Viscosity of rice samples with different amylose contents were studied, and correlation between cooked rice texture and rapid visco analyzer were measured. Protein is second composition of rice . The influence of protein on rice starch viscosity were analyzed. The study was undertaken to examine the of cooking of rice starch in the presence of lauric, palmitic, myristic and stearic acid on complexing index,iodine spectra,solubility,pasting and rheological properties.Differential scanning calorimetry(DSC) was used to evaluate phase transitions of rice flour and starch. Alkali is an important additive in the food. The objectives were to observe the effects of sodium carbonate and sodium hydroxide on the viscosity of rice starch. And the effect of single sugar and double sugar on rice starch viscosity were determined. The calibration model of RVA viscosity properties of rice were established by near Infrared transmission spectrum.
The following results were obtained.
(1)The protein of rice flour was isolated by four methods. The results showed that alkalin steeping was the best to remove protein.But a lot of water was consumed in the rinse. SDS was able to remove some proteins.But protein contents was high in acquired rice starch.Alkaline protease can be used to recover rice starch from wet-milled rice flour.But Time was too long in alkaline protease assimilation. Combination of neutral protease and high-intensity ultrasound for isolation of rice starch was applied, and acquired rice starch can accord the request of commercial starch. The contents of damaged starch was low.
(2)The viscosity profile of rice starch with different amylose contents were measured by RVA. The results showed that rice samples with different amylose contents were able to be differentiated according to setback and breakdown. Similar samples with amylose contents were also able to be differentiated.And this discrepancy is correlation with eating quality of rice. So the excellent and inferior of eating quality of rice samples can be differentiated according to RVA. Textural properties of rice flour gels formed after RVA analyses were determined with a textural analyser.Correlation between amylose contents and RVA index and textural index were significantly different. The change of hardness and adhesiveness of rice flour gels were conform with setback and breakdown of RVA. Gels will be rigid and adhesiveness will small when setback is big.
(3)The aim of this study is to determine how protein affect the viscosity curve of rice starch.The results showed that the change of brown rice and milled rice was the same with viscosity curves when proteins are removed.In order to determine the effect of disulphide bonding on viscosity of flour from the varieties,Dithiothreitol(DTT) was added to the flour.The addition of DTT to the RVA test aims to disrupt the disulphide bridges and keep them reduced.DTT lowers the curve and has similar effects with protease. In four storage samples, the curve of two samples with low amylose contents drop and the curve of two samples with high amylose contents ascend.100% propanol was the most efficient solvent for the extraction of prolamin from rice flour.Addition of prolamin to rice starch was found to cause a decrease in peak viscosity,final viscosity, setback viscosity but increase in breakdown and decrease in hardness,adhesiveness and gumminess of the starch gel. The higher the rate of N, the higher the protein content,the lower the overall curve,brown rice and milled rice are the same.
(4)The influence were examined about cooking of rice starch in the presence of lauric, palmitic,myristic and stearic acid.The results showed that the complexing index progressively increased with the increase in levels of fatty acids and cooking duration. However, the increase was more pronounced with the addition of lauric acid.Theλmax values of cooked rice starch pastes decreased with the increase in levels of all fatty acids and cooking duration. The 630/520 nm ratio of rice starch paste decreased with increase in the levels of fatty acids and cooking duration. Water-solubility decreased with the increase in level of fatty acids. The decrease was more pronounced with the addition of lauric acid inλmax values, 630/520 nm ratio and water-solubility.
The addition of both the fatty acids inhibited the swelling of the rice starch granules and consequently, increased the TG′.Addition of both fatty acids decreased the peak G′, while the addition of lauric acid resulted in a more decrease in peak G′in both the starches.The synersis in cooked rice starch paste increased with increase in storage duration and increased with addition of both the fatty acids.
(5)DSC was used to evaluate phase transitions of six rice flours and rice starches with different amylose contents in systems with different water content. The To and TG for flours and starches in the presence of excess of water increased with the increase of amylose contents. The total gelatinization enthalpy was found to be low. The△HG increased with the increase of water content in systems. The△HG was found to be higher in starches than in flours. Both△HG were higher in waxy genotypes than in non-waxy genotypes. The To of flours and starches increased with the increase of water content, while TG decreased with the increase of water content.
(6)This study is to determine how the alkalin,sugar and anion affect the viscosity curve of rice starch.The results showed that the addition of Na2CO3 and NaOH resulted in significant decrease in the curve.The viscosity curve of rice starches decreased with the increase of Na2CO3.The addition of signal sugar and double sugar made the viscosity curve drop.The law that anion made rice starch paste was that the stronger alkali property of anions were the easier rice starch to become paste. The order that anion made starch paste is OH—>HOC6H4COO—>SCN—>I—>Br—>CL—>SO62—.
(7)One hundred and sixty-four samples of small amount of milled rice were scanned by Foss Tecator Infratec 1255, and their amylose contents , gel consistency and RVA viscosity value were determined by chemistry method. With the WINISI calibration maker software, several mathematics treatments to the sample spectra and several different regression methods were adopted to optimize a good calibration equation for determination of amylose content, gel consistency and RVA viscosity value in milled rice.
(1)用四种方法分别去除稻米中的蛋白质,结果表明,碱法能很好的去除稻米中的蛋白质,所得稻米淀粉中蛋白质含量最低,不过在清洗过程中要消耗大量的水;SDS也能去除稻米中一定量的蛋白质,但是所得稻米淀粉中剩余蛋白质含量较高,不能达到商业淀粉的要求;碱性蛋白酶酶解蛋白质达到降低蛋白质含量的目的,但是在酶解的过程中,酶解时间较长;中性蛋白酶与超声波结合去除稻米中的蛋白质,所得淀粉中蛋白质含量基本能达到应用要求,并且破损淀粉少。
(2)用快速粘度仪测定不同直链淀粉含量(AC)的稻米淀粉的黏滞谱,结果显示根据RVA谱的主要特征值消减值和崩解值,可以区分出稻米样品的的AC高低,就是AC相仿的品种之间的粘滞特性的差异也可区分开,并且这种差异与稻米食用品质有密切的关系,因而可根据RVA谱黏滞特性判断稻米样品食用品质的优劣。按测定稻米淀粉黏滞谱的过程制作稻米淀粉凝胶,用质构仪测定淀粉凝胶的质构性,相关性分析表明稻米淀粉中直链淀粉含量与黏滞性和质构性指标之间的相关性均达到极显著水平。淀粉凝胶的硬度和粘性的下降和上升趋势与RVA谱中的崩解值和消减值的变化趋势相似,消减值越大,凝胶就越硬,粘性就越小。
(3)选择六个稻米样品用RVA测定了稻米中蛋白质对稻米淀粉黏滞谱特征值的影响。结果显示糙米和精米在去除蛋白质前后黏滞谱的差别基本是一致的,蛋白质去除后稻米淀粉黏滞谱下降;用还原剂二硫苏糖醇打破蛋白质中的二硫键,测定其对精米及储藏精米淀粉黏滞性的影响,结果显示精米的谱线总体是下降的,而储藏样品中低直链淀粉含量的两个样品的谱线是下降,高直链淀粉含量的两个样品谱线是上升的。用丙醇优化能很好的提取出稻米中的醇溶蛋白,测定其对淀粉黏滞性和质构性的影响,醇溶蛋白能使RVA特征值中的峰值粘度、最终粘度和消减值降低,崩解值升高,能使硬度、粘性、粘附性降低。另外还选择两个稻米样品研究施氮量对稻米淀粉黏滞性的影响,随着施氮量的增加稻米中蛋白质含量增加,而稻米淀粉的RVA谱线下降越低,在糙米和精米中结果表现一致。
(4)选择四种饱和脂肪酸添加到稻米淀粉中,测定四种饱和脂肪酸对淀粉糊化性质的影响。结果显示,随着脂肪酸量的增加复合指数增加,并且月桂酸使复合指数增加的最多;直链淀粉-脂肪酸复合物使碘光谱最大吸收值下降,相比月桂酸使碘光谱最大吸收值下降的最多;由于月桂酸与直链淀粉形成复合物的能力强,使吸收比率下降的也最显著。
选择两个稻米样品在淀粉悬浊液中加入月桂酸和棕榈酸,测定脂肪酸对稻米淀粉流变性的影响。结果显示,两种脂肪酸与直链淀粉结合限制了稻米淀粉颗粒的膨胀,使得淀粉TG′增加,淀粉峰值G′降低,月桂酸使两个样品淀粉的峰值G′下降比较大;淀粉凝胶在4℃下冷藏,两个稻米淀粉凝胶脱水随着冷藏时间的延长而增加,添加脂肪酸,淀粉脱水增加,并且月桂酸使两种淀粉糊脱水比棕榈酸增加。(5)用DSC测定了六个直链淀粉含量不同的稻米样品的米粉和淀粉在热力学上的差异,以及水与米粉和淀粉按不同比例混合后,稻米淀粉热力学性质的差别。结果显示,随着六个样品中直链淀粉含量的增加,米粉和淀粉的起始温度和凝胶温度增加,热焓降低。米粉和淀粉的热焓都随着水分含量增加而增加,在不同水分含量下淀粉的热焓总体比米粉的热焓高,二者都表现出糯米的热焓高于其它非蜡质淀粉,并且在米粉中糯米比其它样品热焓达到恒定值要早;同样米粉和淀粉的起始温度随水分含量的增加而增加,凝胶温度随着水分含量的增加而降低。
(6)选择六个直链淀粉含量不同的稻米淀粉样品,测定分别在稻米淀粉中加入1.00% Na2CO3和NaOH,比较二者对淀粉RVA谱的影响,以及加入不同量的Na2CO3对稻米淀粉的影响;在稻米淀粉中加入单糖和双糖对稻米淀粉黏滞谱的影响,以及阴离子使稻米淀粉糊化的温度和浓度。结果显示,与原淀粉相比加入Na2CO3和NaOH后淀粉黏滞谱线显著下降,并且NaOH使谱线的下降更大,都达到了显著水平;在六个稻米样品淀粉中添加不同浓度的Na2CO3,结果显示随着Na2CO3浓度的增加,也就是随着pH值的增加,黏滞谱线逐渐下降。在Na2CO3达到一定浓度后,pH值的增加缓慢,在对RVA特征值影响上也趋于稳定,对六个样品的影响基本是一致的;选择的单糖和双糖添加到淀粉中,都使淀粉的特征值有所下降;阴离子使稻米淀粉糊化的规律是:根据阴离子碱性的强弱而显示出使稻米淀粉糊化的快慢,使淀粉糊化的顺序是:OH—>HOC6H4COO—>SCN—>I—>Br—>CL—>SO62—。
(7)收集164份稻米样品建立了精米直链淀粉含量、胶稠度和淀粉黏滞谱特征值的近红外透射光谱定标模型。结果显示直链淀粉含量数学模型在测定精米直链淀粉含量是可行的;胶稠度近红外定标模型能达到间接测定胶稠度的要求;所建立的稻米淀粉黏滞谱特征值定标模型都能达到测定精米淀粉峰值粘度、热浆粘度、崩解值、消减值、最终粘度和回复值的要求。这为稻米品质测定提供了一个快速无损的检测技术。
Among commercial starches, rice starch finds special application because it has a small granule size and its residual protein is non-allergenic,so exploitation and utilization of rice starch have become the hot topic in the world.In order to exploit rice starch production with high value, there is a great urgency to study the physical property of rice starch. Firstly rice starch is isolated by alkalin steeping, alkaline protease, sodium dodecyl sulfate,combination of neutral protease and high-intensity ultrasound, respectively. Viscosity of rice samples with different amylose contents were studied, and correlation between cooked rice texture and rapid visco analyzer were measured. Protein is second composition of rice . The influence of protein on rice starch viscosity were analyzed. The study was undertaken to examine the of cooking of rice starch in the presence of lauric, palmitic, myristic and stearic acid on complexing index,iodine spectra,solubility,pasting and rheological properties.Differential scanning calorimetry(DSC) was used to evaluate phase transitions of rice flour and starch. Alkali is an important additive in the food. The objectives were to observe the effects of sodium carbonate and sodium hydroxide on the viscosity of rice starch. And the effect of single sugar and double sugar on rice starch viscosity were determined. The calibration model of RVA viscosity properties of rice were established by near Infrared transmission spectrum.
The following results were obtained.
(1)The protein of rice flour was isolated by four methods. The results showed that alkalin steeping was the best to remove protein.But a lot of water was consumed in the rinse. SDS was able to remove some proteins.But protein contents was high in acquired rice starch.Alkaline protease can be used to recover rice starch from wet-milled rice flour.But Time was too long in alkaline protease assimilation. Combination of neutral protease and high-intensity ultrasound for isolation of rice starch was applied, and acquired rice starch can accord the request of commercial starch. The contents of damaged starch was low.
(2)The viscosity profile of rice starch with different amylose contents were measured by RVA. The results showed that rice samples with different amylose contents were able to be differentiated according to setback and breakdown. Similar samples with amylose contents were also able to be differentiated.And this discrepancy is correlation with eating quality of rice. So the excellent and inferior of eating quality of rice samples can be differentiated according to RVA. Textural properties of rice flour gels formed after RVA analyses were determined with a textural analyser.Correlation between amylose contents and RVA index and textural index were significantly different. The change of hardness and adhesiveness of rice flour gels were conform with setback and breakdown of RVA. Gels will be rigid and adhesiveness will small when setback is big.
(3)The aim of this study is to determine how protein affect the viscosity curve of rice starch.The results showed that the change of brown rice and milled rice was the same with viscosity curves when proteins are removed.In order to determine the effect of disulphide bonding on viscosity of flour from the varieties,Dithiothreitol(DTT) was added to the flour.The addition of DTT to the RVA test aims to disrupt the disulphide bridges and keep them reduced.DTT lowers the curve and has similar effects with protease. In four storage samples, the curve of two samples with low amylose contents drop and the curve of two samples with high amylose contents ascend.100% propanol was the most efficient solvent for the extraction of prolamin from rice flour.Addition of prolamin to rice starch was found to cause a decrease in peak viscosity,final viscosity, setback viscosity but increase in breakdown and decrease in hardness,adhesiveness and gumminess of the starch gel. The higher the rate of N, the higher the protein content,the lower the overall curve,brown rice and milled rice are the same.
(4)The influence were examined about cooking of rice starch in the presence of lauric, palmitic,myristic and stearic acid.The results showed that the complexing index progressively increased with the increase in levels of fatty acids and cooking duration. However, the increase was more pronounced with the addition of lauric acid.Theλmax values of cooked rice starch pastes decreased with the increase in levels of all fatty acids and cooking duration. The 630/520 nm ratio of rice starch paste decreased with increase in the levels of fatty acids and cooking duration. Water-solubility decreased with the increase in level of fatty acids. The decrease was more pronounced with the addition of lauric acid inλmax values, 630/520 nm ratio and water-solubility.
The addition of both the fatty acids inhibited the swelling of the rice starch granules and consequently, increased the TG′.Addition of both fatty acids decreased the peak G′, while the addition of lauric acid resulted in a more decrease in peak G′in both the starches.The synersis in cooked rice starch paste increased with increase in storage duration and increased with addition of both the fatty acids.
(5)DSC was used to evaluate phase transitions of six rice flours and rice starches with different amylose contents in systems with different water content. The To and TG for flours and starches in the presence of excess of water increased with the increase of amylose contents. The total gelatinization enthalpy was found to be low. The△HG increased with the increase of water content in systems. The△HG was found to be higher in starches than in flours. Both△HG were higher in waxy genotypes than in non-waxy genotypes. The To of flours and starches increased with the increase of water content, while TG decreased with the increase of water content.
(6)This study is to determine how the alkalin,sugar and anion affect the viscosity curve of rice starch.The results showed that the addition of Na2CO3 and NaOH resulted in significant decrease in the curve.The viscosity curve of rice starches decreased with the increase of Na2CO3.The addition of signal sugar and double sugar made the viscosity curve drop.The law that anion made rice starch paste was that the stronger alkali property of anions were the easier rice starch to become paste. The order that anion made starch paste is OH—>HOC6H4COO—>SCN—>I—>Br—>CL—>SO62—.
(7)One hundred and sixty-four samples of small amount of milled rice were scanned by Foss Tecator Infratec 1255, and their amylose contents , gel consistency and RVA viscosity value were determined by chemistry method. With the WINISI calibration maker software, several mathematics treatments to the sample spectra and several different regression methods were adopted to optimize a good calibration equation for determination of amylose content, gel consistency and RVA viscosity value in milled rice.
引文
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