【技术领域】【Technical field】
本发明属于变性淀粉技术领域，具体涉及一种高抗性淀粉含量的交联淀粉及其制备方法。The invention belongs to the technical field of modified starch, and in particular relates to a cross-linked starch with high content of resistant starch and a preparation method thereof.
【背景技术】【Background technique】
抗性淀粉(Resistant Starch，RS)是一种在健康人类的小肠中不能被消化，但能在大肠中发酵或部分发酵的淀粉和淀粉降解产物。抗性淀粉的消化特性赋予其多种重要的生理功能，据研究表明，抗性淀粉在大肠中被微生物发酵代谢能够产生一些短链脂肪酸，从而有助于结肠癌的防治；能够有效降低胆固醇，有利于体重控制；能够较好的调控血糖指数，因此有利于糖尿病的防治等。根据淀粉特性的不同将抗性淀粉分为五类：物理包埋淀粉，颗粒抗性淀粉，老化淀粉，变性淀粉与淀粉-脂类复合淀粉。变性淀粉(ModifiedStarch)是指利用物理、化学或酶的手段来改变天然淀粉的性质，通过分子切断、重排、氧化或在淀粉分子中引入取代基，制备得到性质得到优化或具备新的性质的淀粉衍生物。由于变性淀粉不仅具有良好的生理功效，还具有化学结构稳定、加工特性优良等优点，因此具有良好的发展潜力。交联改性是常用的一种化学改性方法，通过使用交联剂引入新的化学键使淀粉的稳定性增强。常用的交联剂有环氧丙烷、环氧氯丙烷、三偏磷酸钠、六偏磷酸钠等。目前国内的研究中，多采用单一交联剂对淀粉进行改性，且多采用传统的水浴加热法，这些方法制备的交联淀粉抗性淀粉含量低、生产耗时长、耗能大，生产效率低，从而限制了交联淀粉的工业化生产及应用。Resistant starch (Resistant Starch, RS) is a kind of starch and starch degradation products that cannot be digested in the small intestine of healthy humans, but can be fermented or partially fermented in the large intestine. The digestive properties of resistant starch endow it with a variety of important physiological functions. According to research, resistant starch is fermented and metabolized by microorganisms in the large intestine to produce some short-chain fatty acids, which contribute to the prevention and treatment of colon cancer; can effectively reduce cholesterol, It is beneficial to weight control; it can better regulate the blood sugar index, so it is beneficial to the prevention and treatment of diabetes. According to different starch properties, resistant starch can be divided into five categories: physically embedded starch, granular resistant starch, aged starch, modified starch and starch-lipid composite starch. Modified starch (Modified Starch) refers to the use of physical, chemical or enzymatic means to change the properties of native starch, through molecular cutting, rearrangement, oxidation or the introduction of substituents in starch molecules, the properties of which are optimized or have new properties. Starch derivatives. Because modified starch not only has good physiological effects, but also has the advantages of stable chemical structure and excellent processing characteristics, it has good development potential. Cross-linking modification is a commonly used chemical modification method, and the stability of starch is enhanced by using a cross-linking agent to introduce new chemical bonds. Commonly used crosslinking agents are propylene oxide, epichlorohydrin, sodium trimetaphosphate, sodium hexametaphosphate, etc. At present, in domestic research, a single cross-linking agent is mostly used to modify starch, and the traditional water bath heating method is mostly used. The cross-linked starch prepared by these methods has low content of resistant starch, long production time, large energy consumption, and low production efficiency. Low, thus limiting the industrial production and application of cross-linked starch.
【发明内容】【Content of invention】
本发明提供了一种高抗性淀粉含量的交联淀粉及其制备方法，以解决所述问题。The present invention provides a cross-linked starch with high resistant starch content and a preparation method thereof to solve the above problems.
为解决以上技术问题，本发明采用以下技术方案：In order to solve the above technical problems, the present invention adopts the following technical solutions:
一种高抗性淀粉含量的交联淀粉，所述高抗性淀粉含量的交联淀粉的抗性淀粉含量>80％，取代度>1.57*10-4，反应效率>70％。A cross-linked starch with high resistant starch content, the cross-linked starch with high resistant starch content has a resistant starch content > 80%, a substitution degree > 1.57*10-4 , and a reaction efficiency > 70%.
本发明还提供了一种高抗性淀粉含量的交联淀粉的制备方法，按以下步骤实施：将淀粉与双蒸水混合制备淀粉乳液A，将三聚磷酸钠-三偏磷酸钠复合交联剂、无水硫酸钠加入淀粉乳液A中，获得淀粉乳液B，调节淀粉乳液B体系pH，搅拌均匀，放置在微波合成反应工作站中反应，微波反应后，采用1mol/L的HCl溶液调整淀粉乳液的pH至6.0-6.5，以终止交联反应，然后离心、抽滤、洗涤、烘干、粉碎、过筛，制得高抗性淀粉含量的交联淀粉。The present invention also provides a preparation method of crosslinked starch with high resistant starch content, which is carried out according to the following steps: starch emulsion A is prepared by mixing starch with double distilled water, and sodium tripolyphosphate-sodium trimetaphosphate is compositely crosslinked Adding agent and anhydrous sodium sulfate to starch emulsion A to obtain starch emulsion B, adjust the pH of starch emulsion B system, stir evenly, and place it in a microwave synthesis reaction workstation for reaction. After microwave reaction, use 1mol/L HCl solution to adjust the starch emulsion pH to 6.0-6.5 to terminate the cross-linking reaction, and then centrifuged, suction filtered, washed, dried, crushed and sieved to obtain cross-linked starch with high resistant starch content.
优选地，所述淀粉为薯类淀粉。Preferably, the starch is potato starch.
优选地，所述淀粉乳液A浓度为28％-40％。Preferably, the concentration of the starch emulsion A is 28%-40%.
优选地，所述三聚磷酸钠-三偏磷酸钠复合交联剂的添加量为淀粉乳液B含量的10-15％，所述含量以淀粉干基计。Preferably, the added amount of the sodium tripolyphosphate-sodium trimetaphosphate composite crosslinking agent is 10-15% of the content of the starch emulsion B, and the content is calculated on a starch dry basis.
优选地，所述三聚磷酸钠-三偏磷酸钠复合交联剂中，三聚磷酸钠与三偏磷酸钠的比例为(1-30)：(70-99)。Preferably, in the sodium tripolyphosphate-sodium trimetaphosphate composite crosslinking agent, the ratio of sodium tripolyphosphate to sodium trimetaphosphate is (1-30):(70-99).
优选地，所述无水硫酸钠的添加量为淀粉乳液B含量的8-11％，所述含量以淀粉干基计。Preferably, the added amount of the anhydrous sodium sulfate is 8-11% of the content of the starch emulsion B, and the content is calculated on a dry starch basis.
优选地，所述淀粉乳液B体系pH为9-13。Preferably, the pH of the starch emulsion B system is 9-13.
优选地，所述微波温度40～55℃，微波功率为450-500W，微波反应时间为1-2min。Preferably, the microwave temperature is 40-55°C, the microwave power is 450-500W, and the microwave reaction time is 1-2min.
优选地，所述离心转速为3000r/min。Preferably, the centrifugal speed is 3000r/min.
本发明具有以下有益效果：The present invention has the following beneficial effects:
(1)本发明制备高抗性淀粉含量的交联淀粉采用的是复合交联剂，复合交联剂在交联过程中发挥着协同作用，能够显著提高交联反应效率；(1) The preparation of cross-linked starch with high resistant starch content in the present invention uses a composite cross-linking agent, which plays a synergistic role in the cross-linking process and can significantly improve the efficiency of the cross-linking reaction;
(2)本发明采用微波设备进行交联，相较于传统的水浴加热设备，微波设备具有加热均匀、速度快、耗能低等特点；(2) The present invention uses microwave equipment for cross-linking. Compared with traditional water bath heating equipment, microwave equipment has the characteristics of uniform heating, fast speed, and low energy consumption;
(3)用本发明的方法制备得到的交联淀粉，其抗性淀粉含量大于80％，取代度大于1.57*10-4，反应效率大于70％，高抗性淀粉含量的增加使交联淀粉的保健功能显著增强；(3) The cross-linked starch prepared by the method of the present invention has a resistant starch content greater than 80%, a degree of substitution greater than 1.57*10-4 , and a reaction efficiency greater than 70%. The increase in the content of high resistant starch makes the cross-linked starch The health care function is significantly enhanced;
(4)用本发明的方法制备得到的交联淀粉，其膨胀度和溶解度低，热稳定性与抗剪切稳定性好，不易发生回生老化，因此，本发明的交联淀粉具有良好的加工特性，为扩宽交联淀粉的应用范围提供依据。(4) The cross-linked starch prepared by the method of the present invention has low expansion and solubility, good thermal stability and shear stability, and is not prone to retrograde aging. Therefore, the cross-linked starch of the present invention has good processing properties. The characteristics provide a basis for broadening the application range of cross-linked starch.
【具体实施方式】【detailed description】
下面结合具体实施例进行具体说明。The following will be described in detail in conjunction with specific embodiments.
实施例1Example 1
准确称取25g马铃薯淀粉(干基)与双蒸水混合，制备得到浓度为40％的淀粉乳液A，将12％的三聚磷酸钠-三偏磷酸钠(三聚磷酸钠：三偏磷酸钠＝20:80)复合交联剂与10％无水硫酸钠加入淀粉乳中，其中加入量均以淀粉干基计，获得淀粉乳液B，调节淀粉乳液B体系pH为9，搅拌均匀，放置微波合成反应工作站中，在45℃下反应2min，功率设置为450W，微波反应过程中，同时进行磁力搅拌以保证加热的均匀性。微波反应后，采用1mol/L的HCl溶液调整淀粉乳液的pH至6.0，以终止交联反应，然后在3000r/min的离心机下离心、抽滤、洗涤、烘干、粉碎、过筛，制得高抗性淀粉含量的马铃薯交联淀粉。Accurately take by weighing 25g potato starch (dry basis) and mix with double distilled water, the starch emulsion A that preparation obtains concentration is 40%, with 12% sodium tripolyphosphate-sodium trimetaphosphate (sodium tripolyphosphate: sodium trimetaphosphate =20:80) composite cross-linking agent and 10% anhydrous sodium sulfate were added to the starch milk, and the amount added was based on starch dry basis to obtain starch emulsion B. Adjust the pH of the starch emulsion B system to 9, stir evenly, and place in microwave In the synthesis reaction workstation, the reaction was carried out at 45°C for 2 minutes, and the power was set to 450W. During the microwave reaction, magnetic stirring was carried out at the same time to ensure the uniformity of heating. After the microwave reaction, adjust the pH of the starch emulsion to 6.0 with 1mol/L HCl solution to terminate the crosslinking reaction, then centrifuge under a centrifuge at 3000r/min, filter with suction, wash, dry, pulverize, and sieve to prepare Potato cross-linked starch with high resistant starch content.
实施例2Example 2
准确称取25g马铃薯淀粉(干基)与双蒸水混合，制备得到浓度为40％的淀粉乳浊液，将10％三聚磷酸钠-三偏磷酸钠(三聚磷酸钠：三偏磷酸钠＝20:80)复合交联剂与10％无水硫酸钠加入淀粉乳中，其中加入量均以淀粉干基计，获得淀粉乳液B，调节淀粉乳液B体系pH为10，搅拌均匀，放置微波合成反应工作站中，在50℃下反应1.8min，功率设置为500W，微波反应过程中，同时进行磁力搅拌以保证加热的均匀性。微波反应后，采用1mol/L的HCl溶液调整淀粉乳液的pH至6.2，以终止交联反应，然后在3000r/min的离心机下离心、抽滤、洗涤、烘干、粉碎、过筛，制得高抗性淀粉含量的马铃薯交联淀粉。Accurately take by weighing 25g potato starch (dry basis) and mix with double distilled water, prepare the starch emulsion that concentration is 40%, with 10% sodium tripolyphosphate-sodium trimetaphosphate (sodium tripolyphosphate: sodium trimetaphosphate =20:80) composite cross-linking agent and 10% anhydrous sodium sulfate were added to the starch milk, and the amount added was based on starch dry basis to obtain starch emulsion B. Adjust the pH of the starch emulsion B system to 10, stir evenly, and place in microwave In the synthesis reaction workstation, react at 50°C for 1.8min, and set the power to 500W. During the microwave reaction, magnetic stirring is carried out at the same time to ensure the uniformity of heating. After the microwave reaction, adjust the pH of the starch emulsion to 6.2 with 1mol/L HCl solution to terminate the crosslinking reaction, then centrifuge under a centrifuge at 3000r/min, filter with suction, wash, dry, pulverize, and sieve to prepare Potato cross-linked starch with high resistant starch content.
实施例3Example 3
准确称取25g马铃薯淀粉(干基)与双蒸水混合，制备得到浓度为30％的淀粉乳浊液，将10％三聚磷酸钠-三偏磷酸钠(三聚磷酸钠：三偏磷酸钠＝10:90)复合交联剂与10％无水硫酸钠加入淀粉乳中，其中加入量均以淀粉干基计，获得淀粉乳液B，调节淀粉乳液B体系pH为11，搅拌均匀，放置微波合成反应工作站中，在50℃下反应1.2min，功率设置为500W，微波反应过程中，同时进行磁力搅拌以保证加热的均匀性。微波反应后，采用1mol/L的HCl溶液调整淀粉乳液的pH至6.5，以终止交联反应，然后在3000r/min的离心机下离心、抽滤、洗涤、烘干、粉碎、过筛，制得高抗性淀粉含量的马铃薯交联淀粉。Accurately take by weighing 25g potato starch (dry basis) and mix with double distilled water, prepare the starch emulsion that concentration is 30%, with 10% sodium tripolyphosphate-sodium trimetaphosphate (sodium tripolyphosphate: sodium trimetaphosphate =10:90) composite cross-linking agent and 10% anhydrous sodium sulfate were added to the starch emulsion, and the amount added was based on starch dry basis to obtain starch emulsion B. Adjust the pH of starch emulsion B system to 11, stir evenly, and place in microwave In the synthesis reaction workstation, react at 50°C for 1.2min, and set the power to 500W. During the microwave reaction, magnetic stirring is carried out at the same time to ensure the uniformity of heating. After the microwave reaction, adjust the pH of the starch emulsion to 6.5 with 1mol/L HCl solution to terminate the crosslinking reaction, then centrifuge under a centrifuge at 3000r/min, filter with suction, wash, dry, pulverize, and sieve to prepare Potato cross-linked starch with high resistant starch content.
实施例4Example 4
准确称取25g马铃薯淀粉(干基)与双蒸水混合，制备得到浓度为35％的淀粉乳浊液，将12％三聚磷酸钠-三偏磷酸钠(三聚磷酸钠：三偏磷酸钠＝30:70)复合交联剂与10％无水硫酸钠加入淀粉乳中，其中加入量均以淀粉干基计，，获得淀粉乳液B，调节淀粉乳液B体系pH为11，搅拌均匀，放置微波合成反应工作站中，在45℃下反应2min，功率设置为450W，微波反应过程中，同时进行磁力搅拌以保证加热的均匀性。微波反应后，采用1mol/L的HCl溶液调整淀粉乳液的pH至6.5，以终止交联反应，然后在3000r/min的离心机下离心、抽滤、洗涤、烘干、粉碎、过筛，制得高抗性淀粉含量的马铃薯交联淀粉。Accurately take by weighing 25g potato starch (dry base) and mix with double distilled water, prepare the starch emulsion that concentration is 35%, with 12% sodium tripolyphosphate-sodium trimetaphosphate (sodium tripolyphosphate: sodium trimetaphosphate =30:70) composite cross-linking agent and 10% anhydrous sodium sulfate are added to the starch milk, wherein the amount added is based on the starch dry basis, to obtain the starch emulsion B, adjust the pH of the starch emulsion B system to 11, stir evenly, and place In the microwave synthesis reaction workstation, the reaction was carried out at 45°C for 2 minutes, and the power was set to 450W. During the microwave reaction, magnetic stirring was carried out at the same time to ensure the uniformity of heating. After the microwave reaction, adjust the pH of the starch emulsion to 6.5 with 1mol/L HCl solution to terminate the crosslinking reaction, then centrifuge under a centrifuge at 3000r/min, filter with suction, wash, dry, pulverize, and sieve to prepare Potato cross-linked starch with high resistant starch content.
本发明制备得到的交联淀粉的结合磷含量、抗性淀粉含量、取代度、反应效率、糊化特性的测定按以下方法进行：The determination of the combined phosphorus content, resistant starch content, degree of substitution, reaction efficiency and gelatinization characteristics of the cross-linked starch prepared by the present invention is carried out as follows:
(1)结合磷含量(1) Bound phosphorus content
为了解交联后与马铃薯淀粉分子结合的磷含量，采用GB/T 22427-2008《淀粉及其衍生物磷总含量测定》中的方法对马铃薯淀粉的结合磷含量进行测定。交联淀粉中的磷总含量以样品磷总质量占样品质量的百分比表示，计算公式如下：In order to understand the phosphorus content combined with potato starch molecules after crosslinking, the method in GB/T 22427-2008 "Determination of Total Phosphorus Content in Starch and Its Derivatives" was used to determine the combined phosphorus content of potato starch. The total phosphorus content in the cross-linked starch is represented by the percentage of the total phosphorus mass of the sample in the sample mass, and the calculation formula is as follows:
式中：In the formula:
Δp——样品磷总含量，％；Δp - the total phosphorus content of the sample, %;
m1——从标准曲线上确定的样品液的磷质量，单位为微克(μg)；m1 - the mass of phosphorus in the sample solution determined from the standard curve, in micrograms (μg);
V0——样品液的定量体积，单位为毫升(mL)；V0 ——quantitative volume of the sample solution, in milliliters (mL);
m0——试验样品的质量，单位为克(g)；m0 - the mass of the test sample, in grams (g);
V1——用于测定的样品液的等分体积，单位为毫升(mL)。V1 ——the aliquot volume of the sample solution used for determination, in milliliter (mL).
(2)抗性淀粉含量(2) Resistant starch content
参照AOAC法(Enzymatic Digestion Resistant Starch in Starch and PlantMaterials.Arlington,VA:Association of Official Analytical Chemists(AOAC),2002)对马铃薯淀粉的抗性淀粉进行酶解，酶解后采用3，5-二硝基水杨酸法(薛慧.木薯抗性淀粉的制备与性质研究，河南工业大学,2013)对葡萄糖含量进行测定。Refer to the AOAC method (Enzymatic Digestion Resistant Starch in Starch and Plant Materials. Arlington, VA: Association of Official Analytical Chemists (AOAC), 2002) to enzymatically hydrolyze the resistant starch of potato starch, and use 3,5-dinitro Glucose content was determined by the salicylic acid method (Xue Hui. Preparation and Properties of Cassava Resistant Starch, Henan University of Technology, 2013).
(3)取代度(3) Degree of substitution
取代度反映每100g淀粉中结合磷的含量，其计算公式如下：The degree of substitution reflects the content of bound phosphorus per 100g of starch, and its calculation formula is as follows:
式中：In the formula:
np——每100g淀粉中结合磷的物质的量(np＝Δp/31)np - the amount of phosphorus-binding substances per 100g starch (np = Δp/31)
162——脱水葡萄糖的摩尔质量；162 - the molar mass of anhydroglucose;
100——干淀粉样品的质量，单位为g；100 - the mass of the dry starch sample, in g;
102——NaPO32-的摩尔质量。102——The molar mass of NaPO32- .
(4)反应效率(4) Reaction efficiency
反应效率值得是实际DS和理论DS(假设所加入的全部交联剂都与淀粉发生了反应)的比值，其计算公式如下：The reaction efficiency value is the ratio of the actual DS to the theoretical DS (assuming that all the crosslinking agents added have reacted with the starch), and its calculation formula is as follows:
(5)糊化性质测定(5) Determination of pasting properties
采用快速粘度测定仪(Rapid Visco Analyzer,RVA)对马铃薯淀粉及交联淀粉的糊化特性进行测定。用蒸馏水配制得到10％的淀粉乳，将淀粉乳充分搅拌后放置入快速粘度测定仪中，由室温升至50℃并保持1min，3.67min内上升到95℃，保持2.5min，然后下降到50℃并保持2min，记录这一过程的糊化温度、峰值粘度、最低粘度、消减值、最终粘度与回生值。The gelatinization properties of potato starch and cross-linked starch were measured by Rapid Visco Analyzer (RVA). Prepare 10% starch milk with distilled water. Stir the starch milk fully and put it into a rapid viscosity measuring instrument. Rise from room temperature to 50°C and keep it for 1min, rise to 95°C within 3.67min, keep it for 2.5min, and then drop to Keep at 50°C for 2 minutes, and record the gelatinization temperature, peak viscosity, minimum viscosity, subtraction value, final viscosity and retrogradation value of this process.
表1交联淀粉的结合磷含量、抗性淀粉含量、取代度、反应效率指标Table 1 Combined phosphorus content, resistant starch content, degree of substitution, and reaction efficiency indexes of cross-linked starch
注：表中的对照样品指的是采用传统的水浴法(70℃)与单一交联剂(三偏磷酸钠)所制备得到的交联淀粉。Note: The control sample in the table refers to the cross-linked starch prepared by the traditional water bath method (70°C) and a single cross-linking agent (sodium trimetaphosphate).
由表1可知，马铃薯淀粉磷含量为0.02％。实施例1、2、3、4制备得到的交联淀粉中的结合磷含量差异不大，但均远大于马铃薯原淀粉的结合磷含量，同时也大于对照样品的结合磷含量。但实施例中的交联淀粉中的结合磷含量均低于0.4％，符合国标对食用变性淀粉中结合磷的要求。It can be seen from Table 1 that the phosphorus content of potato starch is 0.02%. The bound phosphorus content in the cross-linked starches prepared in Examples 1, 2, 3, and 4 has little difference, but they are all far greater than the bound phosphorus content of the original potato starch, and also greater than the bound phosphorus content of the control sample. However, the combined phosphorus content in the cross-linked starches in the examples is all lower than 0.4%, which meets the requirements of the national standard for combined phosphorus in edible modified starch.
由表1可知，实施例1、2、3、4制备的交联淀粉的抗性淀粉含量均远高于马铃薯淀粉与传统方法制备的交联淀粉，表明采用微波设备与复合交联剂能够显著提高抗性淀粉的得率。It can be seen from Table 1 that the resistant starch content of the cross-linked starch prepared in Examples 1, 2, 3, and 4 is much higher than that of potato starch and the cross-linked starch prepared by traditional methods, indicating that microwave equipment and composite cross-linking agent can significantly Increase the yield of resistant starch.
由表1可知，实施例1、2、3、4中的交联淀粉的取代度与反应效率均远高于传统方法制备的交联淀粉，表明采用微波设备与复合交联剂能够显著提高交联反应的反应效率以及交联淀粉的取代度。It can be seen from Table 1 that the degree of substitution and reaction efficiency of cross-linked starches in Examples 1, 2, 3, and 4 are much higher than those prepared by traditional methods, indicating that the use of microwave equipment and composite cross-linking agents can significantly improve the cross-linked starch. The reaction efficiency of the cross-linking reaction and the degree of substitution of the cross-linked starch.
表2交联淀粉快速粘度测定结果Table 2 cross-linked starch rapid viscosity measurement results
注：表中的对照样品指的是采用传统的水浴法(70℃)与单一交联剂(三偏磷酸钠)所制备得到的交联淀粉。Note: The control sample in the table refers to the cross-linked starch prepared by the traditional water bath method (70°C) and a single cross-linking agent (sodium trimetaphosphate).
消减值为峰值粘度与最低粘度的差值，由表2可知，实施例1、2、3、4制备得到的交联淀粉的消减值均低于马铃薯淀粉与传统方法制备得到的交联淀粉的消减值，这是由于交联反应过程中淀粉之间形成的交联键能够使淀粉颗粒在高温与高剪切条件下尽量保持完整，降低粘度的损失，因此较低的消减值意味着较好的热稳定性与剪切稳定性。同时，复合交联剂微波法制备的交联淀粉的热稳定性与剪切稳定性要优于马铃薯淀粉与传统方法制备得到的交联淀粉。The subtraction value is the difference between the peak viscosity and the minimum viscosity. As can be seen from Table 2, the subtraction values of the cross-linked starches prepared in Examples 1, 2, 3, and 4 are all lower than the cross-linked starches prepared by potato starch and traditional methods. The reduction value of starch, which is due to the cross-linking bonds formed between starches during the cross-linking reaction can keep the starch granules as complete as possible under high temperature and high shear conditions, reducing the loss of viscosity, so the lower reduction value Means better thermal stability and shear stability. At the same time, the heat stability and shear stability of cross-linked starch prepared by composite cross-linking agent microwave method are better than potato starch and cross-linked starch prepared by traditional method.
回升值是最终粘度与最低粘度的差值，由表2可知，相较于马铃薯淀粉，实施例1、2、3、4以及对照样品的交联淀粉的回升值均明显提高，表明交联反应使淀粉更容易发生老化，但实施例1、2、3、4中制备得到的交联淀粉的回升值低于传统方法制备得到的交联淀粉的回升值，表明采用本发明制备得到的交联淀粉较不容易发生老化，而传统方法制备得到的交联淀粉比较容易发生老化。The recovery value is the difference between the final viscosity and the minimum viscosity. As can be seen from Table 2, compared with potato starch, the recovery values of the cross-linked starches of Examples 1, 2, 3, 4 and the control sample are all significantly improved, indicating that the cross-linking reaction Make starch more prone to aging, but the recovery value of the cross-linked starch prepared in Examples 1, 2, 3 and 4 is lower than that of the cross-linked starch prepared by the traditional method, indicating that the cross-linked starch prepared by the present invention Starch is less prone to aging, while cross-linked starch prepared by traditional methods is more prone to aging.
综合以上可以表明，与现有制备方法比较，本发明提供的方法能够获得高抗性淀粉含量的交联淀粉，且反应速率快、时间短、节能环保。此外，本发明制备得到的交联淀粉的热稳定性、抗剪切性较好，具有广阔的应用前景。Based on the above, it can be shown that compared with the existing preparation methods, the method provided by the present invention can obtain cross-linked starch with a high content of resistant starch, and has a fast reaction rate, short time, energy saving and environmental protection. In addition, the cross-linked starch prepared by the invention has good thermal stability and shear resistance, and has broad application prospects.
以上内容不能认定本发明具体实施只局限于这些说明，对于本发明所属技术领域的普通技术人员来说，在不脱离本发明构思前提下，还可以做出若干简单推演或替换，都应当视为属于本发明由所提交的权利要求书确定的专利保护范围。The above content cannot be considered that the specific implementation of the present invention is limited to these descriptions. For those of ordinary skill in the technical field of the present invention, they can also make some simple deduction or replacement without departing from the concept of the present invention, which should be regarded as Belonging to the scope of patent protection of the present invention determined by the submitted claims.
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| CN201711140751.3ACN107663241B (en) | 2017-11-16 | 2017-11-16 | Cross-linked starch with high resistant starch content and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111643730A (en)* | 2020-07-14 | 2020-09-11 | 华熙生物科技股份有限公司 | Preparation method and application of crosslinked hyaluronic acid gel for injection |
| CN111657498A (en)* | 2020-05-25 | 2020-09-15 | 华南理工大学 | High heat-resistant slowly digestible and resistant starch prepared by cell wall crosslinking and production method thereof |
| CN112176778A (en)* | 2020-09-25 | 2021-01-05 | 张淑玲 | Paper-plastic production process of one-step forming environment-friendly packaging box |
| CN113861300A (en)* | 2021-09-15 | 2021-12-31 | 华南理工大学 | Chemical cross-linked starch with slow gas production characteristic and preparation method and application thereof |
| CN116891538A (en)* | 2023-07-22 | 2023-10-17 | 广州市洲星食品有限公司 | Water chestnut resistant starch, preparation method and application |
| WO2024216831A1 (en)* | 2023-04-21 | 2024-10-24 | 中南林业科技大学 | Method for adjusting physical properties and digestion properties of starch |
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2771048C1 (en)* | 2020-10-29 | 2022-04-25 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Липецкий государственный технический университет" | Method for producing phosphorylated resistant starch |
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1995067A (en)* | 2006-12-20 | 2007-07-11 | 浙江工商大学 | Method for promoting resistant starch content of starch |
| CN105418774A (en)* | 2015-12-14 | 2016-03-23 | 熊小芳 | Method for preparing crosslinked starch by utilizing sodium trimetaphosphate crosslinking agent |
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1995067A (en)* | 2006-12-20 | 2007-07-11 | 浙江工商大学 | Method for promoting resistant starch content of starch |
| CN105418774A (en)* | 2015-12-14 | 2016-03-23 | 熊小芳 | Method for preparing crosslinked starch by utilizing sodium trimetaphosphate crosslinking agent |
| Title |
|---|
| K. S. WOO等: "Cross-Linked Resistant Starch: Preparation and Properties", 《CEREAL CHEM.》* |
| 倪海明等: "第6卷", 《大众科技》* |
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111657498A (en)* | 2020-05-25 | 2020-09-15 | 华南理工大学 | High heat-resistant slowly digestible and resistant starch prepared by cell wall crosslinking and production method thereof |
| CN111643730A (en)* | 2020-07-14 | 2020-09-11 | 华熙生物科技股份有限公司 | Preparation method and application of crosslinked hyaluronic acid gel for injection |
| CN112176778A (en)* | 2020-09-25 | 2021-01-05 | 张淑玲 | Paper-plastic production process of one-step forming environment-friendly packaging box |
| CN113861300A (en)* | 2021-09-15 | 2021-12-31 | 华南理工大学 | Chemical cross-linked starch with slow gas production characteristic and preparation method and application thereof |
| WO2024216831A1 (en)* | 2023-04-21 | 2024-10-24 | 中南林业科技大学 | Method for adjusting physical properties and digestion properties of starch |
| CN116891538A (en)* | 2023-07-22 | 2023-10-17 | 广州市洲星食品有限公司 | Water chestnut resistant starch, preparation method and application |
| Publication number | Publication date |
|---|---|
| CN107663241B (en) | 2020-05-12 |
| Publication | Publication Date | Title |
|---|---|---|
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