WO2024082619A1 - 一种"挤压-脱支"方式制备rs3型抗性淀粉的方法 - Google Patents

一种"挤压-脱支"方式制备rs3型抗性淀粉的方法 Download PDF

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WO2024082619A1
WO2024082619A1 PCT/CN2023/093840 CN2023093840W WO2024082619A1 WO 2024082619 A1 WO2024082619 A1 WO 2024082619A1 CN 2023093840 W CN2023093840 W CN 2023093840W WO 2024082619 A1 WO2024082619 A1 WO 2024082619A1
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starch
extrusion
debranching
resistant starch
preparing
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焦爱权
刘青
金征宇
杨月月
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江南大学
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    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00—Preparation of compounds containing saccharide radicals
    • C12P19/04—Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B30/00—Preparation of starch, degraded or non-chemically modified starch, amylose, or amylopectin
    • C08B30/20—Amylose or amylopectin
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00—Preparation of compounds containing saccharide radicals
    • C12P19/14—Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase

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  • the invention belongs to the technical field of functional foods, and specifically relates to a method for preparing RS 3 type resistant starch by an "extrusion-debranching" method.
  • starch can be divided into rapidly digestible starch (RDS), slowly digestible starch (SDS) and resistant starch (RS).
  • RDS rapidly digestible starch
  • SDS slowly digestible starch
  • RS resistant starch
  • the consumption of rapidly digestible starch will cause a rapid increase in blood sugar levels after a meal, while slowly digestible starch is digested more slowly and the blood sugar level after consumption is relatively low.
  • Resistant starch cannot be digested in the small intestine, but is fermented and degraded by intestinal flora in the colon to produce short-chain fatty acids and gas.
  • Resistant starch plays a key role in promoting a variety of beneficial health effects, including hypoglycemic and hypocholesterolemic effects, inhibiting body fat accumulation, increasing mineral absorption, reducing digestive tract cancer and preventing gallstone formation.
  • beneficial health effects including hypoglycemic and hypocholesterolemic effects, inhibiting body fat accumulation, increasing mineral absorption, reducing digestive tract cancer and preventing gallstone
  • Resistant starch is generally divided into five types: RS 1 , RS 2 , RS 3 , RS 4 and RS 5.
  • RS 3 has received special attention due to its thermal stability during the cooking process and its safety when consumed.
  • RS 3 mainly refers to recrystallized amylose, so the amylose content is the main factor affecting the formation and content of RS 3.
  • the amylose content in ordinary starch is low ( ⁇ 30%).
  • pullulanase debranching is a commonly used method to increase the amylose content.
  • debranching needs to be carried out after starch gelatinization.
  • the Chinese patent "A method for preparing high-amylose mung bean resistant starch” discloses a method for preparing mung bean resistant starch by ultrasonic combined enzymatic method, wherein the ratio of mung bean starch to water is 1:15-1:25 (w/v), and the pullulanase hydrolysis time is 10.0-14.0h;
  • the Chinese patent "A method for preparing glutinous wheat resistant starch” discloses a composite enzyme technology using pullulanase and branching enzyme synergistically to prepare glutinous wheat resistant starch, the mass concentration of starch milk is 4%-8%, and the pullulanase hydrolysis time is 4-6h.
  • the present invention aims to solve the problem of amylose and type III resistant starch (RS 3 )
  • RS 3 amylose and type III resistant starch
  • an extrusion-debranching method is proposed to achieve efficient and continuous industrial production of amylose and RS 3 type resistant starch.
  • Extrusion is a temperature-controlled, strong shear, short-time, low-cost industrial continuous thermomechanical production technology with the advantages of versatility and high yield.
  • the present application achieves full gelatinization, degradation and viscosity reduction of starch through the first extrusion, and the second extrusion and the action of debranching enzymes to achieve rapid and efficient debranching of high-concentration starch to obtain amylose, and obtain high-content resistant starch after recrystallization.
  • the object of the present invention is to provide a method for preparing RS 3 type resistant starch by an "extrusion-debranching" method, the method comprising the following steps:
  • step (2) The gelatinized starch crushed in step (1) is mixed with pullulanase, added into a twin-screw extruder, and extruded for a second time, the debranched starch after extrusion is collected and recrystallized, then washed with water, centrifuged, and the precipitate is collected and dried to obtain RS 3 type resistant starch; the rotation speed of the twin-screw extruder is 100-250rpm; the temperature of the six temperature zones of the extruder is increased successively to 35-100°C; the water content of the material in the extruder is 40-60wt%, and the starch mass concentration is 40-60%.
  • the rotation speed of the twin-screw extruder in step (1) is 100-250 rpm; the temperature of the 6 temperature zones of the extruder is increased successively to 35-120° C.; and the moisture content of the material is 30-60 wt %.
  • the starch in step (1) includes one or more of common starch and waxy starch.
  • the drying in step (1) can be carried out in conventional drying equipment at a drying temperature of 40-50°C, preferably 45°C.
  • the temperatures of the first five temperature zones of the twin-screw extruder in step (2) are 35-70°C, and the temperature of the last temperature zone is 95-100°C; preferably, the temperatures of the first five temperature zones are 35, 45, 55, 60, 65°C, respectively, and the temperature of the last temperature zone is 95°C.
  • the amount of pullulanase added in step (2) is 20-100 U/g (based on dry starch); preferably 80 U/g.
  • the recrystallization conditions in step (2) are: temperature of 2-25°C, time of 10-36h; preferably 4°C, time of 24h.
  • the centrifugal force in step (2) is 2000-5000 g, and the time is 5 to 20 min.
  • the drying in step (2) can be carried out in conventional drying equipment at a drying temperature of 40-50°C, preferably 45°C.
  • Another object of the present invention is to provide an RS 3 type resistant starch prepared by the above method.
  • the third object of the present invention is to provide an application of the above method in the field of food preparation.
  • the present invention provides a method for efficiently preparing RS 3 resistant starch by an "extrusion-debranching" method, which utilizes the synergistic effect of extrusion technology and pullulanase, and obtains high-content amylose and resistant starch by two extrusions, significantly reducing the digestibility of starch.
  • the method is simple and efficient, and can achieve rapid and efficient debranching of high-concentration starch, overcoming the problems of the substrate starch content (less than 15wt%) and the long debranching time in the prior art, and can achieve industrialized continuous production.
  • the optimum pH range of pullulanase is 4.2-4.8.
  • hydrochloric acid is usually added or the starch is dispersed in a buffered salt solution to adjust the pH.
  • the high concentration of starch allows pullulanase to have a wider optimum pH range than in the liquid system.
  • the present invention adopts the method of extrusion debranching at a high starch concentration, which reduces the dependence of pullulanase on pH and simplifies the production process.
  • the present invention will provide a theoretical basis and practical guidance for the continuous industrial production of amylose, and provide feasible strategies and methods for the industrial production of resistant starch and the development of low glycemic index foods.
  • a method for preparing RS 3 resistant starch by an "extrusion-debranching" method the method specifically comprising the following steps:
  • step (1) The corn starch gelatinized in step (1) is mixed with 20 U/g of pullulanase (based on the dry weight of ordinary corn starch), and added to the feeding end of a twin-screw extruder, the moisture content of the material is set to 60 wt%, and the mass concentration of corn starch is 40%; the temperatures of zones I, II, III, IV, V, and VI of the extruder are set to 35, 45, 55, 60, 65, and 95° C., respectively, the screw speed is 150 rpm, and extrusion is started, the debranched corn starch is collected and recrystallized at 4° C. for 24 h, and the soluble short chains are removed by centrifugation and water washing at 4000 g for 10 min, the precipitate is collected and dried at 45° C. to obtain resistant starch.
  • pullulanase based on the dry weight of ordinary corn starch
  • the amylose content in the sample was determined to be 71.53% using the Megazyme amylose and amylopectin assay kit, and the resistant starch content in the sample was determined to be 26.49% using the Englyst in vitro simulated digestion method, as shown in Tables 1 and 2, respectively.
  • a method for preparing RS 3 resistant starch by an "extrusion-debranching" method the method specifically comprising the following steps:
  • step (1) The corn starch gelatinized in step (1) is mixed with 40 U/g of pullulanase (based on the dry weight of ordinary corn starch), and added to the feeding end of a twin-screw extruder, the moisture content of the material is set to 60 wt%, and the mass concentration of corn starch is 40%; the temperatures of zones I, II, III, IV, V, and VI of the extruder are set to 35, 45, 55, 60, 65, and 95° C., respectively, the screw speed is 150 rpm, and extrusion is started, the debranched corn starch is collected and recrystallized at 4° C. for 24 h, centrifuged and washed at 4000 g for 10 min to remove the soluble short chains therein, and the precipitate is collected and dried at 45° C. to obtain resistant starch.
  • pullulanase based on the dry weight of ordinary corn starch
  • the amylose content in the sample was determined to be 75.34% using the Megazyme amylose and amylopectin assay kit, and the resistant starch content in the sample was determined to be 29.67% using the Englyst in vitro simulated digestion method, as shown in Tables 1 and 2, respectively.
  • a method for preparing RS 3 resistant starch by an "extrusion-debranching" method the method specifically comprising the following steps:
  • step (1) The corn starch gelatinized in step (1) is mixed with 60 U/g of pullulanase (based on the dry weight of ordinary corn starch), and added to the feeding end of a twin-screw extruder, the moisture content of the material is set to 60 wt%, and the mass concentration of corn starch is 40%; the temperatures of zones I, II, III, IV, V, and VI of the extruder are set to 35, 45, 55, 60, 65, and 95° C., respectively, the screw speed is 150 rpm, and extrusion is started, the debranched corn starch is collected and recrystallized at 4° C. for 24 h, centrifuged and washed at 4000 g for 10 min to remove the soluble short chains therein, and the precipitate is collected and dried at 45° C. to obtain resistant starch.
  • pullulanase based on the dry weight of ordinary corn starch
  • the amylose content in the sample was determined to be 80.70% using the Megazyme amylose and amylopectin assay kit, and the resistant starch content in the sample was determined to be 35.31% using the Englyst in vitro simulated digestion method, as shown in Tables 1 and 2, respectively.
  • a method for preparing RS 3 resistant starch by an "extrusion-debranching" method the method specifically comprising the following steps:
  • step (1) The corn starch gelatinized in step (1) was mixed with 80 U/g of pullulanase (based on the dry matter weight of ordinary corn starch). The mixture was mixed and added to the feeding end of a twin-screw extruder, and the moisture content of the material was set to 60wt%, and the mass concentration of corn starch was set to 40%; the temperatures of zones I, II, III, IV, V, and VI of the extruder were set to 35, 45, 55, 60, 65, and 95°C, respectively, and the screw speed was 150rpm. Extrusion was started, and the debranched corn starch was collected and recrystallized at 4°C for 24h. The soluble short chains were removed by centrifugation and washing at 4000g for 10min. The precipitate was collected and dried at 45°C to obtain resistant starch.
  • pullulanase based on the dry matter weight of ordinary corn starch.
  • the amylose content in the sample was determined to be 85.27% using the Megazyme amylose and amylopectin assay kit, and the resistant starch content in the sample was determined to be 40.39% using the Englyst in vitro simulated digestion method, as shown in Tables 1 and 2, respectively.
  • a method for preparing RS 3 resistant starch by an "extrusion-debranching" method the method specifically comprising the following steps:
  • step (1) The corn starch gelatinized in step (1) is mixed with 100 U/g of pullulanase (based on the dry weight of ordinary corn starch), and added to the feeding end of a twin-screw extruder, the moisture content of the material is set to 60 wt%, and the mass concentration of corn starch is 40%; the temperatures of zones I, II, III, IV, V, and VI of the extruder are set to 35, 45, 55, 60, 65, and 95° C., respectively, the screw speed is 150 rpm, and extrusion is started, the debranched corn starch is collected and recrystallized at 4° C. for 24 h, centrifuged and washed at 4000 g for 10 min to remove the soluble short chains therein, and the precipitate is collected and dried at 45° C. to obtain resistant starch.
  • pullulanase based on the dry weight of ordinary corn starch
  • the amylose content in the sample was determined to be 90.21% using the Megazyme amylose and amylopectin assay kit, and the resistant starch content in the sample was determined to be 41.50% using the Englyst in vitro simulated digestion method, as shown in Tables 1 and 2, respectively.
  • a method for preparing RS 3 resistant starch by an "extrusion-debranching" method the method specifically comprising the following steps:
  • step (1) The corn starch gelatinized in step (1) is mixed with 80 U/g of pullulanase (based on the dry weight of ordinary corn starch), and added to the feeding end of a twin-screw extruder.
  • the moisture content of the material is adjusted to 40 wt % and the mass concentration of corn starch is adjusted to 60%.
  • the temperatures of zones I, II, III, IV, V, and VI of the extruder are set to 35, 45, 55, 60, 65, and 95° C., respectively, and the screw speed is 150 rpm.
  • Extrusion is started, the debranched corn starch is collected and recrystallized at 4° C. for 24 h, and the soluble short chains are removed by centrifugation and water washing at 4000 g for 10 min. The precipitate is collected and dried at 45° C. to obtain resistant starch.
  • amylose content in the sample was determined to be 74.94% using the Megazyme amylose and amylopectin assay kit, and the resistant starch content in the sample was determined to be 29.78% using the Englyst in vitro simulated digestion method, as shown in Tables 1 and 2, respectively.
  • the amylose content in Comparative Example 1 was determined to be 29.52% using the Megazyme amylose and amylopectin assay kit, and the resistant starch content in the sample was determined to be 5.61% using the Englyst in vitro simulated digestion method, as shown in Tables 1 and 2, respectively.
  • step (1) The corn starch dried and crushed in step (1) is mixed with 20 U/g of pullulanase (based on the dry mass of ordinary corn starch), and water is added to make the mass concentration of corn starch 40%; at this time, the system is in a viscous solid state and cannot be stirred for enzymatic hydrolysis reaction.
  • pullulanase based on the dry mass of ordinary corn starch
  • the amylose content in Comparative Example 2 was determined to be 31.61% using the Megazyme amylose and amylopectin assay kit, and the resistant starch content in the sample was determined to be 8.16% using the Englyst in vitro simulated digestion method, as shown in Tables 1 and 2, respectively.
  • the preparation method of RS 3 resistant starch of the present invention realizes efficient debranching of starch at high starch substrate concentration and in a short time by extrusion-debranching means, and provides a feasible method for the industrial production of amylose and resistant starch.
  • the amylose content in the starch can be as high as 90.21%, and the resistant starch content can be as high as 41.50%; the method is simple to operate, has high production efficiency, and can be applied to industrial continuous production.

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Abstract

提供一种"挤压-脱支"方式制备RS3型抗性淀粉的方法，属于功能食品型抗性淀粉的方法，属于功能食品技术领域。所述"挤压-脱支"方式制备RS3型抗性淀粉的方法包括如下：将淀粉原料加入双螺杆挤压机，进行一次挤压，收集挤压糊化、降解后的淀粉并干燥粉碎；将粉碎后的糊化淀粉与普鲁兰酶充分混合，加入到双螺杆挤压机，进行二次挤压，收集挤压后的脱支淀粉，并进行重结晶，之后离心水洗、收集沉淀并干燥，得到RS3型抗性淀粉。该方法实现了高底物淀粉浓度的快速高效脱支，增加了RS3型抗性淀粉含量，解决了RS3型抗性淀粉产出效率较低的问题；为抗性淀粉的连续工业化生产提供理论基础和实际指导。

Description

一种“挤压-脱支”方式制备RS3型抗性淀粉的方法 技术领域
本发明属于功能性食品技术领域，具体涉及一种“挤压-脱支”方式制备RS3型抗性淀粉的方法。
背景技术
根据消化速率，淀粉可以被分为快消化淀粉(Rapidly digestible starch，RDS)，慢消化淀粉(Slowly digestible starch，SDS)和抗性淀粉(Resistant starch，RS)。食用快消化淀粉会引起餐后血糖水平的快速升高，而慢消化淀粉消化较慢，食用后血糖水平相对较低。抗性淀粉不能在小肠中被消化，而是在结肠中被肠道菌群发酵降解，产生短链脂肪酸和气体。抗性淀粉在促进多种有益健康的作用中发挥关键作用，包括降血糖和降胆固醇作用、抑制体脂积累、增加矿物质吸收、减少消化道癌症和预防胆结石形成。随着糖尿病对人类健康威胁的日益增加，抗性淀粉的发展对肥胖患者和糖尿病人具有重要的意义。然而，目前抗性淀粉的工业化水平较低，商业化可用的抗性淀粉产品较少。
抗性淀粉通常分为5种类型：RS1，RS2，RS3，RS4和RS5。其中，RS3因其在熟化过程中的热稳定性和食用时的安全性而受到特别关注。RS3主要指的是重结晶的直链淀粉，因此，直链淀粉含量是影响RS3形成和含量的主要因素。然而，普通淀粉中直链淀粉含量较低(＜30％)。目前，普鲁兰酶脱支是增加直链淀粉含量常用的方法，但是，脱支需在淀粉糊化后进行，由于糊化淀粉的高粘度，脱支反应需要在高液相体系中进行，淀粉浓度通常较低(＜15wt％)，且酶解时间较长。中国专利“一种高直链绿豆抗性淀粉的制备方法”(申请号202111157414.1)公开了一种超声联合酶法制备绿豆抗性淀粉的方法，其中，绿豆淀粉和水的比例为1:15-1:25(w/v)，普鲁兰酶酶解时间为10.0-14.0h；中国专利“一种糯麦抗性淀粉的制备方法”(申请号202111651682.9)公开了一种采用普鲁兰酶和分支酶协同作用的复合酶技术来制备糯麦抗性淀粉，淀粉乳的质量浓度为4％-8％，普鲁兰酶酶解时间为4-6h。较低的底物浓度和较长的酶解时间限制了酶脱支提高直链淀粉含量的效率，无法满足直链淀粉工业化生产的需要。
因此，发现新的策略来提高淀粉脱支得到直链淀粉的效率对于抗性淀粉的工业化生产具有重要的意义。
发明内容
针对现有技术存在的技术缺陷，本发明的目的在于解决直链淀粉和III型抗性淀粉(RS3) 产出效率较低的问题，为此提出一种挤压-脱支手段来实现直链淀粉和RS3型抗性淀粉的高效持续工业化生产。挤压是温度可控，强剪切，短时，低成本的工业化持续热机械生产技术，具有多功能性和高产率的优势。本申请通过第一次挤压实现淀粉的充分糊化，降解和粘度的降低，第二次挤压并配合脱支酶的作用实现高浓度淀粉的快速高效脱支，得到直链淀粉，重结晶后得到高含量的抗性淀粉。
本发明的目的是提供一种“挤压-脱支”方式制备RS3型抗性淀粉的方法，所述方法包括以下步骤：
(1)将淀粉原料加入双螺杆挤压机，进行一次挤压，收集挤压糊化降解后的淀粉并干燥粉碎；
(2)将步骤(1)粉碎后的糊化淀粉与普鲁兰酶混合，加入双螺杆挤压机，进行二次挤压，收集挤压后的脱支淀粉，并进行重结晶，之后水洗离心、收集沉淀并干燥，得到RS3型抗性淀粉；所述双螺杆挤压机的转速为100-250rpm；挤压机6个温区温度依次升高，为35-100℃；挤压机中物料含水量为40～60wt％，淀粉质量浓度为40～60％。
在一种实施方式中，步骤(1)所述双螺杆挤压机的转速为100-250rpm；挤压机6个温区温度依次升高，为35-120℃；物料含水量为30-60wt％。
在一种实施方式中，步骤(1)所述淀粉包括普通淀粉、蜡质淀粉中的一种或多种。
在一种实施方式中，步骤(1)干燥在常规干燥设备中进行即可，干燥温度为40-50℃，优选为45℃。
在一种实施方式中，步骤(2)所述双螺杆挤压机的前5个温区的温度为35-70℃，最后一个温区的温度为95-100℃；优选的前5个温区的温度分别为35，45，55，60，65℃，最后一个温区的温度为95℃。
在一种实施方式中，步骤(2)所述普鲁兰酶的添加量为20-100U/g(基于淀粉干基计)；优选为80U/g。
在一种实施方式中，步骤(2)所述重结晶的条件为：温度为2-25℃，时间为10-36h；优选为4℃，时间为24h。
在一种实施方式中，步骤(2)所述离心力为2000-5000g，时间为5～20min。
在一种实施方式中，步骤(2)所述干燥在常规干燥设备中进行即可，干燥温度为40-50℃，优选为45℃。
本发明的另一目的是提供一种由上述所述方法制备得到的RS3型抗性淀粉。
本发明的第三个目的是提供一种上述所述方法在食品制备领域中的应用。
本发明的有益效果：
(1)本发明的一种“挤压-脱支”方式高效制备RS3型抗性淀粉的方法，利用挤压技术和普鲁兰酶的协同作用，通过两次挤压手段，即获得高含量的直链淀粉和抗性淀粉，显著降低了淀粉的消化性能。该方法简单、高效，能够实现高浓度淀粉的快速高效脱支，克服了现有技术中底物淀粉含量(低于15wt％)不能过高和脱支时间长的问题，能够实现工业化的连续生产。
(2)普鲁兰酶最适pH值范围为4.2-4.8，淀粉脱支时，通常要加盐酸或将淀粉分散在缓冲盐溶液中来调节pH值。而在挤压体系中，由于淀粉基质的缓冲特异性，高浓度的淀粉使得普鲁兰酶比在液体体系中具有更宽的最适pH范围。本发明采用高淀粉浓度挤压脱支的手段，减少了普鲁兰酶对pH的依赖性，简化了生产工艺。
(3)本发明将为直链淀粉的连续工业化生产提供理论基础和实际指导，并为工业化生产抗性淀粉，开发低血糖指数食品提供可行的策略和方法。
具体实施方式
下面将结合本发明中的实施例，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
一种“挤压-脱支”方式制备RS3型抗性淀粉的方法，所述方法具体包括如下步骤：
(1)将普通玉米淀粉加入双螺杆挤压机喂料端，设置物料含水量为40wt％，螺杆转速为150rpm，挤压机(ZE-16)Ⅰ、Ⅱ、Ⅲ、Ⅳ、Ⅴ、VI区温度分别设置为35，45，60，80，100和120℃，并开始挤压，收集充分糊化的玉米淀粉于45℃干燥后粉碎；
(2)将步骤(1)糊化后的玉米淀粉与20U/g的普鲁兰酶(以普通玉米淀粉干物质量计)混合，加入到双螺杆挤压机喂料端，设置物料含水量为60wt％，玉米淀粉质量浓度为40％；挤压机Ⅰ、Ⅱ、Ⅲ、Ⅳ、Ⅴ、VI区温度分别设置为35，45，55，60，65和95℃，螺杆转速为150rpm，并开始挤压，收集脱支的玉米淀粉并于4℃重结晶24h，4000g离心水洗10min去掉其中的可溶性短链，收集沉淀并于45℃干燥后，得到抗性淀粉。
普鲁兰酶含量为20U/g时，使用Megazyme直链淀粉和支链淀粉测定试剂盒测定样品中直链淀粉含量为71.53％，使用Englyst体外模拟消化法测定样品中抗性淀粉含量为26.49％，分别如表1、表2所示。
实施例2
一种“挤压-脱支”方式制备RS3型抗性淀粉的方法，所述方法具体包括如下步骤：
(1)将普通玉米淀粉加入双螺杆挤压机喂料端，设置物料含水量为40wt％，螺杆转速为150rpm，挤压机(ZE-16)Ⅰ、Ⅱ、Ⅲ、Ⅳ、Ⅴ、VI区温度分别设置为35，45，60，80，100和120℃，并开始挤压，收集充分糊化的玉米淀粉于45℃干燥后粉碎；
(2)将步骤(1)糊化后的玉米淀粉与40U/g的普鲁兰酶(以普通玉米淀粉干物质量计)混合，加入到双螺杆挤压机喂料端，设置物料含水量为60wt％，玉米淀粉质量浓度为40％；挤压机Ⅰ、Ⅱ、Ⅲ、Ⅳ、Ⅴ、VI区温度分别设置为35，45，55，60，65和95℃，螺杆转速为150rpm，并开始挤压，收集脱支的玉米淀粉并于4℃重结晶24h，4000g离心水洗10min去掉其中的可溶性短链，收集沉淀并于45℃干燥后得到抗性淀粉。
普鲁兰酶含量为40U/g时，使用Megazyme直链淀粉和支链淀粉测定试剂盒测定样品中直链淀粉含量为75.34％，使用Englyst体外模拟消化法测定样品中抗性淀粉含量为29.67％，分别如表1、表2所示。
实施例3
一种“挤压-脱支”方式制备RS3型抗性淀粉的方法，所述方法具体包括如下步骤：
(1)将普通玉米淀粉加入双螺杆挤压机喂料端，设置物料含水量为40wt％，螺杆转速为150rpm，挤压机(ZE-16)Ⅰ、Ⅱ、Ⅲ、Ⅳ、Ⅴ、VI区温度分别设置为35，45，60，80，100和120℃，并开始挤压，收集充分糊化的玉米淀粉于45℃干燥后并粉碎；
(2)将步骤(1)糊化后的玉米淀粉与60U/g的普鲁兰酶(以普通玉米淀粉干物质量计)混合，加入到双螺杆挤压机喂料端，设置物料含水量为60wt％，玉米淀粉质量浓度为40％；挤压机Ⅰ、Ⅱ、Ⅲ、Ⅳ、Ⅴ、VI区温度分别设置为35，45，55，60，65和95℃，螺杆转速为150rpm，并开始挤压，收集脱支的玉米淀粉并于4℃重结晶24h，4000g离心水洗10min去掉其中的可溶性短链，收集沉淀并于45℃干燥后得到抗性淀粉。
普鲁兰酶含量为60U/g时，使用Megazyme直链淀粉和支链淀粉测定试剂盒测定样品中直链淀粉含量为80.70％，使用Englyst体外模拟消化法测定样品中抗性淀粉含量为35.31％，分别如表1、表2所示。
实施例4
一种“挤压-脱支”方式制备RS3型抗性淀粉的方法，所述方法具体包括如下步骤：
(1)将普通玉米淀粉加入双螺杆挤压机喂料端，设置物料含水量为40wt％，螺杆转速为150rpm，挤压机(ZE-16)Ⅰ、Ⅱ、Ⅲ、Ⅳ、Ⅴ、VI区温度分别设置为35，45，60，80，100和120℃，并开始挤压，收集充分糊化的玉米淀粉于45℃干燥后并粉碎；
(2)将步骤(1)糊化后的玉米淀粉与80U/g的普鲁兰酶(以普通玉米淀粉干物质量计) 混合，加入到双螺杆挤压机喂料端，设置物料含水量为60wt％，玉米淀粉质量浓度为40％；挤压机Ⅰ、Ⅱ、Ⅲ、Ⅳ、Ⅴ、VI区温度分别设置为35，45，55，60，65和95℃，螺杆转速为150rpm，并开始挤压，收集脱支的玉米淀粉并于4℃重结晶24h，4000g离心水洗10min去掉其中的可溶性短链，收集沉淀并于45℃干燥后得到抗性淀粉。
普鲁兰酶含量为80U/g时，使用Megazyme直链淀粉和支链淀粉测定试剂盒测定样品中直链淀粉含量为85.27％，使用Englyst体外模拟消化法测定样品中抗性淀粉含量为40.39％，分别如表1、表2所示。
实施例5
一种“挤压-脱支”方式制备RS3型抗性淀粉的方法，所述方法具体包括如下步骤：
(1)将普通玉米淀粉加入双螺杆挤压机喂料端，设置物料含水量为40wt％，螺杆转速为150rpm，挤压机(ZE-16)Ⅰ、Ⅱ、Ⅲ、Ⅳ、Ⅴ、VI区温度分别设置为35，45，60，80，100和120℃，并开始挤压，收集充分糊化的玉米淀粉于45℃干燥后并粉碎；
(2)将步骤(1)糊化后的玉米淀粉与100U/g的普鲁兰酶(以普通玉米淀粉干物质量计)混合，加入到双螺杆挤压机喂料端，设置物料含水量为60wt％，玉米淀粉质量浓度为40％；挤压机Ⅰ、Ⅱ、Ⅲ、Ⅳ、Ⅴ、VI区温度分别设置为35，45，55，60，65和95℃，螺杆转速为150rpm，并开始挤压，收集脱支的玉米淀粉并于4℃重结晶24h，4000g离心水洗10min去掉其中的可溶性短链，收集沉淀并于45℃干燥后得到抗性淀粉。
普鲁兰酶含量为100U/g时，使用Megazyme直链淀粉和支链淀粉测定试剂盒测定样品中直链淀粉含量为90.21％，使用Englyst体外模拟消化法测定样品中抗性淀粉含量为41.50％，分别如表1、表2所示。
实施例6
一种“挤压-脱支”方式制备RS3型抗性淀粉的方法，所述方法具体包括如下步骤：
(1)将普通玉米淀粉加入双螺杆挤压机喂料端，设置物料含水量为40wt％，螺杆转速为150rpm，挤压机(ZE-16)Ⅰ、Ⅱ、Ⅲ、Ⅳ、Ⅴ、VI区温度分别设置为35，45，60，80，100和120℃，并开始挤压，收集充分糊化的玉米淀粉于45℃干燥后粉碎；
(2)将步骤(1)糊化后的玉米淀粉与80U/g的普鲁兰酶(以普通玉米淀粉干物质量计)混合，加入到双螺杆挤压机喂料端，分别调整设置物料含水量为40wt％，玉米淀粉质量浓度为60％；挤压机Ⅰ、Ⅱ、Ⅲ、Ⅳ、Ⅴ、VI区温度分别设置为35，45，55，60，65和95℃，螺杆转速为150rpm，开始挤压，收集脱支的玉米淀粉并于4℃重结晶24h，4000g离心水洗10min去掉其中的可溶性短链，收集沉淀并于45℃干燥后，得到抗性淀粉。
玉米淀粉质量浓度为60％时，使用Megazyme直链淀粉和支链淀粉测定试剂盒测定样品中直链淀粉含量为74.94％，使用Englyst体外模拟消化法测定样品中抗性淀粉含量为29.78％，分别如表1、表2所示。
对比例1
将普通玉米淀粉加入双螺杆挤压机喂料端，设置水分为40wt％，螺杆转速为150rpm，挤压机(ZE-16)Ⅰ、Ⅱ、Ⅲ、Ⅳ、Ⅴ、VI区温度分别设置为35，45，60，80，100和120℃，并开始挤压，收集充分糊化的玉米淀粉于45℃干燥后粉碎后即得。
使用Megazyme直链淀粉和支链淀粉测定试剂盒测定对比例1中直链淀粉含量为29.52％，使用Englyst体外模拟消化法测定样品中抗性淀粉含量为5.61％，分别如表1、表2所示。
对比例2
(1)将普通玉米淀粉加入双螺杆挤压机喂料端，设置水分为40wt％，螺杆转速为150rpm，挤压机(ZE-16)Ⅰ、Ⅱ、Ⅲ、Ⅳ、Ⅴ、VI区温度分别设置为35，45，60，80，100和120℃，并开始挤压，收集充分糊化的玉米淀粉于45℃干燥后并粉碎；
(2)将糊化的玉米淀粉加入双螺杆挤压机喂料端，设置水分为60wt％，挤压机Ⅰ、Ⅱ、Ⅲ、Ⅳ、Ⅴ、VI区温度分别设置为35，45，55，60，65和95℃，螺杆转速为150rpm，并开始挤压，收集挤出物并于4℃重结晶24h，并于45℃干燥后即得。
对比例3
(1)将普通玉米淀粉加入双螺杆挤压机喂料端，设置物料含水量为40wt％，螺杆转速为150rpm，挤压机(ZE-16)Ⅰ、Ⅱ、Ⅲ、Ⅳ、Ⅴ、VI区温度分别设置为35，45，60，80，100和120℃，并开始挤压，收集充分糊化的玉米淀粉于45℃干燥后粉碎；
(2)将步骤(1)干燥粉碎后的玉米淀粉与20U/g的普鲁兰酶(以普通玉米淀粉干物质量计)混合，加水使玉米淀粉质量浓度为40％；此时体系呈黏性固态，无法进行搅拌酶解反应。
使用Megazyme直链淀粉和支链淀粉测定试剂盒测定对比例2中直链淀粉含量为31.61％，使用Englyst体外模拟消化法测定样品中抗性淀粉含量为8.16％，分别如表1、表2所示。
表1样品的直链淀粉含量

(注：abcdef字母不同，表示各组数据之间有显著性差异，p<0.05)
表2样品中快消化淀粉，慢消化淀粉与抗性淀粉含量

(注：abcdef字母不同，表示各组数据之间有显著性差异，p<0.05)
本发明的RS3型抗性淀粉的制备方法，采用挤压-脱支手段实现了高淀粉底物浓度和短时间下淀粉的高效脱支，为直链淀粉和抗性淀粉的工业化生产提供了可行的方法。经挤压-脱支后，淀粉中直链淀粉含量可高达90.21％，抗性淀粉含量可高达41.50％；该方法操作简单、生产效率高，能够应用于工业化的连续生产。
上述的实施例的描述是为便于该技术领域的普通技术人员能理解和使用发明。熟悉本领域技术的人员显然可以容易地对这些实施例做出各种修改，并把在此说明的一般原理应用到其他实施例中而不必经过创造性的劳动。因此，本发明不限于上述实施例，本领域技术人员 根据本发明的揭示，不脱离本发明范畴所做出的改进和修改都应该在本发明的保护范围之内。

Claims (10)

  1. 一种“挤压-脱支”方式制备RS3型抗性淀粉的方法，其特征在于，所述方法包括以下步骤：
    (1)将淀粉原料加入双螺杆挤压机，进行一次挤压，收集挤压糊化、降解后的淀粉并干燥粉碎；
    (2)将步骤(1)粉碎后的糊化淀粉与普鲁兰酶充分混合，加入到双螺杆挤压机，进行二次挤压，收集挤压后的脱支淀粉，并进行重结晶，之后水洗离心、收集沉淀并干燥，得到RS3型抗性淀粉；所述双螺杆挤压机的转速为100-250rpm；，挤压机6个温区温度依次升高，为35-100℃；挤压机中物料含水量为40～60wt％，淀粉质量浓度为40～60％。
  2. 根据权利要求1所述的“挤压-脱支”方式制备RS3型抗性淀粉的方法，其特征在于，步骤(1)所述双螺杆挤压机的转速为100-250rpm；挤压机6个温区温度依次升高，为35-120℃；物料含水量为30-60wt％。
  3. 根据权利要求1所述的“挤压-脱支”方式制备RS3型抗性淀粉的方法，其特征在于，步骤(1)所述淀粉包括普通淀粉、蜡质淀粉中的一种或多种。
  4. 根据权利要求1所述的“挤压-脱支”方式制备RS3型抗性淀粉的方法，其特征在于，步骤(1)干燥在常规干燥设备中进行，干燥温度为40-50℃。
  5. 根据权利要求1所述的“挤压-脱支”方式制备RS3型抗性淀粉的方法，其特征在于，步骤(2)所述双螺杆挤压机的前5个温区的温度为35-70℃，最后一个温区的温度为95-100℃。
  6. 根据权利要求1所述的“挤压-脱支”方式制备RS3型抗性淀粉的方法，其特征在于，步骤(2)所述普鲁兰酶的添加量以淀粉干基计为20-100U/g。
  7. 根据权利要求1所述的“挤压-脱支”方式制备RS3型抗性淀粉的方法，其特征在于，步骤(2)所述重结晶的条件为：温度为2-25℃，时间为10-36h。
  8. 根据权利要求1所述的“挤压-脱支”方式制备RS3型抗性淀粉的方法，其特征在于，步骤(2)所述离心力为2000-5000g，时间为5-20min.
  9. 根据权利要求1所述的“挤压-脱支”方式制备RS3型抗性淀粉的方法，其特征在于，步骤(2)所述干燥在常规干燥设备中进行，干燥温度为40-50℃。
  10. 由权利要求1～9任一项所述的“挤压-脱支”方式制备RS3型抗性淀粉的方法在食品制备领域中的应用。
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20060037153A (ko) * 2004-10-27 2006-05-03 동아제분 주식회사 압출성형공법을 이용한 효소저항전분의 생산방법
US20190169663A1 (en) * 2016-04-11 2019-06-06 Zibohuichuang Biological Scientific Technology Limited Company Material pretreatement method using low-temperature extrusion and multienzyme synergistic degradation
CN110144014A (zh) * 2019-06-01 2019-08-20 江苏昕宇药业有限公司 一种玉米制作抗性淀粉的工艺
US20200345046A1 (en) * 2019-07-30 2020-11-05 Jiangnan University Preparation Method of Rice Noodle with Low Glycemic Index
CN115466759A (zh) * 2022-10-21 2022-12-13 江南大学 一种“挤压-脱支”方式制备rs3型抗性淀粉的方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20060037153A (ko) * 2004-10-27 2006-05-03 동아제분 주식회사 압출성형공법을 이용한 효소저항전분의 생산방법
US20190169663A1 (en) * 2016-04-11 2019-06-06 Zibohuichuang Biological Scientific Technology Limited Company Material pretreatement method using low-temperature extrusion and multienzyme synergistic degradation
CN110144014A (zh) * 2019-06-01 2019-08-20 江苏昕宇药业有限公司 一种玉米制作抗性淀粉的工艺
US20200345046A1 (en) * 2019-07-30 2020-11-05 Jiangnan University Preparation Method of Rice Noodle with Low Glycemic Index
CN115466759A (zh) * 2022-10-21 2022-12-13 江南大学 一种“挤压-脱支”方式制备rs3型抗性淀粉的方法

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
PONGJANTA, ET AL: "Enzymes-Resistant Starch (RS III) from Pullulanase-Debranched High Amylose Rice Starch", KASETSART J. ( NAT. SCI.)., vol. 42, 1 January 2008 (2008-01-01), pages 198 - 205, XP055869100 *
ZHIGANG XIAO: "Optimization of Preparation Process of Resistant Starch by Extrusion and Enzymatic Hydrolysis", GAIN PROCESSING, CN, vol. 41, no. 02, 31 December 2016 (2016-12-31), CN , pages 27 - 33, XP093162827, ISSN: 1007-6395 *

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