CN105237647A - Method for preparing high-purity resistant dextrin by improving acidity - Google Patents

Method for preparing high-purity resistant dextrin by improving acidity Download PDF

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CN105237647A
CN105237647A CN201510803737.1A CN201510803737A CN105237647A CN 105237647 A CN105237647 A CN 105237647A CN 201510803737 A CN201510803737 A CN 201510803737A CN 105237647 A CN105237647 A CN 105237647A
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resistant dextrin
acid
starch
temperature
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刘宗利
王乃强
刘峰
李克文
栾庆民
柏帅
窦续同
应汉杰
张维维
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Baolingbao Biology Co Ltd
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Abstract

本发明提供了一种通过提高酸度制备高纯度抗性糊精的方法,包括如下步骤:以玉米淀粉为原料,用酸处理,在高温下进行热解反应,获得含有抗性糊精的粗品,粗品再通过酶解、脱色、离交、色谱、浓缩和喷雾干燥后,制得抗性糊精。本发明采用提高酸度的方法,通过高温热解,获得高纯度抗性糊精,较传统制备方法热解温度低,反应时间短,副反应物少,节约生产成本。The invention provides a method for preparing high-purity resistant dextrin by increasing acidity, comprising the following steps: using cornstarch as raw material, treating with acid, performing pyrolysis reaction at high temperature, and obtaining a crude product containing resistant dextrin, The crude product is subjected to enzymatic hydrolysis, decolorization, separation, chromatography, concentration and spray drying to obtain resistant dextrin. The invention adopts the method of increasing the acidity, and obtains high-purity resistant dextrin through high-temperature pyrolysis, which has lower pyrolysis temperature than the traditional preparation method, short reaction time, less side reactants, and saves production cost.

Description

一种通过提高酸度制备高纯度抗性糊精的方法A method for preparing high-purity resistant dextrin by increasing acidity

技术领域 technical field

本发明涉及淀粉深加工领域,特别涉及一种高纯度抗性糊精的制备方法。 The invention relates to the field of starch deep processing, in particular to a preparation method of high-purity resistant dextrin.

背景技术 Background technique

膳食纤维是维系人类身体健康。不能被其他物质所代替的“第七营养素”。现在许多发达国家已经意识到膳食纤维的生理作用对于机体不可替代的功能,研发了多重复函膳食纤维的食品,并占据了大部分食品市场。 Dietary fiber is to maintain human health. The "seventh nutrient" that cannot be replaced by other substances. Now many developed countries have realized that the physiological role of dietary fiber is an irreplaceable function for the body, and have developed foods with multiple functions of dietary fiber, which have occupied most of the food market.

抗性糊精由淀粉加工而成,属于水溶性膳食纤维。抗性糊精具有较好的热稳定性、低热值低血糖指数等特性,而且含有α-1,2和α-1,3键相连的葡萄糖苷结构,且在部分还原末端含有β-1,6的结构。因此它在体内不易被分解,可直接进入大肠,作为膳食纤维发挥其生理作用。 Resistant dextrin is processed from starch and belongs to water-soluble dietary fiber. Resistant dextrin has good thermal stability, low calorie value and low glycemic index, and contains glucoside structures linked by α-1,2 and α-1,3 bonds, and contains β-1, 6 structures. Therefore, it is not easy to be decomposed in the body, and can directly enter the large intestine to play its physiological role as dietary fiber.

传统制备抗性糊精的方法中是在较低酸度下进行热解反应,再经酶解精制干燥得到抗性糊精,该方法的缺点是淀粉需要预处理,热解反应温度高,反应时间长,副反应产物成分复杂且多,成本较高。如: The traditional method of preparing resistant dextrin is to carry out pyrolysis reaction at low acidity, and then obtain resistant dextrin through enzymatic purification and drying. The disadvantage of this method is that starch needs to be pretreated, the pyrolysis reaction temperature is high, and the reaction time Long, the side reaction products have complex and many components, and the cost is higher. Such as:

中国专利文献CN104403009A(申请号201410671093.0)公开了一种制备抗性糊精的方法,包括以下步骤:(1)在淀粉中加入酸,搅匀,得酸处理淀粉,将酸处理淀粉经预干燥处理,得预干燥淀粉;(2)选取海砂,将海砂与预干燥淀粉混匀,调节温度为170-220℃进行热解反应;(3)热解反应结束后获得焦糊精粗品,将其精制得到抗性糊精产品。所述酸的加入量为淀粉中质量的0.02-0.2%。 Chinese patent document CN104403009A (Application No. 201410671093.0) discloses a method for preparing resistant dextrin, which includes the following steps: (1) Add acid to starch, stir well to obtain acid-treated starch, and pre-dry the acid-treated starch , to obtain pre-dried starch; (2) select sea sand, mix sea sand with pre-dried starch, adjust the temperature at 170-220°C for pyrolysis reaction; (3) obtain crude pyrodextrin after the pyrolysis reaction is completed, and It is refined to obtain resistant dextrin products. The added amount of the acid is 0.02-0.2% of the mass in the starch.

发明内容 Contents of the invention

本发明针对现有技术的不足,提供一种通过提高酸度制备高纯度抗性糊精的方法。该技术方法节省了淀粉预处理步骤,降低了热解反应温度,缩短了热解反应时间,降低了生成成本,且产品纯度大于90%,热稳定性强,低热量低血糖指数。 The invention aims at the deficiencies of the prior art, and provides a method for preparing high-purity resistant dextrin by increasing the acidity. The technical method saves the starch pretreatment step, reduces the pyrolysis reaction temperature, shortens the pyrolysis reaction time, and reduces the production cost, and the product has a purity greater than 90%, strong thermal stability, low calorie and low glycemic index.

本发明的技术方法是一种通过提高酸度制备高纯度抗性糊精的方法,包括如下步骤: The technical method of the present invention is a method for preparing high-purity resistant dextrin by increasing acidity, comprising the following steps:

(1)在玉米淀粉中均匀喷洒适量的酸,搅拌均匀,静置30-60min,制得淀粉酸处理样品。 (1) Spray an appropriate amount of acid evenly in cornstarch, stir evenly, and let it stand for 30-60min to prepare starch acid-treated samples.

(2)将步骤(1)制得的淀粉酸处理样品,在一定温度下进行热解反应。 (2) The starch acid-treated sample prepared in step (1) is subjected to pyrolysis reaction at a certain temperature.

(3)热解反应结束后制得抗性糊精粗品,将其精制得到抗性糊精纯品。 (3) After the pyrolysis reaction, the crude resistant dextrin is obtained, which is refined to obtain the pure resistant dextrin.

(4)步骤(1)中所述的酸优选为盐酸、硫酸和柠檬酸中的一种。 (4) The acid described in step (1) is preferably one of hydrochloric acid, sulfuric acid and citric acid.

(5)步骤(1)中,所述的酸浓度优选为为1-4%。 (5) In step (1), the acid concentration is preferably 1-4%.

(6)步骤(1)中,酸的添加量优选为5-15%。 (6) In step (1), the amount of acid added is preferably 5-15%.

(7)步骤(2)中,热解温度优选为110-180℃。 (7) In step (2), the pyrolysis temperature is preferably 110-180°C.

(8)步骤(2)中,热解反应的时间优选为0.5-3h。 (8) In step (2), the pyrolysis reaction time is preferably 0.5-3h.

(9)步骤(3)精制过程中:现将抗性糊精粗产品加水溶解,使其质量分数为20-40%,然后使用高温α淀粉酶、复合糖化酶(葡萄糖淀粉酶与普鲁兰酶)进行酶解,每吨干淀粉耐高温α-淀粉酶添加量优选为2×107-4×107U,复合糖化酶添加量优选为1×107-2×107U,活性炭添加量优选为淀粉总干基的2%-6%,脱色温度为60-80℃,脱色时间为30-70min,离子交换树脂优选为酸性阳树脂D001和碱性阴树脂D330按照1:1组成混合床树脂,然后进行色谱、浓缩,喷雾干燥得到抗性糊精产品。 (9) During the refining process of step (3): Now dissolve the crude resistant dextrin product in water so that its mass fraction is 20-40%, and then use high-temperature α-amylase, compound glucoamylase (glucoamylase and pullulan enzyme) for enzymolysis, the amount of high temperature resistant α-amylase per ton of dry starch is preferably 2×10 7 -4×10 7 U, the amount of compound glucoamylase is preferably 1×10 7 -2×10 7 U, activated carbon The added amount is preferably 2%-6% of the total dry basis of starch, the decolorization temperature is 60-80°C, and the decolorization time is 30-70min. The ion exchange resin is preferably composed of acidic cation resin D001 and basic anion resin D330 at a ratio of 1:1. The mixed bed resin is then chromatographed, concentrated, and spray dried to obtain the resistant dextrin product.

本发明的优良效果具体如下: Excellent effect of the present invention is specifically as follows:

1、在传统工艺基础上,通过提高淀粉中的酸度,降低了热解反应温度,缩短了热解反应时间,降低了生产成本; 1. On the basis of traditional technology, by increasing the acidity in starch, the pyrolysis reaction temperature is reduced, the pyrolysis reaction time is shortened, and the production cost is reduced;

2、本发明操作节省了原有工艺的淀粉预处理步骤,副反应产物减少,制备的抗性糊精产品纯度提高,热稳定性强,低热量低血糖指数。 2. The operation of the present invention saves the starch pretreatment step of the original process, reduces side reaction products, improves the purity of the prepared resistant dextrin product, has strong thermal stability, low calorie and low glycemic index.

具体实施方式 detailed description

为了更好的理解本发明的内容,一下结合实例作进一步说明。 In order to better understand the content of the present invention, it will be further described below in conjunction with examples.

酶试剂来源: Enzyme reagent source:

耐高温α-淀粉酶诺维信公司酶活为20000U/ml High temperature resistant α-amylase Novozymes company enzyme activity is 20000U/ml

复合糖化酶诺维信公司酶活为20000U/ml The enzyme activity of compound glucoamylase from Novozymes is 20000U/ml

实施例1Example 1

一种通过提高酸度制备高纯度抗性糊精的方法,包括步骤如下: A method for preparing high-purity resistant dextrin by increasing acidity, comprising the following steps:

(1)在玉米淀粉中均匀喷洒盐酸,酸浓度为1%,添加量为干淀粉总量的15%,搅拌均匀,静置30min,制得淀粉酸处理样品; (1) Spray hydrochloric acid evenly in the cornstarch, the acid concentration is 1%, and the added amount is 15% of the total amount of dry starch, stir evenly, and let it stand for 30 minutes to prepare starch acid treated samples;

(2)将步骤(1)制得的淀粉酸处理样品,在180℃下进行热解反应,热解时间为0.5h; (2) The starch acid-treated sample prepared in step (1) was subjected to pyrolysis reaction at 180°C, and the pyrolysis time was 0.5h;

(3)抗性糊精粗产品加水溶解,使其质量分数为20%,然后使用高温α-淀粉酶、复合糖化酶(葡萄糖淀粉酶与普鲁兰酶)进行酶解。每吨干淀粉耐高温α-淀粉酶添加量优选为2×107U,复合糖化酶添加量优选为1×107U。活性炭添加量优选为淀粉总干基的2%,脱色温度为60℃,脱色时间为30min。离子交换树脂优选为酸性阳树脂D001和碱性阴树脂D330按照1:1组成混合床树脂。然后进行色谱、浓缩,喷雾干燥得到抗性糊精产品,检测得到抗性糊精产品纯度为91.7%。 (3) The crude product of resistant dextrin was dissolved in water to make its mass fraction 20%, and then it was hydrolyzed by high-temperature α-amylase and compound glucoamylase (glucoamylase and pullulanase). The added amount of high temperature resistant α-amylase per ton of dry starch is preferably 2×10 7 U, and the added amount of compound glucoamylase is preferably 1×10 7 U. The amount of activated carbon added is preferably 2% of the total dry basis of starch, the decolorization temperature is 60°C, and the decolorization time is 30min. The ion exchange resin is preferably a mixed bed resin composed of acidic cation resin D001 and basic anion resin D330 according to the composition of 1:1. Then chromatographic, concentrated, and spray-dried to obtain a resistant dextrin product, which was detected to have a purity of 91.7%.

实施例2Example 2

一种通过提高酸度制备高纯度抗性糊精的方法,包括步骤如下: A method for preparing high-purity resistant dextrin by increasing acidity, comprising the following steps:

(1)在玉米淀粉中均匀喷洒硫酸,酸浓度为4%,添加量为干淀粉总量的5%,搅拌均匀,静置60min,制得淀粉酸处理样品; (1) Spray sulfuric acid evenly in the cornstarch, the acid concentration is 4%, the added amount is 5% of the total amount of dry starch, stir evenly, and let it stand for 60 minutes to prepare starch acid treated samples;

(2)将步骤(1)制得的淀粉酸处理样品,在110℃下进行热解反应,热解反应时间为3h; (2) The starch acid-treated sample prepared in step (1) was subjected to pyrolysis reaction at 110°C, and the pyrolysis reaction time was 3 hours;

(3)抗性糊精粗产品加水溶解,使其质量分数为40%,然后使用高温α-淀粉酶、复合糖化酶(葡萄糖淀粉酶与普鲁兰酶)进行酶解。每吨干淀粉耐高温α-淀粉酶添加量优选为4×107U,复合糖化酶添加量优选为2×107U。活性炭添加量优选为淀粉总干基的6%,脱色温度为80℃,脱色时间为60min。离子交换树脂优选为酸性阳树脂D001和碱性阴树脂D330按照1:1组成混合床树脂。然后进行色谱、浓缩,喷雾干燥得到抗性糊精产品,检测得到抗性糊精产品纯度为96.3%。 (3) The crude product of resistant dextrin was dissolved in water to make its mass fraction 40%, and then it was hydrolyzed by high-temperature α-amylase and compound glucoamylase (glucoamylase and pullulanase). The added amount of high temperature-resistant α-amylase per ton of dry starch is preferably 4×10 7 U, and the added amount of compound glucoamylase is preferably 2×10 7 U. The amount of activated carbon added is preferably 6% of the total dry basis of starch, the decolorization temperature is 80°C, and the decolorization time is 60min. The ion exchange resin is preferably a mixed bed resin composed of acidic cation resin D001 and basic anion resin D330 according to the composition of 1:1. Then carry out chromatography, concentrate, and spray dry to obtain the resistant dextrin product, and the purity of the resistant dextrin product obtained by detection is 96.3%.

实施例3Example 3

一种通过提高酸度制备高纯度抗性糊精的方法,包括步骤如下: A method for preparing high-purity resistant dextrin by increasing acidity, comprising the following steps:

(1)在玉米淀粉中均匀喷洒柠檬酸,酸浓度为2.5%,添加量为干淀粉总量的8%,搅拌均匀,静置45min,制得淀粉酸处理样品; (1) Spray citric acid evenly in the cornstarch, the acid concentration is 2.5%, the added amount is 8% of the total amount of dry starch, stir evenly, and let it stand for 45min to prepare starch acid treated samples;

(2)将步骤(1)制得的淀粉酸处理样品,在140℃下进行热解反应,热解反应时间为2h; (2) The starch acid-treated sample prepared in step (1) was subjected to a pyrolysis reaction at 140°C, and the pyrolysis reaction time was 2 hours;

(3)抗性糊精粗产品加水溶解,使其质量分数为30%,然后使用高温α-淀粉酶、复合糖化酶(葡萄糖淀粉酶与普鲁兰酶)进行酶解。每吨干淀粉耐高温α-淀粉酶添加量优选为3×107U,复合糖化酶添加量优选为1.5×107U。活性炭添加量优选为淀粉总干基的4%,脱色温度为70℃,脱色时间为50min。离子交换树脂优选为酸性阳树脂D001和碱性阴树脂D330按照1:1组成混合床树脂。然后进行色谱、浓缩,喷雾干燥得到抗性糊精产品,检测得到抗性糊精产品纯度为93.1%。 (3) The crude resistant dextrin product was dissolved in water to make its mass fraction 30%, and then it was hydrolyzed by high-temperature α-amylase and compound glucoamylase (glucoamylase and pullulanase). The added amount of high temperature-resistant α-amylase per ton of dry starch is preferably 3×10 7 U, and the added amount of compound glucoamylase is preferably 1.5×10 7 U. The amount of activated carbon added is preferably 4% of the total dry basis of starch, the decolorization temperature is 70°C, and the decolorization time is 50min. The ion exchange resin is preferably a mixed bed resin composed of acidic cation resin D001 and basic anion resin D330 according to the composition of 1:1. Then chromatographic, concentrated, and spray-dried to obtain a resistant dextrin product, which was detected to have a purity of 93.1%.

Claims (7)

1.一种通过提高酸度制备高纯度抗性糊精的方法,其特征在于,包括如下步骤: 1. a method for preparing high-purity resistant dextrin by improving acidity, is characterized in that, comprises the steps: (1)在玉米淀粉中均匀喷洒适量的酸,搅拌均匀,静置30-60min,制得淀粉酸处理样品; (1) Spray an appropriate amount of acid evenly in cornstarch, stir evenly, and let it stand for 30-60min to prepare starch acid treated samples; (2)将步骤(1)制得的淀粉酸处理样品,在一定温度下进行热解反应; (2) The starch acid-treated sample prepared in step (1) is subjected to a pyrolysis reaction at a certain temperature; (3)热解反应结束后制得抗性糊精粗品,将其精制得到抗性糊精纯品。 (3) After the pyrolysis reaction, the crude resistant dextrin is obtained, which is refined to obtain the pure resistant dextrin. 2.根据权利要求1所述的方法,其特征在于,所述步骤(1)中,所述的酸为盐酸、硫酸和柠檬酸中的一种。 2. The method according to claim 1, characterized in that, in the step (1), the acid is one of hydrochloric acid, sulfuric acid and citric acid. 3.根据权利要求1所述的方法,其特征在于,所述步骤(1)中,所述的酸浓度为1-4%。 3. The method according to claim 1, characterized in that, in the step (1), the acid concentration is 1-4%. 4.根据权利要求1所述的方法,其特征在于,所述步骤(1)中,酸的添加量为5-15%。 4. The method according to claim 1, characterized in that, in the step (1), the amount of acid added is 5-15%. 5.根据权利要求1所述的方法,其特征在于,所述步骤(2)中,热解温度为110-180℃。 5. The method according to claim 1, characterized in that, in the step (2), the pyrolysis temperature is 110-180°C. 6.根据权利要求1所述的方法,其特征在于,所述步骤(2)中,热解反应的时间为0.5-3h。 6. The method according to claim 1, characterized in that, in the step (2), the pyrolysis reaction time is 0.5-3h. 7.根据权利要求1所述的方法,其特征在于,所述步骤(3)中,抗性糊精粗品精制包括酶解、脱色、离交、色谱、浓缩,最后经过喷雾干燥得到抗性糊精产品。 7. The method according to claim 1, characterized in that in the step (3), the refining of the resistant dextrin crude product includes enzymatic hydrolysis, decolorization, separation, chromatography, concentration, and finally spray drying to obtain the resistant dextrin Refined products.
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CN105542019A (en) * 2016-01-27 2016-05-04 山东百龙创园生物科技有限公司 Resistant dextrin and preparation method thereof
CN105542019B (en) * 2016-01-27 2017-08-18 山东百龙创园生物科技股份有限公司 Resistant dextrin and preparation method thereof
CN105693871A (en) * 2016-03-10 2016-06-22 翁源广业清怡食品科技有限公司 Preparation method of resistant dextrin
CN105693871B (en) * 2016-03-10 2018-08-07 翁源广业清怡食品科技有限公司 A kind of preparation method of resistant dextrin
CN106173962A (en) * 2016-06-27 2016-12-07 郑州国食科技有限公司 A kind of preparation method containing resistant dextrin huyashi-chuuka (cold chinese-style noodles)
CN106755203A (en) * 2016-11-28 2017-05-31 保龄宝生物股份有限公司 A kind of preparation method of resistant dextrin
CN108503716A (en) * 2018-04-10 2018-09-07 陈磊 A kind of production method of resistant dextrin
CN108503716B (en) * 2018-04-10 2019-02-22 陈磊 A kind of production method of resistant dextrin
CN110724718A (en) * 2019-12-02 2020-01-24 保龄宝生物股份有限公司 Method for preparing resistant dextrin by using microwaves
CN112725312A (en) * 2021-01-25 2021-04-30 浙江大学 Preparation method of complex enzyme and resistant dextrin
CN115323015A (en) * 2022-08-29 2022-11-11 山东星光首创生物科技有限公司 A kind of method that utilizes infrared rays to prepare resistant dextrin

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