WO2016041219A1 - 一种糊精的分级方法 - Google Patents

一种糊精的分级方法 Download PDF

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WO2016041219A1
WO2016041219A1 PCT/CN2014/087501 CN2014087501W WO2016041219A1 WO 2016041219 A1 WO2016041219 A1 WO 2016041219A1 CN 2014087501 W CN2014087501 W CN 2014087501W WO 2016041219 A1 WO2016041219 A1 WO 2016041219A1
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dextrin
polyethylene glycol
solution
added
molecular weight
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French (fr)
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金征宇
田耀旗
胡秀婷
孙冰华
章宝
魏本喜
吴春森
杨哪
徐学明
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Jiangnan University
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Jiangnan University
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    • 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
    • C08B30/12—Degraded, destructured or non-chemically modified starch, e.g. mechanically, enzymatically or by irradiation; Bleaching of starch
    • C08B30/18—Dextrin, e.g. yellow canari, white dextrin, amylodextrin or maltodextrin; Methods of depolymerisation, e.g. by irradiation or mechanically

Definitions

  • the invention relates to a method for classifying dextrin, which relates to the application of polyethylene glycol stepwise precipitation technology in the classification of dextrin, and belongs to the technical field of food processing.
  • the methods of grading dextrin mainly include exclusion chromatography fractionation and alcohol precipitation fractionation.
  • the former is expensive due to the high price of the filler and the high price of the chromatographic power system, that is, the pump; in addition, the chromatographic classification method has a small processing amount, and it is difficult to achieve industrial production.
  • the alcohol precipitation fractionation method has the following disadvantages: the co-precipitation phenomenon occurs locally during the addition of alcohol, resulting in poor classification effect; the total volume expansion of the dextrin solution during the addition of alcohol causes the dextrin concentration to decrease, resulting in dextrin The rate is low; and the classification process is extremely sensitive to ambient temperature and therefore has poor repeatability.
  • the present invention is directed to a new method of grading dextrin, thereby providing a novel method of preparing low dispersibility dextrin.
  • the present inventors have found that dextrin and polyethylene glycol are incompatible in aqueous solution, and the greater the molecular weight of dextrin, the more incompatible with polyethylene glycol. Therefore, the polyethylene glycol is gradually added to the aqueous dextrin solution, so that the concentration of the polyethylene glycol is gradually increased, and the dextrin having a large molecular weight can be precipitated step by step. Based on the above phenomenon, the present invention establishes a new method of grading of dextrin, and is named "polyethylene glycol stepwise precipitation fractionation method of dextrin".
  • the technical scheme of the invention a method for grading dextrin, using a stepwise precipitation technique of polyethylene glycol to classify dextrin, the process is:
  • Dissolution of dextrin solution Weigh 15-25g of tapioca starch and disperse it in 100mL of n-butanol, add 1mL of concentrated hydrochloric acid, hydrolyze at 40 °C for 3d, add 14mL of 1M NaNO 3 to terminate the reaction, centrifuge at 4000g for 15min, precipitate with 50 The % ethanol solution was washed several times to a chloride-free ion, dried in an oven at 40 ° C for 24 hours, pulverized, and sieved to obtain a dextrin. The dextrin was dissolved in distilled water and a dextrin solution of 0.9% to 3.6% was placed.
  • polyethylene glycol stepwise precipitation classification take 100mL mass concentration of 0.9% -3.6% dextrin solution, add 5g polyethylene glycol, heated and stirred until the polyethylene glycol dissolved solution is clarified, naturally cooled to 25 in the air °C, placed in a 25 ° C water bath for 24h, if precipitation occurs, centrifuged at 4000g for 15min, the resulting precipitate was washed with chloroform to remove residual polyethylene glycol, dried at 40 ° C for 24h, crushed, sieved to obtain graded Dextrin component 1, the supernatant is further added with 5 g of polyethylene glycol to repeat the above process to obtain a graded dextrin component 2; if no precipitation occurs, continue to add 5 g of polyethylene glycol to the precipitate; repeat the above process until The total amount of polyethylene glycol added is 60g, thus obtaining 9-12 graded dextrin groups. Minute.
  • the polyethylene glycol is a polyethylene glycol having a number average molecular weight of 4000 Da, 6000 Da or 8000 Da.
  • the invention has the beneficial effects that the invention has the advantages of simple production process, low cost, high yield, large processing amount and good classification effect, compared with the prior art.
  • the molecular weight information of 11 dextrin components is as follows: dextrin 1 (when polyethylene glycol is added 5g), the weight average molecular weight is 2.380 ⁇ 10 4 Da, the dispersion coefficient is 1.38; the weight average molecular weight of dextrin 2 (when polyethylene glycol is added 10g) is 2.1660 ⁇ 10 4 Da, the dispersion coefficient is 1.13; the weight average molecular weight of dextrin 3 (when polyethylene glycol is added 15g) It is 2.011 ⁇ 10 4 Da, the dispersion coefficient is 1.16; the weight average molecular weight of dextrin 4 (when polyethylene glycol is added 20g) is 1.879 ⁇ 10 4 Da, the dispersion coefficient is 1.21, and dextrin 5 (when polyethylene glycol is added 25g) The weight average molecular weight is 1.329 ⁇ 10 4 Da, the dispersion coefficient is 1.13;
  • the molecular weight information of 9 dextrin components is as follows: Dextrin 1 (when polyethylene glycol is added 15g), the weight average molecular weight is 3.297 ⁇ 10 4 Da, the dispersion coefficient is 1.34; the weight average molecular weight of dextrin 2 (when polyethylene glycol is added 20g) is 1.141 ⁇ 10 4 Da, the dispersion coefficient is 1.17; the weight average molecular weight of dextrin 3 (when polyethylene glycol is added 25g) It is 9.235 ⁇ 10 3 Da, the dispersion coefficient is 1.24; the weight average molecular weight of dextrin 4 (when polyethylene glycol is added 30g) is 1.066 ⁇ 10 4 Da, the dispersion coefficient is 1.09; dextrin 5 (when polyethylene glycol is added 40g) The weight average molecular weight is 9.386 ⁇ 10 3 Da, the dispersion coefficient is 1.17; the

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)

Abstract

一种糊精的分级方法，属于食品加工技术领域。本发明原理基于淀粉降解产物—糊精与聚乙二醇在水溶液中具有不相容性，且糊精分子量愈大与聚乙二醇不相容性愈显著，因此，向糊精水溶液中逐步加入聚乙二醇，使得聚乙二醇浓度逐步提高，可实现逐级沉淀出分子量由大到小的糊精组分。步骤为配置糊精溶液和糊精分级，以木薯淀粉为原料，经正丁醇-盐酸于40℃下降解3d，得湖精，溶于蒸馏水制备0.9％-3.6％的糊精溶液100mL，添加5g聚乙二醇，加热搅拌至溶液澄清在空气中冷却至25℃，在25℃下保持24h，离心，烘箱干燥、粉碎即得分级组分1；上清液继续添加5g聚乙二醇重复上述过程，得分级组分2；重复上述过程至聚乙二醇添加量为60g为止，得9-11个糊精组分。

Description

一种糊精的分级方法 技术领域
一种糊精的分级方法，涉及聚乙二醇逐步沉淀技术在糊精分级上的应用，属于食品加工技术领域。
背景技术
目前，糊精分级的方法主要有排阻色谱分级法和醇沉淀分级法。前者由于填料价格昂贵、色谱动力系统即泵价格高导致此法成本高；此外，色谱分级法处理量小，难以实现工业化生产。而醇沉淀分级法存在如下缺点：在添加醇过程中局部易发生共沉现象而导致分级效果不佳；在醇的添加过程中糊精溶液总体积扩增引起糊精浓度下降，导致糊精得率低；且分级过程对环境温度极其敏感，因而重复性较差。
因此，本发明旨在提供糊精分级的新方法，从而提供低分散性糊精的制备新方法。本发明发现糊精和聚乙二醇在水溶液中存在不相容性，并且糊精分子量越大，与聚乙二醇的不相容性越显著。因此，向糊精水溶液中逐步加入聚乙二醇，使得聚乙二醇浓度逐步增高，可以逐级沉淀出分子量由大到小的糊精。基于上述现象，本发明建立了糊精分级的新方法，并且命名为“糊精的聚乙二醇逐步沉淀分级法”。
发明内容
本发明的目的是提供一种糊精的分级方法。
本发明的技术方案：一种糊精的分级方法，利用聚乙二醇逐步沉淀技术分级糊精，工艺为：
1、糊精溶液的配置：称取15-25g木薯淀粉分散于100mL正丁醇中，加入1mL浓盐酸，于40℃下水解3d，加入14mL 1M NaNO3终止反应，4000g离心15min，沉淀用50％乙醇溶液洗涤数次至无氯离子，40℃烘箱干燥24h，粉碎，过筛，得糊精。将糊精溶于蒸馏水中，配置0.9％-3.6％的糊精溶液。
2、聚乙二醇逐步沉淀分级：取100mL质量浓度0.9％-3.6％的糊精溶液，加入5g聚乙二醇，加热搅拌直到聚乙二醇溶解即溶液澄清，在空气中自然冷却到25℃，置于25℃水浴锅维持24h，若出现沉淀，则4000g下离心15min，得到的沉淀物用三氯甲烷洗涤除去残留的聚乙二醇，40℃干燥24h，粉碎、过筛得到分级的糊精组分1，上清液继续添加5g聚乙二醇重复上述过程，得到分级的糊精组分2；若没有出现沉淀，则继续添加5g聚乙二醇至沉淀产生；重复上述过程至聚乙二醇总添加量为60g为止，如此得到9-12个分级的糊精组 分。
3、糊精分散性鉴定：采用高效排阻色谱联合多角度激光检测器和示差检测器对糊精组分分析，计算糊精的分子量和分散系数。
所述聚乙二醇为数均分子量为4000Da、6000Da或者8000Da的聚乙二醇。
本发明的有益效果：与现有技术相比，本发明具有生产工艺简单、成本低、得率高、处理量大、分级效果好等有益效果。
具体实施方式
实施例1
称取25g木薯淀粉分散于100mL正丁醇(分析纯)中，加入1mL浓盐酸(分析纯)，于40℃下水解72h，加入14mL 1M NaNO3终止反应，于4000g下离心15min，沉淀用50％乙醇溶液洗涤数次至无氯离子，40℃烘箱干燥24h，得糊精。将糊精溶于蒸馏水，配置成3.6％的糊精溶液。取100mL糊精溶液，加入5g数均分子量8000Da的聚乙二醇(化学纯)，加热搅拌直到聚乙二醇溶解即溶液澄清，在空气中自然冷却到25℃，置于25℃水浴锅24h，于4000g下离心15min，得到的浓相用三氯甲烷洗涤除去残留的聚乙二醇，40℃干燥24h，粉碎、干燥得到分级的糊精组分1；上清液继续加入5g聚乙二醇，重复上述过程至聚乙二醇添加量为60g停止，得到11个分级的糊精组分。采用高效排阻色谱联合多角度激光检测器和示差检测器对糊精产品分析，11个糊精组分分子量信息如下：糊精1(聚乙二醇添加5g时)重均分子量为2.380×104Da，分散系数为1.38；糊精2(聚乙二醇添加10g时)重均分子量为2.1660×104Da，分散系数为1.13；糊精3(聚乙二醇添加15g时)重均分子量为2.011×104Da，分散系数为1.16；糊精4(聚乙二醇添加20g时)重均分子量为1.879×104Da，分散系数为1.21，糊精5(聚乙二醇添加25g时)重均分子量为1.329×104Da，分散系数为1.13；糊精6(聚乙二醇添加30g时)重均分子量为1.281×104Da，分散系数为1.18；糊精7(聚乙二醇添加35g时)重均分子量为8.029×103Da，分散系数为1.19；糊精8(聚乙二醇添加40g时)重均分子量为6.081×103Da，分散系数为1.17；糊精9(聚乙二醇添加45g时)重均分子量为5.584×103Da，分散系数为1.17；糊精10(聚乙二醇添加50g时)重均分子量为5.561×103Da，分散系数为1.21；糊精11(聚乙二醇添加60g时)重均分子量为5.443×103Da，分散系数为1.38。
实施例2
称取15g木薯淀粉分散于100mL正丁醇(分析纯)中，加入1mL浓盐酸(分析纯)，于40℃下水解72h，加入14mL 1M NaNO3终止反应，于4000g下离心15min，沉淀用50％乙醇 溶液洗涤数次至无氯离子，40℃烘箱干燥24h，得糊精。将糊精加热溶于蒸馏水，配置成0.9％的溶液。取100mL糊精溶液，加入5g数均分子量为4000Da(化学纯)的聚乙二醇，加热搅拌直到聚乙二醇溶解即溶液澄清，在空气中冷却到25℃，置于25℃水浴锅24h，于4000g下离心15min，得到的沉淀物用三氯甲烷洗涤除去残留的聚乙二醇，40℃干燥24h，粉碎、干燥得到分级的糊精组分1；上清液继续加入5g聚乙二醇，重复上述过程，至聚乙二醇添加量为60g停止，如此得到9个分级的糊精组分。采用高效排阻色谱联合多角度激光检测器和示差检测器对糊精产品分析，9个糊精组分分子量信息如下：糊精1(聚乙二醇添加15g时)重均分子量为3.297×104Da，分散系数为1.34；糊精2(聚乙二醇添加20g时)重均分子量为1.141×104Da，分散系数为1.17；糊精3(聚乙二醇添加25g时)重均分子量为9.235×103Da，分散系数为1.24；糊精4(聚乙二醇添加30g时)重均分子量为1.066×104Da，分散系数为1.09；糊精5(聚乙二醇添加40g时)重均分子量为9.386×103Da，分散系数为1.17；糊精6(聚乙二醇添加45g时)重均分子量为8.992×103Da，分散系数为1.18；糊精7(聚乙二醇添加50g时)重均分子量为7.987×103Da，分散系数为1.28；糊精8(聚乙二醇添加55g时)重均分子量为7.786×103Da，分散系数为1.15；糊精9(聚乙二醇添加60g时)重均分子量为6.381×103Da，分散系数为1.47。

Claims (3)

  1. 一种糊精的分级方法，其特征在于包括配置糊精溶液和糊精分级步骤，糊精分级采用聚乙二醇逐步沉淀法，具体操作如下：取糊精质量浓度为0.9％-3.6％的糊精溶液100mL、加入5g聚乙二醇，加热搅拌直到聚乙二醇溶解即溶液澄清，在空气中自然冷却到25℃，置于25℃水浴锅维持24h，若出现沉淀，则4000g下离心15min，得到的沉淀物用三氯甲烷洗涤除去残留的聚乙二醇，40℃干燥24h，粉碎、过筛得到分级的糊精组分1，上清液继续添加5g聚乙二醇重复上述过程，得到分级的糊精组分2；若没有出现沉淀，则继续添加5g聚乙二醇至沉淀产生；重复上述过程至聚乙二醇总添加量为60g为止，如此得到9-11个分级的糊精组分。
  2. 根据权利要求1所述的糊精的分级方法，其特征在于：所述糊精通过淀粉的醇酸降解得到，即称取15-25g木薯淀粉分散于100mL正丁醇中，加入1mL浓盐酸，于40℃下水解3d，加入14mL、1M NaNO3终止反应，4000g离心15min，沉淀用50％乙醇溶液洗涤数次至无氯离子，40℃烘箱干燥，粉碎，过筛，得糊精。
  3. 根据权利要求1所述的糊精的分级方法，其特征在于：使用的聚乙二醇数均分子量为4000Da、6000Da或8000Da。
PCT/CN2014/087501 2014-09-17 2014-09-26 一种糊精的分级方法 Ceased WO2016041219A1 (zh)

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CN105418772B (zh) * 2015-10-23 2017-09-22 南昌大学 一种分级糊精的方法
CN105348394B (zh) * 2015-11-20 2017-07-18 江苏焦点农业科技有限公司 一种玉米淀粉3级颗粒的纯化方法
CN107950998A (zh) * 2017-12-20 2018-04-24 阮小军 改善血液循环的纳豆激酶组合物及其加工方法
CN109265570A (zh) * 2018-10-10 2019-01-25 南昌大学 一种高效制备淀粉纳米晶的方法
WO2021077380A1 (zh) * 2019-10-25 2021-04-29 合肥工业大学 双功能型淀粉基复合纳米颗粒及其制备方法与应用
CN111329022A (zh) * 2020-02-28 2020-06-26 西昌市正中食品有限公司 一种速溶苦荞营养粉
CN112439538B (zh) * 2020-10-16 2022-08-05 中南林业科技大学 一种不同粒度淀粉的分离方法
CN118063632B (zh) * 2023-11-29 2025-04-01 江南大学 一种麦芽糊精的制备方法

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