CN103030712B - 一种魔芋葡甘露低聚糖的制备方法 - Google Patents

一种魔芋葡甘露低聚糖的制备方法 Download PDF

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CN103030712B
CN103030712B CN201210415241.3A CN201210415241A CN103030712B CN 103030712 B CN103030712 B CN 103030712B CN 201210415241 A CN201210415241 A CN 201210415241A CN 103030712 B CN103030712 B CN 103030712B
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konjac mannan
mannan oligosaccharide
konjaku
oligosaccharide
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CN103030712A (zh
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张郁
胡开群
李章贵
汪超
李红斌
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Zhang Yu
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Abstract

本发明公开了一种魔芋葡甘露低聚糖的制备方法。该方法特征在于将魔芋精粉放入浓度为70%～95%（V/V）二甲基亚砜溶液容器中，经不同频率超声波超声60min～90min后，取出，过滤，得滤渣按1:5～1:10（M/V）无水乙醇反复沉淀过滤3～5次后，干燥，即可得到分子量相对均一的魔芋葡甘露低聚糖，所得产物保持了魔芋葡甘聚糖的化学结构。本发明方法工艺设备简单，易于操作，可用于批量魔芋葡甘露低聚糖的生产，所得产物应用广泛。

Description

一种魔芋葡甘露低聚糖的制备方法
技术领域
本发明属于天然高分子化学领域，具体涉及一种魔芋葡甘露低聚糖的制备方法。
背景技术
魔芋葡甘聚糖是天南星科草本块茎植物魔芋的主要成分，由D-葡萄糖与D-甘露糖按1:1.6的比例以β-1,4-糖苷键连接的杂多糖，主链D-甘露糖C3位上有β-1,3-糖苷键连接的支链，每19个糖残基C6位上连有乙酰基。其溶胶粘度大，被应用于食品、包装、涂料、生物医药及化妆等领域。魔芋葡甘聚糖分子量可达百万道尔顿，高分子量一方面使其具有优良的增稠、胶凝性，另一方面也限制其应用范围。将魔芋葡甘聚糖降解，所得魔芋葡甘露低聚糖极大扩展其应用领域。
魔芋葡甘露低聚糖是魔芋葡甘聚糖降解后的产物。根据动物实验和临床研究表明，魔芋葡甘露低聚糖对促进双歧杆菌生长非常有效。并能改善肠道菌群结构，而且其性能及效果优于乳果糖、大豆低聚糖及半乳糖及转移低聚糖。同时还具有防治高血脂、降血脂、抗氧化、增强免疫功能等作用。目前多糖的降解方法主要有化学法（黄永春，谢清若，何仁，陈燕，微波辅助H2O2降解魔芋葡甘聚糖的研究，食品科学，2005，8：197-199）、物理法（徐振林，孙远明，丁金龙，魔芋葡甘聚糖的辐照降解研究，农产品加工，2006，10：27-29）和酶法（陶兴无，杨海娇，余勇，付维来，β-葡聚糖酶分级降解魔芋葡甘聚糖工艺研究，食品工业科技，2006，10:139-141）。二甲基亚砜溶剂超声法是通过超声波的“空穴效应”产生能量而达到加速氢键破坏剂作用，得到分子量相对均一的魔芋葡甘低聚糖，可扩大再生资源魔芋葡甘聚糖的应用范围。
发明内容
本发明的目的就是针对上述特点而提出的一种以二甲基亚砜为媒介溶剂超声降解魔芋粉来获得魔芋葡甘露低聚糖的一种魔芋葡甘露低聚糖的制备方法。获得的魔芋葡甘露低聚糖粘度小、水溶性好，并保持了魔芋葡甘聚糖的化学结构。
为了实现上述目的，一种魔芋葡甘露低聚糖的制备方法，其不同之处在于：所述魔芋葡甘露低聚糖是将魔芋粉放入二甲基亚砜溶液中超声降解所得。
按以上方案，所述制备方法的具体步骤为：将魔芋粉放入盛有浓度为70%～95%（V/V）二甲基亚砜溶液的容器中，经40KHz～80KHz的超声波超声60min～90min后取出过滤，将得到的滤渣用无水乙醇反复沉淀过滤3～5次后干燥，即可得到分子量均一的魔芋葡甘露低聚糖，所得产物保持了魔芋葡甘聚糖的化学结构。
按以上方案，所述滤渣与无水乙醇的重量比为1:10～1:50（M/V）。
本发明所得的魔芋葡甘露低聚糖为白色或类白色粉末，易溶于水，粘度较魔芋精粉明显降低。本发明制备魔芋葡甘露低聚糖的方法与现有方法相比，该法制备的魔芋葡甘露低聚糖分子量均一，工艺简单，溶剂可循环利用等优点，产物收率为80%-90%。
附图说明
图1为本发明魔芋葡甘露低聚糖和原料魔芋精分的FT-IR对比图；
图2为本发明实施例1中GPC-LS-RI分析魔芋葡甘露低聚糖在水溶液中光谱图；
图 3为本发明实施例2中 GPC-LS-RI分析魔芋葡甘露低聚糖在水溶液中光谱图；
图4为本发明实施例3中GPC-LS-RI分析魔芋葡甘露低聚糖在水溶液中光谱图。
具体实施方式
结合附图和实施例对本发明做进一步说明。
魔芋葡甘露低聚糖的分子量的测定方法如下：取本发明所得的魔芋葡甘露低聚糖。将样品溶于0.1M NaNO3溶液，样品浓度1×10-3g/mL，采用激光光散射仪(LS-GPC联用)分析。分析条件：Shodex-G805、G806凝胶柱，示差检测器(Optilab rEX)，波长658nm，温度25℃，流动相0.1M NaNO3溶液，流速1.0mL/min，进样量20μL。数据处理软件ASTRA5.3.2.7(Wyatt Technology Corporation，America)。
参见图1，D-KGM表示魔芋低聚糖，KGM表示原料魔芋粉。图中1734cm-1乙酰基团的羰基吸收峰未消失，说明魔芋葡甘露低聚糖保持了魔芋葡甘聚糖的结构，因而也保留了其化学特性。
实施例1
一种魔芋葡甘露低聚糖的制备方法，其步骤是：取市售魔芋粉放入浓度为95%（V/V）二甲基亚砜溶液容器中，经频率为80KHz超声波超声60min后，取出，过滤，得滤渣按1:50（M/V）乙醇反复沉淀过滤5次后，干燥，即可得到分子量均一的魔芋葡甘露低聚糖，所得产物保持了魔芋葡甘聚糖的化学结构，见图1。参见图2，本发明方法中制备的魔芋葡甘聚糖精粉经GPC-LS测定，产物收率为90%，其重均分子量为2.747×104，其相对分子量分布图近似正态分布，峰宽较窄，可见魔芋葡甘露低聚糖分子大小分布相对集中，为相对均一的低聚糖。
实施例2
一种魔芋葡甘露低聚糖的制备方法，其步骤是：取市售魔芋粉放入浓度为80%（V/V）二甲基亚砜溶液容器中，经频率为60KHz超声波超声30min后，取出，过滤，得滤渣按1:25（M/V）乙醇反复沉淀过滤4次后，干燥，即可得到分子量均一的魔芋葡甘露低聚糖，所得产物保持了魔芋葡甘聚糖的化学结构，见图1。参见图3，本发明方法中制备的魔芋葡甘聚糖精粉经GPC-LS测定，产物收率为80%，其重均分子量为4.181×105，其相对分子量分布图近似正态分布，峰宽较窄，可见魔芋葡甘露低聚糖分子大小分布相对集中，为相对均一的低聚糖。
实施例3
一种魔芋葡甘露低聚糖的制备方法，其步骤是：取市售魔芋粉放入浓度为70%（V/V）二甲基亚砜溶液容器中，经频率为KHz超声波超声90min后，取出，过滤，得滤渣按1:10（M/V）乙醇反复沉淀过滤3次后，干燥，即可得到分子量均一的魔芋葡甘露低聚糖，所得产物保持了魔芋葡甘聚糖的化学结构，见图1。参见图4，本发明方法中制备的魔芋葡甘聚糖精粉经GPC-LS测定，产物收率为85%，其重均分子量为3.528×105，其相对分子量分布图近似正态分布，峰宽较窄，可见魔芋葡甘露低聚糖分子大小分布相对集中，为相对均一的低聚糖。

Claims (2)

1.一种魔芋葡甘露低聚糖的制备方法，其特征在于：所述魔芋葡甘露低聚糖是将魔芋粉放入二甲基亚砜溶液中超声降解所得；
其包括具体方法如下：
将魔芋粉放入浓度为70% ～ 95%（V/V）二甲基亚砜溶液容器中，经40KHz ～ 80KHz 的超声波超声60min ～90min 后取出过滤，将得到的滤渣用无水乙醇反复沉淀过滤3～5 次后干燥，即可得到分子量相对均一的魔芋葡甘露低聚糖，所得产物保持了魔芋葡甘聚糖的化学结构。
2.根据权利要求1 的所述魔芋葡甘露低聚糖的制备方法，其特征在于：所述滤渣与无水乙醇的重量比为1:10～1:50（M/V）。
CN201210415241.3A 2012-10-26 2012-10-26 一种魔芋葡甘露低聚糖的制备方法 Expired - Fee Related CN103030712B (zh)

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CN106317239A (zh) * 2016-08-19 2017-01-11 管天球 一种魔芋甘露聚糖的制备方法
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