CN110066348A - 一种提取、精制菊苣低聚糖的方法 - Google Patents
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Abstract
本发明涉及一种提取、精制菊苣低聚糖的方法,采用超声波辅助提取法得到菊苣低聚糖产物,之后对菊苣低聚糖产物采用吡啶‑醋酸酐法、利用硅胶柱纯化得到全乙酰化产物,最后经TLC(薄层色谱)分析得到精制的菊苣低聚糖。将该方法用于菊苣低聚糖的制备工艺,可有效解决菊苣低聚糖提取率低、提取纯度低等问题,亦可适用于提取、精制其他植物类低聚糖。
Description
技术领域
本发明涉及一种提取、精制低聚糖的方法,特别是涉及一种提取、精制菊苣低聚糖的方法,属于低聚糖提取技术领域。
背景技术
菊苣Cichorii Herba为菊科(Compositae)植物,菊苣Cichorium intybus L.及毛菊苣Cichorium glandulosum Boiss.et Hout的干燥地上部分或根,又名蓝菊,维语称“卡申纳”,作为维吾尔族习用药材收载于《新疆中草药手册》,其性味微苦、咸、凉,具有清肝利胆、健胃消食、利尿消肿之功效,用于治疗湿热黄疸、胃痛食少、水肿尿少等病症。除药用外,菊苣还作为牧草和蔬菜广泛应用,其作为保健饮品和功能性食品也受到了国际保健食品界的青睐。
低聚糖(Oligosaccharides)又称寡糖,指由2-10个相同或不同的单糖通过糖苷键连接聚合而成的直链或支链的低度聚合糖,包括功能性低聚糖和普通低聚糖。功能性低聚糖在自然界分布广泛,种多,因其具有低热量、防龋齿、防便秘、降低血清胆固醇、增强机体免疫力、抗肿瘤等特点,使得功能性低聚糖成为功能性食品生产中重要的基础原料与食品添加剂,现已被世界许多国家的工业生产所用。
本发明是采用超声波辅助提取法得到菊苣低聚糖产物,之后对菊苣低聚糖产物采用吡啶-醋酸酐法、利用硅胶柱纯化得到全乙酰化产物,最后经TLC(薄层色谱)分析得到精制的菊苣低聚糖。经调查,申请的专利中已经有了对菊苣低聚果糖制备的专利,申请号为CN201710142165.6,名为“利用内切菊粉酶以菊苣或菊芋为原料生产低聚果糖”的专利,其方法是以菊苣或菊芋为原料利用内切菊粉酶,在酶解的温度55℃-65℃,搅拌50r/min-70r/min,酶解时间2h-4h条件下生产低聚果糖;另外,申请号为CN201210144883.4,名为“一种纯化菊苣低聚果糖的新方法”的专利,其方法是利用黑曲霉菊粉内切酶-微波提取联用技术,大孔树脂脱色除杂,超滤、纳滤结合纯化菊苣中低聚果糖。公开报道的专利中对菊苣低聚果糖提取、纯化、制备的方法较多,但对菊苣低聚糖的研究尚未见报道,尤其是如何解决精制菊苣低聚糖提取方法未见有公开报道,因此,开发一种提取、精制菊苣低聚糖的方法具有十分重要的意义。
发明内容
针对上述情况,为克服现有技术之缺陷,本发明的目的是提供一种提取、精制菊苣低聚糖的方法,可有效解决菊苣低聚糖在制备降血糖、降血脂、降血压的药物和保健品中的应用问题。该方法提取效率高、提取纯度高且制备的低聚糖保存活性高,大大节约提取和生产成本。
为实现上述发明的目的,本发明采取的技术方案如下:一种提取、精制菊苣低聚糖的方法,包括以下步骤:
(1)选取原材料:选取根肉质多的菊苣,去除腐败、变质的部分;
(2)粉碎、过筛:将菊苣粉碎过筛(20目试验标准筛),加水搅拌;
(3)超声波辅助提取:试验在液料比30-40∶1mL/g,超声波时间25-35min,超声波功率400-500W条件下进行;
(4)加酵母:酵母用量为原料量的1-5%,将酵母在35-45℃、含糖量1-5%、酵母用10-15倍以上的水溶液中复水活化,30-60min后即可添加使用;
(5)抽滤分离:真空浓缩至原体积的1/3;加入5倍体积的90%-95%乙醇沉降8-10h;过滤,并于真空旋转蒸发浓缩旋干后加原体积旳1/3的水复溶至无醇味;
(6)吡啶-醋酸酐法:加入10mL醋酸酐和20mL吡啶,搅拌反应10~15h,加入50mL质量分数为10%的乙酸钠,加入40mL氯仿萃取有机相,萃取2~3次,洗涤、干燥,旋转蒸发;
(7)硅胶柱纯化全乙酰化产物:将硅胶和适量洗脱液(环己烷:乙酸乙酯=2∶3(v∶v))混合,搅拌,并冲柱子2h,静置5h,以3min/管,3mL/管收集样品;
(8)TLC(薄层色谱)分析:展开剂为环己烷∶乙酸乙酯=2∶3(v∶v),显色剂为:二苯胺2.5g,苯胺5ml,25ml 85%磷酸混合,加丙酮至250mL。收集纯化的全乙酰化菊苣低聚糖;
(9)冷冻浓缩:将收集纯化的全乙酰化菊苣低聚糖在-30℃至-10℃条件下冻干24h,冻干后保存即可。
本发明相对于现有技术的创新点是:本发明是采用超声波辅助提取法得到菊苣低聚糖产物,之后对菊苣低聚糖产物采用吡啶-醋酸酐法、利用硅胶柱纯化得到全乙酰化产物,最后经TLC(薄层色谱)分析得到精制的菊苣低聚糖。该提取、精制低聚糖的方法简单、易操作且提取的低聚糖保存活性高、得率高。菊苣原料丰富,产品应用广泛,以菊苣为原料同时制备菊苣低聚糖,开发了菊苣的应用范围,菊苣低聚糖可用于制备降血糖、降血脂、降血压的药物和保健品,开拓了菊苣低聚糖的应用价值,具有良好的经济效益和社会效益。
具体实施方式
下面通过实例对本发明的具体情况做进一步详细说明。
本发明在具体实施中,可由以下实施例给出:
实施例1
一种提取、精制菊苣低聚糖的方法,包括以下步骤:
(1)选取原材料:选取根肉质多的菊苣,去除腐败、变质的部分;
(2)粉碎、过筛:将菊苣粉碎过筛(20目试验标准筛),加水搅拌;
(3)超声波辅助提取:试验在液料比30∶1mL/g,超声波时间25min,超声波功率400W条件下进行;
(4)加酵母:酵母用量为原料量的1%,将酵母在35℃、含糖量1%、酵母用10倍以上的水溶液中复水活化,30-60min后即可添加使用;
(5)抽滤分离:真空浓缩至原体积的1/3;加入5倍体积的90%乙醇沉降8h;过滤,并于真空旋转蒸发浓缩旋干后加原体积旳1/3的水复溶至无醇味;
(6)吡啶-醋酸酐法:加入10mL醋酸酐和20mL吡啶,搅拌反应11h,加入50mL质量分数为10%的乙酸钠,加入40mL氯仿萃取有机相,萃取2次,洗涤、干燥,旋转蒸发;
(7)硅胶柱纯化全乙酰化产物:将硅胶和适量洗脱液(环己烷∶乙酸乙酯=2∶3(v∶v))混合,搅拌,并冲柱子2h,静置5h,以3min/管,3mL/管收集样品;
(8)TLC(薄层色谱)分析:展开剂为环己烷∶乙酸乙酯=2∶3(v∶v),显色剂为:二苯胺2.5g,苯胺5ml,25ml 85%磷酸混合,加丙酮至250mL。收集纯化的全乙酰化菊苣低聚糖;
(9)冷冻浓缩:将蒸发后的渣于-30℃条件下冻干24h,冻干后保存即可。
实施例2
一种提取、精制菊苣低聚糖的方法,包括以下步骤:
(1)选取原材料:选取根肉质多的菊苣,去除腐败、变质的部分;
(2)粉碎、过筛:将菊苣粉碎过筛(20目试验标准筛),加水搅拌;
(3)超声波辅助提取:试验在液料比32∶1mL/g,超声波时间27min,超声波功率425W条件下进行;
(4)加酵母:酵母用量为原料量的2%,将酵母在37℃、含糖量2%、酵母用11倍以上的水溶液中复水活化,37min后即可添加使用;
(5)抽滤分离:真空浓缩至原体积的1/3;加入5倍体积的91%乙醇沉降8.5h;过滤,并于真空旋转蒸发浓缩旋干后加原体积旳1/3的水复溶至无醇味;
(6)吡啶-醋酸酐法:加入10mL醋酸酐和20mL吡啶,搅拌反应12h,加入50mL质量分数为10%的乙酸钠,加入40mL氯仿萃取有机相,萃取2次,洗涤、干燥,旋转蒸发;
(7)硅胶柱纯化全乙酰化产物:将硅胶和适量洗脱液(环己烷∶乙酸乙酯=2∶3(v∶v))混合,搅拌,并冲柱子2h,静置5h,以3min/管,3mL/管收集样品;
(8)TLC(薄层色谱)分析:展开剂为环己烷∶乙酸乙酯=2∶3(v∶v),显色剂为:二苯胺2.5g,苯胺5ml,25ml 85%磷酸混合,加丙酮至250mL。收集纯化的全乙酰化菊苣低聚糖;
(9)冷冻浓缩:将蒸发后的渣于-25℃条件下冻干24h,冻干后保存即可。
实施例3
一种提取、精制菊苣低聚糖的方法,包括以下步骤:
(1)选取原材料:选取根肉质多的菊苣,去除腐败、变质的部分;
(2)粉碎、过筛:将菊苣粉碎过筛(20目试验标准筛),加水搅拌;
(3)超声波辅助提取:试验在液料比35∶1mL/g,超声波时间30min,超声波功率450W条件下进行;
(4)加酵母:酵母用量为原料量的3%,将酵母在40℃、含糖量3%、酵母用13倍以上的水溶液中复水活化,45min后即可添加使用;
(5)抽滤分离:真空浓缩至原体积的1/3;加入5倍体积的93%乙醇沉降9h;过滤,并于真空旋转蒸发浓缩旋干后加原体积旳1/3的水复溶至无醇味;
(6)吡啶-醋酸酐法:加入10mL醋酸酐和20mL吡啶,搅拌反应13h,加入50mL质量分数为10%的乙酸钠,加入40mL氯仿萃取有机相,萃取3次,洗涤、干燥,旋转蒸发;
(7)硅胶柱纯化全乙酰化产物:将硅胶和适量洗脱液(环己烷∶乙酸乙酯=2∶3(v∶v))混合,搅拌,并冲柱子2h,静置5h,以3min/管,3mL/管收集样品;
(8)TLC(薄层色谱)分析:展开剂为环己烷∶乙酸乙酯=2∶3(v∶v),显色剂为:二苯胺2.5g,苯胺5ml,25ml 85%磷酸混合,加丙酮至250mL。收集纯化的全乙酰化菊苣低聚糖;
(9)冷冻浓缩:将蒸发后的渣于-20℃至-10℃条件下冻干24h,冻干后保存即可。
实施例4
一种提取、精制菊苣低聚糖的方法,包括以下步骤:
(1)选取原材料:选取根肉质多的菊苣,去除腐败、变质的部分;
(2)粉碎、过筛:将菊苣粉碎过筛(20目试验标准筛),加水搅拌;
(3)超声波辅助提取:试验在液料比38∶1mL/g,超声波时间33min,超声波功率475W条件下进行;
(4)加酵母:酵母用量为原料量的4%,将酵母在43℃、含糖量4%、酵母用13倍以上的水溶液中复水活化,53min后即可添加使用;
(5)抽滤分离:真空浓缩至原体积的1/3;加入5倍体积的94%乙醇沉降9.5h;过滤,并于真空旋转蒸发浓缩旋干后加原体积旳1/3的水复溶至无醇味;
(6)吡啶-醋酸酐法:加入10mL醋酸酐和20mL吡啶,搅拌反应14h,加入50mL质量分数为10%的乙酸钠,加入40mL氯仿萃取有机相,萃取3次,洗涤、干燥,旋转蒸发;
(7)硅胶柱纯化全乙酰化产物:将硅胶和适量洗脱液(环己烷∶乙酸乙酯=2∶3(v∶v))混合,搅拌,并冲柱子2h,静置5h,以3min/管,3mL/管收集样品;
(8)TLC(薄层色谱)分析:展开剂为环己烷∶乙酸乙酯=2∶3(v∶v),显色剂为:二苯胺2.5g,苯胺5ml,25ml 85%磷酸混合,加丙酮至250mL。收集纯化的全乙酰化菊苣低聚糖;
(9)冷冻浓缩:将蒸发后的渣于-15℃条件下冻干24h,冻干后保存即可。
实施例5
一种提取、精制菊苣低聚糖的方法,包括以下步骤:
(1)选取原材料:选取根肉质多的菊苣,去除腐败、变质的部分;
(2)粉碎、过筛:将菊苣粉碎过筛(20目试验标准筛),加水搅拌;
(3)超声波辅助提取:试验在液料比40∶1mL/g,超声波时间35min,超声波功率500W条件下进行;
(4)加酵母:酵母用量为原料量的5%,将酵母在45℃、含糖量5%、酵母用15倍以上的水溶液中复水活化,60min后即可添加使用。
Claims (3)
1.一种提取、精制菊苣低聚糖的方法,其特征在于,包括以下步骤:
(1)选取原材料:选取根肉质多的菊苣,去除腐败、变质的部分;
(2)粉碎、过筛:将菊苣粉碎过筛(20目试验标准筛),加水搅拌;
(3)超声波辅助提取:试验在液料比30-40∶1mL/g,超声波时间25-35min,超声波功率400-500W条件下进行;
(4)加酵母:酵母用量为原料量的1-5%,将酵母在35-45℃、含糖量1-5%、酵母用10-15倍以上的水溶液中复水活化,30-60min后即可添加使用;
(5)抽滤分离:真空浓缩至原体积的1/3;加入5倍体积的90%-95%乙醇沉降8-10h;过滤,并于真空旋转蒸发浓缩旋干后加原体积旳1/3的水复溶至无醇味;
(6)吡啶-醋酸酐法:加入10mL醋酸酐和20mL吡啶,搅拌反应10~15h,加入50mL质量分数为10%的乙酸钠,加入40mL氯仿萃取有机相,萃取2~3次,洗涤、干燥,旋转蒸发;
(7)硅胶柱纯化全乙酰化产物:将硅胶和适量洗脱液(环己烷∶乙酸乙酯=2∶3(v∶v))混合,搅拌,并冲柱子2h,静置5h,以3min/管,3mL/管收集样品;
(8)TLC(薄层色谱)分析:展开剂为环己烷∶乙酸乙酯=2∶3(v∶v),显色剂为:二苯胺2.5g,苯胺5ml,25ml 85%磷酸混合,加丙酮至250mL。收集纯化的全乙酰化菊苣低聚糖;
(9)冷冻浓缩:将收集纯化的全乙酰化菊苣低聚糖在-30℃至-10℃条件下冻干24h,冻干后保存即可。
2.根据权利1要求所述的一种提取、精制菊苣低聚糖的方法,其特征在于所述的采用吡啶-醋酸酐法、利用硅胶柱纯化得到全乙酰化产物,最后经TLC(薄层色谱)分析得到精制的菊苣低聚糖。
3.根据权利1要求所述的一种提取、精制菊苣低聚糖的方法,其特征在于所述的制备方法不仅适用于提取、精制菊苣低聚糖,亦可适用于提取、精制其他植物类低聚糖。
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