CN106117386A - 分子印迹与超声耦合提取灵芝多糖的方法 - Google Patents

分子印迹与超声耦合提取灵芝多糖的方法 Download PDF

Info

Publication number
CN106117386A
CN106117386A CN201610501816.1A CN201610501816A CN106117386A CN 106117386 A CN106117386 A CN 106117386A CN 201610501816 A CN201610501816 A CN 201610501816A CN 106117386 A CN106117386 A CN 106117386A
Authority
CN
China
Prior art keywords
ganoderan
molecular engram
extracts
extraction
engram material
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610501816.1A
Other languages
English (en)
Inventor
卢月莲
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to CN201610501816.1A priority Critical patent/CN106117386A/zh
Publication of CN106117386A publication Critical patent/CN106117386A/zh
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26—Synthetic macromolecular compounds
    • B01J20/268—Polymers created by use of a template, e.g. molecularly imprinted polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/52—Amides or imides
    • C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F222/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
    • C08F222/10—Esters
    • C08F222/1006—Esters of polyhydric alcohols or polyhydric phenols
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/26—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a solid phase from a macromolecular composition or article, e.g. leaching out
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F222/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
    • C08F222/10—Esters
    • C08F222/1006—Esters of polyhydric alcohols or polyhydric phenols
    • C08F222/102—Esters of polyhydric alcohols or polyhydric phenols of dialcohols, e.g. ethylene glycol di(meth)acrylate or 1,4-butanediol dimethacrylate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2201/00—Foams characterised by the foaming process
    • C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
    • C08J2201/042—Elimination of an organic solid phase
    • C08J2201/0422—Elimination of an organic solid phase containing oxygen atoms, e.g. saccharose
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2201/00—Foams characterised by the foaming process
    • C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
    • C08J2201/046—Elimination of a polymeric phase
    • C08J2201/0462—Elimination of a polymeric phase using organic solvents
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2335/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical, and containing at least one other carboxyl radical in the molecule, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Derivatives of such polymers
    • C08J2335/02—Characterised by the use of homopolymers or copolymers of esters

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Medicinal Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Molecular Biology (AREA)
  • Biochemistry (AREA)
  • Analytical Chemistry (AREA)
  • Sustainable Development (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

本发明公开了一种分子印迹与超声耦合提取灵芝多糖的方法，涉及天然产物的提取分离技术领域。由于分子印迹技术具有构效预定性、特异识别性的特点，提取到的灵芝多糖纯度和提取率都较高，解决了目前灵芝多糖的提取工艺落后，提取到的灵芝多糖色素等杂质较多影响了色泽和抗癌的活性的问题。

Description

分子印迹与超声耦合提取灵芝多糖的方法
技术领域
本发明涉及天然产物的提取分离技术领域，尤其是一种分子印迹与超声耦合提取灵芝多糖的方法。
背景技术
灵芝又称林中灵、琼珍（学名：Ganoderma Lucidum Karst）是多孔菌科真菌灵芝的子实体。灵芝含有多种化学成分，其主要活性成分有多糖及肽多糖类、生物碱类和核苷酸类、氨基酸和蛋白质类、三萜类、微量元素。其中灵芝多糖具有抗肿瘤、免疫调节、降血糖、降血脂、抗氧化和抗衰老等作用，还可做为抗肿瘤和放射治疗的有效辅助治疗药物。然而，由于提取工艺落后，且灵芝多糖中色素含量较多，得到的产品呈黄褐色影响了色泽；同时，过高的杂质含量也影响了其抗癌的活性。
分子印迹技术是目前研究的热点，它具有构效预定性、特异识别性的特点，是一种比较具有产业化价值的技术。这种技术一般是将目标分子作为模版分子，选择在官能团结构上与之相匹配的功能单体，让两者间发生共价作用或非共价作用，再加入交联剂通过热聚合或光聚合，在引发剂的致孔剂的诱发下产生聚合反应，从而形成包裹有目标分子的高聚物，即分子印迹聚合物（MIPs），随后，利用物理或者化学方法，将目标分子从聚合物内部洗脱出来，一次获得具有与目标分子形状相同且官能团位置一定的记忆空穴。
发明内容
本发明提供一种分子印迹与超声耦合提取灵芝多糖的方法，它可以解决目前灵芝多糖的提取工艺落后，提取到的灵芝多糖色素等杂质较多影响了色泽和抗癌的活性的问题。
为了解决上述问题，本发明所采用的技术方案是：这种分子印迹与超声耦合提取灵芝多糖的方法是以灵芝粉末作为提取原料，以水作为提取媒介，利用分子印迹材料吸附提取液中的灵芝多糖，再用超声提取设备从提取液中提取吸附有灵芝多糖的分子印迹材料，提取完毕后，洗脱所述分子印迹材料上吸附的灵芝多糖即可；
所述分子印迹材料由如下方法制得：
取1～1.5mmol灵芝多糖与6mmol甲基丙烯酸溶解在5～10ml氯仿中，置于0℃下保持30min，然后加入15～30mmol二甲基丙烯酸乙二醇酯与15～30mmolN-异丙基丙烯酰胺和40～100mg偶氮二异丁腈，混合后，通入氮气，搅拌至完全溶解，通氮气10min，封口，在65℃条件反应直至聚合完全，粉碎，过200目筛，用体积比为9：1的甲醇：乙醇混合液洗脱灵芝多糖，即可得到分子印迹材料。
上述技术方案中，更具体的技术方案还可以是：所述超声提取过程控制在250W，40MHz。
进一步的：提取完毕后，先用60倍所述分子印迹材料重量的50℃水洗脱吸附在所述分子印迹材料上的杂质，再用30倍所述分子印迹材料重量的25℃水洗脱即可得到灵芝多糖溶液。
由于采用了上述技术方案，本发明与现有技术相比具有如下有益效果：
1、本发明的提取灵芝多糖纯度和提取率都较高，纯度能达95～99%，提取率能达85～98%，工序简单、印迹材料可重复使用，尤其适于工业化生产。
2、本发明提取办法工艺环保，没有用到任何有机试剂制备，同时印迹材料的最低临界溶解温度（LCST）为38℃左右，超声提取因为会积热，温度很容易达到38℃以上，不用外加热源，节能环保。
具体实施方式
以下结合具体实施例对本发明作进一步详述：
这种分子印迹与超声耦合提取灵芝多糖的方法首先要制备分子印迹，制备方法如下：
A、将1kg干燥的灵芝进行粉碎，所得的灵芝粉用6kg质量比浓度为80%的乙醇水溶液浸提3次，合并所得的浸提液，每次浸提过程中控制温度为60℃，每次时间为2h；
B、将步骤A所得的浸提液浓缩得到灵芝多糖浸膏；
C、将步骤B所得灵芝多糖浸膏依次用2倍重量的无水乙醇、丙酮分别洗涤，将洗涤后的沉淀用2倍蒸馏水溶解，过截留分子量为5万的中空纤维膜，收集浓缩液，然后将浓缩液过截留分子量为8万的中空纤维膜，收集透过液离心，过滤，取滤液备用；
D、往步骤C所得滤液加入活性炭脱色，过滤，取滤液干燥，即得灵芝多糖；
E、取1mmol灵芝多糖与6mmol甲基丙烯酸溶解在5ml氯仿中，置于0℃下保持30min，然后加入15mmol二甲基丙烯酸乙二醇酯与15mmolN-异丙基丙烯酰胺和40mg偶氮二异丁腈，混合后，通入氮气，搅拌至完全溶解，通氮气10min，封口，在65℃条件反应直至聚合完全，粉碎，过200目筛，用体积比为9：1的甲醇：乙醇混合液洗脱灵芝多糖，即可得到分子印迹材料。
然后将制得的分子印迹材料与超声耦合进行灵芝多糖的提取，提取过程如下：
以灵芝粉末作为提取原料，以水作为提取媒介，利用制得的分子印迹材料吸附提取液中的灵芝多糖，再用超声提取设备从提取液中提取吸附有灵芝多糖的分子印迹材料，提取过程控制在250W，40MHz。提取完毕后，先用60倍所述分子印迹材料重量的50℃水洗脱吸附在所述分子印迹材料上的杂质，再用30倍所述分子印迹材料重量的25℃水洗脱即可得到灵芝多糖水溶液。
该分子印迹材料可重复使用。

Claims (3)

1.一种分子印迹与超声耦合提取灵芝多糖的方法，其特征在于：以灵芝粉末作为提取原料，以水作为提取媒介，利用分子印迹材料吸附提取液中的灵芝多糖，再用超声提取设备从提取液中提取吸附有灵芝多糖的分子印迹材料，提取完毕后，洗脱所述分子印迹材料上吸附的灵芝多糖即可；
所述分子印迹材料由如下方法制得：
取1～1.5mmol灵芝多糖与6mmol甲基丙烯酸溶解在5～10ml氯仿中，置于0℃下保持30min，然后加入15～30mmol二甲基丙烯酸乙二醇酯与15～30mmolN-异丙基丙烯酰胺和40～100mg偶氮二异丁腈，混合后，通入氮气，搅拌至完全溶解，通氮气10min，封口，在65℃条件反应直至聚合完全，粉碎，过200目筛，用体积比为9：1的甲醇：乙醇混合液洗脱灵芝多糖，即可得到分子印迹材料。
2.根据权利要求1所述的分子印迹与超声耦合提取灵芝多糖的方法，其特征在于：所述超声提取过程控制在250W，40MHz。
3.根据权利要求1所述的分子印迹与超声耦合提取灵芝多糖的方法，其特征在于：提取完毕后，先用60倍所述分子印迹材料重量的50℃水洗脱吸附在所述分子印迹材料上的杂质，再用30倍所述分子印迹材料重量的25℃水洗脱即可得到灵芝多糖溶液。
CN201610501816.1A 2016-06-30 2016-06-30 分子印迹与超声耦合提取灵芝多糖的方法 Pending CN106117386A (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610501816.1A CN106117386A (zh) 2016-06-30 2016-06-30 分子印迹与超声耦合提取灵芝多糖的方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610501816.1A CN106117386A (zh) 2016-06-30 2016-06-30 分子印迹与超声耦合提取灵芝多糖的方法

Publications (1)

Publication Number Publication Date
CN106117386A true CN106117386A (zh) 2016-11-16

Family

ID=57285604

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610501816.1A Pending CN106117386A (zh) 2016-06-30 2016-06-30 分子印迹与超声耦合提取灵芝多糖的方法

Country Status (1)

Country Link
CN (1) CN106117386A (zh)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107722134A (zh) * 2017-11-08 2018-02-23 广西南宁胜祺安科技开发有限公司 一种淮山药多糖的制备方法
CN107778375A (zh) * 2017-11-08 2018-03-09 广西南宁胜祺安科技开发有限公司 一种淮山药黏液多糖和抗性淀粉的制备方法
CN112890196A (zh) * 2021-03-10 2021-06-04 江西仙客来生物科技有限公司 一种灵芝黄精胶囊及其制备方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101367881A (zh) * 2008-09-19 2009-02-18 南京农业大学 一种灵芝多糖的高效制备方法
CN101805414A (zh) * 2010-04-06 2010-08-18 无限极（中国）有限公司 一种高得率的灵芝多糖的制备方法
CN103601813A (zh) * 2013-12-06 2014-02-26 武汉苏妃玛索科技有限公司 一种灵芝多糖的提取方法
CN103664942A (zh) * 2013-12-16 2014-03-26 广西大学 一种分子印迹与超声耦合提取苦参碱的方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101367881A (zh) * 2008-09-19 2009-02-18 南京农业大学 一种灵芝多糖的高效制备方法
CN101805414A (zh) * 2010-04-06 2010-08-18 无限极（中国）有限公司 一种高得率的灵芝多糖的制备方法
CN103601813A (zh) * 2013-12-06 2014-02-26 武汉苏妃玛索科技有限公司 一种灵芝多糖的提取方法
CN103664942A (zh) * 2013-12-16 2014-03-26 广西大学 一种分子印迹与超声耦合提取苦参碱的方法

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107722134A (zh) * 2017-11-08 2018-02-23 广西南宁胜祺安科技开发有限公司 一种淮山药多糖的制备方法
CN107778375A (zh) * 2017-11-08 2018-03-09 广西南宁胜祺安科技开发有限公司 一种淮山药黏液多糖和抗性淀粉的制备方法
CN112890196A (zh) * 2021-03-10 2021-06-04 江西仙客来生物科技有限公司 一种灵芝黄精胶囊及其制备方法

Similar Documents

Publication Publication Date Title
He et al. Water extraction of anthocyanins from black rice and purification using membrane separation and resin adsorption
Hou et al. Adsorption/desorption characteristics and chromatographic purification of polyphenols from Vernonia patula (Dryand.) Merr. using macroporous adsorption resin
CN106117386A (zh) 分子印迹与超声耦合提取灵芝多糖的方法
CN103408602B (zh) 一种从藏茵陈中分离制备四种苷类化学对照品的方法
CN106967142A (zh) 一种同时提取罗汉果甜苷v、ⅵ和11‑o基苷v的方法
CN108176079A (zh) 一种甘草提取物的脱色方法
CN105859803B (zh) 一种没食子酰基葡萄糖的制备方法
CN105348440B (zh) Oblongifolin C分子印迹聚合物及其制备方法和应用
CN102344429B (zh) 柑桔多甲氧基黄酮的提取及纯化方法
CN106046254B (zh) 富集京尼平苷的亲水性分子印迹聚合物及制备方法和应用
CN1869048B (zh) 一种从人参叶中提取分离f组人参皂苷的方法
CN107098942A (zh) 一种亚临界水萃取萝卜叶中山奈苷的方法
CN106117298A (zh) 分子印迹与超声耦合提取灵芝酸的办法
Li et al. Comparison of different extraction methods of active ingredients of Chinese medicine and natural products
CN101210041A (zh) 一种丹参酮ⅱa化学对照品的分离制备方法
CN104072456A (zh) 一种高纯度丹酚酸b的制备方法
CN103224590A (zh) 一种光甘草定分子印迹聚合物及其制备方法和应用
CN106074629A (zh) 分子印迹与超声耦合提取灵芝三萜的方法
CN102827327A (zh) 一种葡聚糖凝胶表面苏丹红分子印迹吸附材料的制备及应用
CN102432656A (zh) 一种蛹虫草子实体中虫草素提取纯化的方法
CN102659861A (zh) 一种曲札茋苷的纯化方法
CN105646464A (zh) 一种从木棉叶中提取高纯度芒果苷的方法
CN105712896A (zh) 一种从玛咖中高效制备玛咖酰胺单体的方法
CN104277177B (zh) 一种姜酚假模板分子印迹聚合物及用其从生姜中提取姜酚的方法
CN107746419B (zh) 一种苹果花有效部位、制备方法及利用其提取山奈酚葡萄糖苷的方法

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20161116

WD01 Invention patent application deemed withdrawn after publication