CN106243165A - The method extracting glycosides from sweet tea - Google Patents

The method extracting glycosides from sweet tea Download PDF

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Publication number
CN106243165A
CN106243165A CN201610860236.1A CN201610860236A CN106243165A CN 106243165 A CN106243165 A CN 106243165A CN 201610860236 A CN201610860236 A CN 201610860236A CN 106243165 A CN106243165 A CN 106243165A
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Prior art keywords
sweet tea
glycosides
filtrate
method extracting
crude extract
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CN201610860236.1A
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黄建军
谢冬养
陆美珍
叶出良
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Guilin Yi Tiancheng Biotechnology Co Ltd
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Guilin Yi Tiancheng Biotechnology Co Ltd
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Priority to CN201610860236.1A priority Critical patent/CN106243165A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H1/00Processes for the preparation of sugar derivatives
    • C07H1/06Separation; Purification
    • C07H1/08Separation; Purification from natural products
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H15/00Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
    • C07H15/20Carbocyclic rings
    • C07H15/24Condensed ring systems having three or more rings
    • C07H15/256Polyterpene radicals

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Biotechnology (AREA)
  • General Health & Medical Sciences (AREA)
  • Genetics & Genomics (AREA)
  • Molecular Biology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Seasonings (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The invention discloses a kind of method extracting glycosides from sweet tea, comprise the following steps: 1) sweet tea is pulverized, with ethanol extraction, extracting solution is filtered, takes decompression filtrate recycling ethanol, obtain crude extract;2) crude extract is dissolved in water, filters, take filtrate standby;3) by step 2) filtrate separated by the macromolecular filtering film that can retain 1000 molecular weight, collect effluent;4) in effluent, EuAlO is added in the ratio that solid-liquid ratio is 1000ml:0.2~1mg3, precipitate 30~50s, filter off precipitation, filtrate is dried, is glycosides.Compared with prior art, without sweet tea polyphenols in the glycosides that the present invention extracts, in good taste, without astringent taste.

Description

The method extracting glycosides from sweet tea
Technical field
The invention belongs to technical field of biological extraction, be specifically related to a kind of method extracting glycosides from sweet tea.
Background technology
Guangxi Folium hydrangeae strigosae, formal name used at school Rubus Suatrssimus S.Lee, is the one in Rosaceae rubus.Sweet Tea whole body is precious, and root, stem, leaf, fruit all can enter tea and be used as medicine.Sweet tea is often used as sweeting agent, and among the people being used as medicine can be used for mending Kidney blood pressure lowering, is described as god's tea, with the big famous-object in Guangxi ten equally celebrated for their achievements such as Fructus Momordicae, Hepu Margarita, Guangxi spice.Sweet tea contains The flavone of more than 3.2%, the sweet tea polyphenols of 8.94% and 4~the glycosides of 5%.Glycosides be a kind of high sugariness, low heat value, Avirulent natural sweetener, is a kind of preferably saccharide succedaneum, to avoid because of long-term excess eat sugar, cause human body to be got fat and The people of the diseases such as induction hypertension, diabetes, cardiovascular diseases, kidney have good auxiliary curative effect.The sugariness of glycosides is 300 times of sucrose, are steviol (Steviol) and diterpene glycoside that glucose is combined into.Glycosides molecular formula is C32H50O12, similar to stevioside (Stevioside) in chemical constitution, all it is made up of identical glycoside unit, its difference only exists C13A part glucose is connect less on position.During the extraction of glycosides, overwhelming majority sweet tea polyphenols is also extracted, and These sweet tea polyphenols are difficult to separate from glycosides completely, cause the taste with some bitternesses in glycosides finished product, Greatly reduce the quality of glycosides.
Summary of the invention
Present invention solves the technical problem that the sweet tea polyphenols being to overcome and contain bitterness in existing glycosides, it is provided that Yi Zhongwei Road is pure, without the extracting method of the glycosides of bitterness.
The technical scheme that the present invention provides is the method extracting glycosides from sweet tea, comprises the following steps:
1) sweet tea is pulverized, with ethanol extraction, extracting solution is filtered, takes decompression filtrate recycling ethanol, obtain crude extract;
2) crude extract is dissolved in water, filters, take filtrate standby;
3) by step 2) filtrate separated by the macromolecular filtering film that can retain 1000 molecular weight, collect and flow out Liquid;
4) in effluent, EuAlO is added in the ratio that solid-liquid ratio is 1000ml:0.2~1mg3, precipitate 30~50s, filter Go precipitation, filtrate is dried, is glycosides.
Step 1) in, sweet tea is 1g:10~20ml with the solid-liquid ratio of ethanol solution.The volumetric concentration of ethanol be 40~ 60%.Using heating and refluxing extraction method, extract 1~3 time, each extraction time is 1~3h.
Step 2) in, the addition of water is 20~30 times of crude extract weight.
Step 3) in, due to step 2) in the filtrate that obtains containing substantial amounts of sweet tea polyphenols impurity, its taste is the most bitter Puckery, filtrate is separated by retaining the macromolecular filtering film of 1000 molecular weight, the macromole Folium hydrangeae strigosae in filtrate can be removed Tea polyphenols.
Step 4) in, sweet tea polyphenols intramolecular has electronics height delocalization, the conjugated system of big π key, the oxygen of strong coordination Atom and suitably steric configuration, can lose electronics and form good part with metal ion.But electronics is from ligand Transitting to need certain energy on the track of metal ion, directly by electron transition to metal, required energy is higher, reaction Time is longer, and deposition efficiency is relatively low, and toward effluent adds composite oxides--the EuAlO of rare earth metal3, sweet tea polyphenols Oxygen atom loses electronics by Eu3+Ion obtains, due to Eu3+Ionic radius is little, and electronegativity is relatively big, Eu3+Ion is electronically formed Half-full Eu2+4f shell structurre linkage electron very capable, this process is very fast, then Eu3+The electronics obtained again can Transfer to the metal Al of composite oxides at once3+, owing in the valency between rare earth element and metal ion, charge transfer transition is very Hurry up, therefore, this process is the rapidest, so that sweet tea polyphenols can be formed under complex compound sediment at a terrific speed Coming, sweet tea polyphenols can complex-precipitation completely, it is ensured that has no astringent taste in finished product.Participate in the EuAlO of reaction3Many with Folium hydrangeae strigosae tea Phenol complexation forms precipitation, and has neither part nor lot in the EuAlO of reaction3Itself is water insoluble, also will not be mixed in glycosides, it can be ensured that The safety of finished product.
Step 4) in, adding EuAlO3Before, in effluent, NaCO is added3Or NaHCO3Regulation pH value is to 6~7. NaCO3Or NaHCO3Regulation pH value, helps sweet tea polyphenols preferably to precipitate and attacks, be avoided that again tea polyphenols oxidative deformation.Flow out When the pH value of liquid is to 6~7, sweet tea polyphenols molecule has hydroxyl to participate in the reaction with metal ion, and pH value is too high, and Folium hydrangeae strigosae tea is many Phenol is the most unstable, is oxidized easily.Thus be difficult to carry out complex-precipitation with metal, pH value is too low, phenolic hydroxyl group hydrogen Dissociating of atom is the most difficult, it is difficult to make reaction carry out towards the direction of complex-precipitation.
Compared with prior art, without sweet tea polyphenols in the glycosides that the present invention extracts, in good taste, without astringent taste.
Detailed description of the invention
The present invention is further elaborated for specific examples below, but not as a limitation of the invention.
Embodiment 1
1) being pulverized by sweet tea, adding volumetric concentration in the ratio that solid-liquid ratio is 1g:10ml is the ethanol of 40%, heats back Stream extracts 1h, is filtered by extracting solution, takes decompression filtrate recycling ethanol, obtain crude extract;
2) crude extract is added the water of its weight 20 times, stirring, dissolve, filter, take filtrate standby;
3) by step 2) filtrate separated by the macromolecular filtering film that can retain 1000 molecular weight, collect and flow out Liquid;
4) in effluent, EuAlO is added in the ratio that solid-liquid ratio is 1000ml:0.2mg3, precipitate 30s, filter off precipitation, Filtrate is dried, is glycosides.Through analyzing, in glycosides, the content of sweet tea polyphenols is only 0.05%, and glycosides mouthfeel is pure Just, without astringent taste.
Embodiment 2
1) being pulverized by sweet tea, adding volumetric concentration in the ratio that solid-liquid ratio is 1g:20ml is the ethanol of 60%, heats back Stream extracts 3 times, and each extraction time is 3h, is filtered by extracting solution, takes decompression filtrate recycling ethanol, obtain crude extract;
2) crude extract is added the water of its weight 30 times, stirring, dissolve, filter, take filtrate standby;
3) by step 2) filtrate separated by the macromolecular filtering film that can retain 1000 molecular weight, collect and flow out Liquid;
4) in effluent, NaCO is added3Or NaHCO3Regulation pH value is to 7, then is the ratio of 1000ml:1mg in solid-liquid ratio Add EuAlO3, precipitate 50s, filter off precipitation, filtrate is dried, is glycosides.Through analyzing, sweet tea polyphenols in glycosides Content is only 0.014%, and glycosides pure in mouth feel, without astringent taste.
Embodiment 3
1) being pulverized by sweet tea, adding volumetric concentration in the ratio that solid-liquid ratio is 1g:15ml is the ethanol of 50%, heats back Stream extracts 2 times, and each extraction time is 2h, is filtered by extracting solution, takes decompression filtrate recycling ethanol, obtain crude extract;
2) crude extract is added the water of its weight 25 times, stirring, dissolve, filter, take filtrate standby;
3) by step 2) filtrate separated by the macromolecular filtering film that can retain 1000 molecular weight, collect and flow out Liquid;
4) in effluent, NaCO is added3Or NaHCO3Regulation pH value is to 6.5, then is 1000ml:0.5mg's by solid-liquid ratio Ratio adds EuAlO3, precipitate 30~50s, filter off precipitation, filtrate is dried, is glycosides.Through analyzing, Folium hydrangeae strigosae in glycosides The content of tea polyphenols is only 0.015%, and glycosides pure in mouth feel, without astringent taste.
Embodiment 4
1) being pulverized by sweet tea, adding volumetric concentration in the ratio that solid-liquid ratio is 1g:10ml is the ethanol of 60%, heats back Stream extracts 3h, is filtered by extracting solution, takes decompression filtrate recycling ethanol, obtain crude extract;
2) crude extract is added the water of its weight 20 times, stirring, dissolve, filter, take filtrate standby;
3) by step 2) filtrate separated by the macromolecular filtering film that can retain 1000 molecular weight, collect and flow out Liquid;
4) in effluent, NaCO is added3Or NaHCO3Regulation pH value is to 7, then by the ratio that solid-liquid ratio is 1000ml:0.2mg Example adds EuAlO3, precipitate 50s, filter off precipitation, filtrate is dried, is glycosides.Through analyzing, sweet tea polyphenols in glycosides Content be only 0.018%, glycosides pure in mouth feel, without astringent taste.

Claims (6)

1. the method extracting glycosides from sweet tea, its feature exists: comprise the following steps:
1) sweet tea is pulverized, with ethanol extraction, extracting solution is filtered, takes decompression filtrate recycling ethanol, obtain crude extract;
2) crude extract is dissolved in water, filters, take filtrate standby;
3) by step 2) filtrate separated by the macromolecular filtering film that can retain 1000 molecular weight, collect effluent;
4) in effluent, EuAlO is added in the ratio that solid-liquid ratio is 1000ml:0.2~1mg3, precipitate 30~50s, it is heavy to filter off Form sediment, filtrate is dried, is glycosides.
The method extracting glycosides from sweet tea the most according to claim 1, it is characterised in that: step 1) in, Folium hydrangeae strigosae Leaf is 1g:10~20ml with the solid-liquid ratio of ethanol solution.
The method extracting glycosides from sweet tea the most according to claim 1, it is characterised in that: step 1) in, described Being extracted as heating and refluxing extraction 1~3 times, each extraction time is 1~3h.
The method extracting glycosides from sweet tea the most according to claim 1, it is characterised in that: step 1) in, ethanol Volumetric concentration be 40~60%.
The method extracting glycosides from sweet tea the most according to claim 1, it is characterised in that: step 2) in, water Addition is 20~30 times of crude extract weight.
The method extracting glycosides from sweet tea the most according to claim 1, it is characterised in that: step 4) in, adding Add EuAlO3Before, in effluent, NaCO is added3Or NaHCO3Regulation pH value is to 6~7.
CN201610860236.1A 2016-09-27 2016-09-27 The method extracting glycosides from sweet tea Pending CN106243165A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018233092A1 (en) 2017-06-19 2018-12-27 桂林莱茵生物科技股份有限公司 Method for preparing rubusoside

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1104621A (en) * 1993-11-18 1995-07-05 安徽省黄山市东方茶多酚厂 Extraction of theophenol
CN101003552A (en) * 2006-01-18 2007-07-25 广西师范大学 Method for preparing glycosides in high purity
CN101054370A (en) * 2007-05-23 2007-10-17 福建师范大学 Method for preparing nano tea polypherals rare earth complexes by liquid phase method
JP2011126795A (en) * 2009-12-16 2011-06-30 Maruzen Pharmaceut Co Ltd Type i collagen production promoter
CN102838644A (en) * 2012-08-23 2012-12-26 长沙绿蔓生物科技有限公司 Production method for extracting sweet tea glucoside from sweet tea leaves
KR20130014192A (en) * 2011-07-29 2013-02-07 한국생명공학연구원 New method for producing rubusoside
US20130040033A1 (en) * 2011-08-10 2013-02-14 Purecircle Sdn Bhd High-Purity Rubusoside And Process For Purification Of The Same
CN104262425A (en) * 2014-08-15 2015-01-07 桂林莱茵生物科技股份有限公司 Novel method for extracting rubusoside
CN105111776A (en) * 2015-09-08 2015-12-02 湖州市菱湖重兆金辉丝织厂 Novel natural dye based on Rosa chinensis cyanin pigment and preparation method thereof
CN105166198A (en) * 2015-09-29 2015-12-23 重庆骄王天然产物股份有限公司 Preparation method of high-purity rubusoside

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1104621A (en) * 1993-11-18 1995-07-05 安徽省黄山市东方茶多酚厂 Extraction of theophenol
CN101003552A (en) * 2006-01-18 2007-07-25 广西师范大学 Method for preparing glycosides in high purity
CN101054370A (en) * 2007-05-23 2007-10-17 福建师范大学 Method for preparing nano tea polypherals rare earth complexes by liquid phase method
JP2011126795A (en) * 2009-12-16 2011-06-30 Maruzen Pharmaceut Co Ltd Type i collagen production promoter
KR20130014192A (en) * 2011-07-29 2013-02-07 한국생명공학연구원 New method for producing rubusoside
US20130040033A1 (en) * 2011-08-10 2013-02-14 Purecircle Sdn Bhd High-Purity Rubusoside And Process For Purification Of The Same
CN102838644A (en) * 2012-08-23 2012-12-26 长沙绿蔓生物科技有限公司 Production method for extracting sweet tea glucoside from sweet tea leaves
CN104262425A (en) * 2014-08-15 2015-01-07 桂林莱茵生物科技股份有限公司 Novel method for extracting rubusoside
CN105111776A (en) * 2015-09-08 2015-12-02 湖州市菱湖重兆金辉丝织厂 Novel natural dye based on Rosa chinensis cyanin pigment and preparation method thereof
CN105166198A (en) * 2015-09-29 2015-12-23 重庆骄王天然产物股份有限公司 Preparation method of high-purity rubusoside

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
明珠,等: "茶汤与金属离子络合反应的研究", 《环境科技》 *
梁靖,等: "茶多酚的络合作用研究进展", 《茶叶》 *
程慧青: "茶多酚稀土(La、Ce、Pr)配合物的合成、表征及应用性能研究", 《福建师范大学硕士学位论文》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018233092A1 (en) 2017-06-19 2018-12-27 桂林莱茵生物科技股份有限公司 Method for preparing rubusoside
US10968470B2 (en) 2017-06-19 2021-04-06 Guilin Layn Natural Ingredients Corp. Method for preparing rubusoside

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