CN103265583A - Method for preparing stachyose crystal - Google Patents
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- CN103265583A CN103265583A CN2013100680903A CN201310068090A CN103265583A CN 103265583 A CN103265583 A CN 103265583A CN 2013100680903 A CN2013100680903 A CN 2013100680903A CN 201310068090 A CN201310068090 A CN 201310068090A CN 103265583 A CN103265583 A CN 103265583A
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Abstract
The invention discloses a method for preparing stachyose crystals. The method comprises the steps of: (1) first sugar liquid preparation: including washing a raw material, extracting by hot water, squeezing juice to obtain the sugar liquid, concentrating the sugar liquid in vacuum to refractive index of 30-50 DEG Brix, adding 95% ethanol as a proportion of sugar liquid:ethanol (V/V) = 1:(2-6), stirring to uniform, filtering by a cardboard after standing, washing residue with 75% ethanol, mixing filtrates, concentrating at 45-75 DEG C in vacuum to 70-80 DEG Brix to get an alcohol-dissolved extract; (2) crude crystallization; (3) re-preparation of sugar liquid; (4) recrystallization; and (5) drying in vacuum to give a stachyose crystal with a purity higher than 99.0%.
Description
Technical field
The present invention relates to a kind of preparation method of stachyose crystallization, particularly relating to a kind of is the method for feedstock production high purity stachyose crystallization with the natural phant.
Background technology
Stachyose extensively is present in leguminous plants, labiate and the goatweed, is a kind of natural functional oligose, can effectively breed profitable strain (bifidus bacillus and Bacterium lacticum etc.) in the enteron aisle, has good physiological function.Along with reaching its maturity and the standardization in stachyose market development of stachyose production extractive technique, the preparation of high purity stachyose crystallization will and detect measuring means for the research of stachyose basic test and lay a good foundation.
It is raw material that the patent of looking into " preparation method of high purity water threose " (patent No. 200910083903.X) adopts plants such as Rhizome of Bear's-foot Fern, silver bar, and the application of fermentation legal system is equipped with high purity stachyose, and stachyose purity reaches more than 85%.It is raw material that patent " method for preparing the high purity water threose with industrial chromatographic separation technology " (patent No. 200910085212.3) adopts plants such as Rhizome of Bear's-foot Fern, silver bar, uses chromatography and prepares high purity stachyose, and stachyose purity reaches more than 90%.It is raw material separation and Extraction stachyose that patent " red sage root stachyose and its production and use " (number of patent application 201210039455.5) adopts the red sage root, and stachyose purity is more than 80%.Above-mentioned patent is all different with stachyose purifying technique of the present invention, and purity is also different.
Patent " crystallization of carbohydrate " (patent No. 03818058.8) relates to a kind ofly removes crystallization inhibitor by nanofiltration, hydrolysis and/or chromatography from the solution that contains one or more reducing sugars, reducing sugar is selected from fructose and wood sugar.Different with crystallization processes of the present invention, raw material is also different with final product.
Be raw material with the glutinous rehmannia in the paper " preparation of stachyose reference material and osmanthus attached glutinous rehmannia side's polysaccharide quality control method research ", adopted column chromatography means such as macroporous adsorbent resin, gac, silica gel, ODS, obtain purity and be about 99.8% stachyose reference material.Different with purification means of the present invention, the products therefrom state is also different.
In sum, the present invention adopts natural phant silver bar, Rhizome of Bear's-foot Fern, the red sage root, glutinous rehmannia etc. to be raw material, adopt water extraction to carry out recrystallization in conjunction with alcohol extracting method and obtain stachyose purity and be higher than 99.0% crystal, for the preparation of stachyose reference material provides environmental protection thinking easily.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of stachyose crystallization is provided.
Technical scheme of the present invention is summarized as follows:
A kind of preparation method of stachyose crystallization, be made up of following steps:
(1) liquid glucose just prepares: the raw material of selecting to be rich in stachyose comprises plants such as fresh silver bar, Rhizome of Bear's-foot Fern, the red sage root, glutinous rehmannia, raw material is cleaned, squeeze the juice after the hot water lixiviate and get liquid glucose, liquid glucose is evaporated to 30 ~ 50 ° of Brix of refractive power, and in liquid glucose: the ratio of ethanol (V/V)=1:(2-6) adds 95% ethanol, stir, leave standstill back cardboard and filter, filter residue 75% washing with alcohol, filtrate is mixed, at 45～75 ℃ of vacuum concentration to 70～80 ° Bix, get pure molten part medicinal extract;
(2) coarse crystallization: medicinal extract is poured in the insulating container, naturally slowly cooling, after 1-10 days, there is crystalline particulate to occur in medicinal extract inside, and prolong crystal in time and become gradually greatly, adopt the 20-80% ethanolic soln to clean medicinal extract, 30-50 ℃ of vacuum-drying, obtain stachyose purity and be higher than 90% coarse crystallization, collect ethanol filtrate;
(3) liquid glucose refabrication: with step (2) gained stachyose coarse crystallization or commercially available stachyose product (stachyose purity 〉=80%) dissolving, be mixed with the liquid glucose of 10-30 ° of Bix, add the 0.5-1.5% activated carbon decolorizing, be heated to 80 ~ 90 ℃, stir 10-30min, cardboard filter becomes filtrate the liquid glucose of refractive power 40-70 ° Brix at 45～75 ℃ of vacuum concentration;
(4) recrystallization: (3) gained liquid glucose set by step: the ratio of ethanol (V/V)=1:(0.5-2) adds the ethanol of 70-95% purity, the solution post-heating that becomes turbid is stirred to 65 ℃ and keeps 5-20min, place and keep slowly cooling in the insulating container, leave standstill and deposit, transparent diamond crystal particle appearred after 1-7 days, adopt the 30-70% ethanolic soln to clean crystalline particle, collect the ethanol filtrate after cleaning, mix concentrated with ethanol filtrate in the step (2), reclaim ethanol, concentrate liquid glucose for the preparation of ordinary purity stachyose product;
(5) crystalline particle after vacuum-drying will be cleaned carries out vacuum-drying at 30-50 ℃, obtains the stachyose recrystallization.Stachyose content is greater than 99.0% in the crystallization.
Described step (1) is preferably: the raw material of selecting to be rich in stachyose comprises plants such as silver bar, Rhizome of Bear's-foot Fern, the red sage root, glutinous rehmannia, raw material is cleaned, squeeze the juice after the hot water lixiviate and get liquid glucose, liquid glucose is evaporated to 45 ° of Brix of refractive power, and in liquid glucose: the ratio of ethanol (V/V)=1:3 adds 95% ethanol, stir, leave standstill back cardboard and filter, filter residue 75% washing with alcohol, filtrate is mixed, at 60 ℃ of vacuum concentration to 73 ° Bix, get pure molten part medicinal extract.
Described step (2) is preferably: medicinal extract is poured in the insulating container, and slowly cooling naturally is after 4 days, there is crystalline particulate to occur in medicinal extract inside, adopts 50% ethanolic soln to clean medicinal extract, 40 ℃ of vacuum-dryings, obtain the coarse crystallization of stachyose purity about 95%, collect ethanol filtrate.
Described step (3) is preferably: with step (2) gained stachyose coarse crystallization or commercially available stachyose product (stachyose purity 〉=85%) dissolving, be mixed with the liquid glucose of 20 ° of Bix, add 1% activated carbon decolorizing, be heated to 85 ℃, stir 20min, cardboard filter becomes filtrate the liquid glucose of 55 ° of Brix of refractive power at 60 ℃ of vacuum concentration.
Described step (4) is preferably: (3) gained liquid glucose set by step: the ratio of ethanol (V/V)=1:1 adds 90% ethanol, the solution post-heating that becomes turbid is stirred to 65 ℃ and keeps 10min, place and keep slowly cooling in the insulating container, leave standstill to deposit and occur transparent diamond crystal particle after 4 days, adopt 50% ethanolic soln to clean crystalline particle, collect the ethanol filtrate after cleaning, mix concentrated with ethanol filtrate in the step (2), reclaim ethanol, concentrate liquid glucose for the preparation of ordinary purity stachyose product, stachyose purity is about 75% in the product.
Under step (5) preferably: the crystalline particle after will cleaning carries out vacuum-drying at 40 ℃, obtains the stachyose recrystallization, and stachyose content is greater than 99.0% in the crystallization.
Characteristics of the present invention:
1. the present invention adopts crystallization process to prepare the stachyose crystal from natural phant, and the stachyose crystal purity reaches more than 99.0%, for preparation and the relevant Basic Experiment Study of stachyose of stachyose reference material have been laid good basis.
2. the simple environmental protection of solvent adopted in preparation stachyose crystallization processes process of the present invention can recycle and reuse.
3. the present invention is raw material with the natural phant, the technology that adopts water to carry in conjunction with the alcohol extracting crystallization makes purity up to the stachyose crystal more than 99.0%, surplus solution also can be used to prepare the ortho-water threose product of purity about 70%, has improved the utility value of natural phant.
Description of drawings
Accompanying drawing 1 is the HPLC figure of fresh Rhizome of Bear's-foot Fern water extract.
Accompanying drawing 2 is the HPLC figure of fresh Rhizome of Bear's-foot Fern liquid glucose alcohol extracting coarse crystallization.
Accompanying drawing 3 is the HPLC figure of fresh Rhizome of Bear's-foot Fern liquid glucose alcohol extracting stachyose crystallization and the contrast of sigma stachyose standard substance.
The HPLC figure of accompanying drawing 3 fresh Rhizome of Bear's-foot Fern liquid glucose alcohol extracting recrystallizations and the contrast of sigma stachyose standard substance, collection of illustrative plates 1 are the HPLC figure of recrystallization, and collection of illustrative plates 2 is the HPLC figure of stachyose standard substance (cas54261-98-2)
Accompanying drawing 4 is schemed for the HPLC of the ortho-water threose product that the ethanol filtrate of collecting prepares.
Embodiment
The present invention adopts natural phant silver bar, Rhizome of Bear's-foot Fern, the red sage root, glutinous rehmannia etc. for raw material, adopts water extraction to carry out recrystallization in conjunction with alcohol extracting method and obtains stachyose purity and be higher than 99.0% crystal
The present invention is further illustrated below in conjunction with specific embodiment.
Embodiment 1
A kind of preparation method of stachyose crystallization, be made up of following steps:
(1) liquid glucose just prepares: fresh Rhizome of Bear's-foot Fern is cleaned, squeeze the juice after the hot water lixiviate and get liquid glucose, liquid glucose is evaporated to 45 ° of Brix of refractive power, in liquid glucose: the ratio of ethanol (V/V)=1:2 adds 95% ethanol, stirs, and leaves standstill back cardboard and filters, filter residue 75% washing with alcohol, filtrate is mixed, and at 55 ℃ of vacuum concentration to 75 ° Bix, gets pure molten part medicinal extract;
(2) coarse crystallization: medicinal extract is poured in the insulating container, naturally slowly cooling, after 7 days, there is crystalline particulate to occur in medicinal extract inside, and prolongs crystal in time and become gradually greatly, adopt 50% ethanolic soln cleaning medicinal extract, 40 ℃ of vacuum-dryings, obtain the stachyose coarse crystallization, purity is 95.1%, collects ethanol filtrate;
(3) liquid glucose refabrication: with step (2) gained stachyose coarse crystallization dissolving, be mixed with the liquid glucose of 20 ° of Bix, add 1.5% activated carbon decolorizing, be heated to 85 ℃, stir 15min, cardboard filter becomes filtrate the liquid glucose of 55 ° of Brix of refractive power at 60 ℃ of vacuum concentration;
(4) recrystallization: (3) gained liquid glucose set by step: ethanol (V/V)=ratio of 1:1 adds the ethanol of 90% purity, the solution post-heating that becomes turbid is stirred to 65 ℃ and keeps 10min, place and keep slowly cooling in the insulating container, leave standstill and deposit, transparent diamond crystal particle appearred after 5 days, adopt 40% ethanolic soln to clean crystalline particle, collect the ethanol filtrate after cleaning, mix concentrated with ethanol filtrate in the step (2), reclaim ethanol, concentrated liquid glucose prepares ordinary purity stachyose product, and product purity is 75.2%;
(5) crystalline particle after vacuum-drying will be cleaned carries out vacuum-drying at 40 ℃, obtains the stachyose recrystallization.Stachyose purity is 99.8% in the crystallization.
Embodiment 2
A kind of preparation method of stachyose crystallization, be made up of following steps:
(1) liquid glucose just prepares: new Rehmannia Root is cleaned, squeeze the juice after the hot water lixiviate and get liquid glucose, liquid glucose is evaporated to 40 ° of Brix of refractive power, in liquid glucose: the ratio of ethanol (V/V)=1:3 adds 95% ethanol, stirs, and leaves standstill back cardboard and filters, filter residue 75% washing with alcohol, filtrate is mixed, and at 75 ℃ of vacuum concentration to 80 ° Bix, gets pure molten part medicinal extract;
(2) coarse crystallization: medicinal extract is poured in the insulating container, and slowly cooling naturally is after 3 days, there is crystalline particulate to occur in medicinal extract inside, and prolongs crystal in time and become gradually greatly, adopt 70% ethanolic soln cleaning medicinal extract, 50 ℃ of vacuum-dryings obtain that stachyose purity is 92.2% in the coarse crystallization;
(3) liquid glucose refabrication: with step (2) gained stachyose coarse crystallization dissolving, be mixed with the liquid glucose of 30 ° of Bix, add 1% activated carbon decolorizing, be heated to 90 ℃, stir 30min, cardboard filter becomes filtrate the liquid glucose of 65 ° of Brix of refractive power at 75 ℃ of vacuum concentration;
(4) recrystallization: (3) gained liquid glucose set by step: ethanol (V/V)=ratio of 1:0.8 adds the ethanol of 95% purity, the solution post-heating that becomes turbid is stirred to 65 ℃ and keeps 20min, place and keep slowly cooling in the insulating container, leave standstill and deposit, transparent diamond crystal particle appearred after 2 days, adopt 50% ethanolic soln to clean crystalline particle, collect the ethanol filtrate after cleaning, mix concentrated with ethanol filtrate in the step (2), reclaim ethanol, concentrated liquid glucose prepares ordinary purity stachyose product, and product purity is 72%;
(5) crystalline particle after vacuum-drying will be cleaned carries out vacuum-drying at 50 ℃, obtains the stachyose recrystallization.Stachyose is 99.5% in the crystallization.
Experimental example 3
A kind of preparation method of stachyose crystallization, be made up of following steps:
(1) liquid glucose preparation: with commercially available stachyose product (stachyose purity is 86%) dissolving, be mixed with the liquid glucose of 10 ° of Bix, add 0.5% activated carbon decolorizing, be heated to 80 ℃, stir 15min, cardboard filter becomes filtrate the liquid glucose of 30 ° of Brix of refractive power at 45 ℃ of vacuum concentration;
(2) recrystallization: with the gained liquid glucose: ethanol (V/V)=ratio of 1:2 adds the ethanol of 90% purity, the solution post-heating that becomes turbid is stirred to 65 ℃ and keeps 5min, place and keep slowly cooling in the insulating container, leave standstill and deposit, occur transparent diamond crystal particle after 7 days, adopt 60% ethanolic soln to clean crystalline particle, the ethanol filtrate of collecting after cleaning concentrates, reclaim ethanol, the stachyose product purity that concentrated filtrate is prepared is 73%;
(3) vacuum-drying: the crystalline particle after will cleaning carries out vacuum-drying at 30 ℃, obtains the stachyose crystallization.Stachyose content is 99.1% in the crystallization.
Claims (6)
1. the preparation method of a stachyose crystallization, it is characterized in that this method comprises the steps: that (1) liquid glucose just prepares: raw material is cleaned, squeeze the juice after the hot water lixiviate liquid glucose, liquid glucose is evaporated to 30 ~ 50 ° of Brix of refractive power, in liquid glucose: the ratio of ethanol (V/V)=1:(2-6) adds 95% ethanol, stirs, and leaves standstill back cardboard and filters, filter residue 75% washing with alcohol, filtrate is mixed, and at 45～75 ℃ of vacuum concentration to 70～80 ° Bix, gets pure molten part medicinal extract; (2) coarse crystallization; (3) liquid glucose refabrication; (4) recrystallization; (5) vacuum-drying obtains a kind of stachyose purity and is higher than 99.0% stachyose crystallization.
2. the preparation method of a kind of stachyose crystallization according to claim 1, it is characterized in that raw material packet is drawn together plants such as fresh silver bar, Rhizome of Bear's-foot Fern, the red sage root, glutinous rehmannia in the described step (1), squeeze the juice after raw material is clean and get liquid glucose, liquid glucose is evaporated to 30 ~ 50 ° of Brix of refractive power, in liquid glucose: the ratio of ethanol (V/V)=1:(2-6) adds 95% ethanol, stir, leaving standstill back cardboard filters, filter residue 75% washing with alcohol, filtrate is mixed, at 45～75 ℃ of vacuum concentration to 70～80 ° Bix, get pure molten part medicinal extract.
3. the preparation method of a kind of stachyose crystallization according to claim 1, it is characterized in that described step (2) is: medicinal extract is poured in the insulating container, naturally slowly cooling, after 1-10 days, there is crystalline particulate to occur in medicinal extract inside, and prolongs crystal in time and become big gradually, adopt the 20-80% ethanolic soln to clean medicinal extract, 30-50 ℃ of vacuum-drying obtains stachyose purity and is higher than 90% coarse crystallization, collects ethanol filtrate.
4. the preparation method of a kind of stachyose crystallization according to claim 1, it is characterized in that described step (3) is: with step (2) gained stachyose coarse crystallization or commercially available stachyose product (stachyose purity 〉=80%) dissolving, be mixed with the liquid glucose of 10-30 ° of Bix, add the 0.5-1.5% activated carbon decolorizing, be heated to 80 ~ 90 ℃, stir 10-30min, cardboard filter becomes filtrate the liquid glucose of refractive power 40-70 ° Brix at 45～75 ℃ of vacuum concentration.
5. the preparation method of a kind of stachyose crystallization according to claim 1, it is characterized in that described step (4) is: (3) gained liquid glucose set by step: the ratio of ethanol (V/V)=1:(0.5-2) adds the ethanol of 70-95% purity, the solution post-heating that becomes turbid is stirred to 65 ℃ and keeps 5-20min, place and keep slowly cooling in the insulating container, leave standstill and deposit, transparent diamond crystal particle appearred after 1-7 days, adopt the 30-70% ethanolic soln to clean crystalline particle, collect the ethanol filtrate after cleaning, mix concentrated with ethanol filtrate in the step (2), reclaim ethanol, concentrate liquid glucose for the preparation of ordinary purity stachyose product.
6. the preparation method of a kind of stachyose crystallization according to claim 1, it is characterized in that described step (5) is: the crystalline particle after will cleaning carries out vacuum-drying at 30-50 ℃, obtains the stachyose recrystallization, and stachyose content is greater than 99.0% in the crystallization.
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Cited By (4)
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| CN104262418A (en) * | 2014-09-26 | 2015-01-07 | 何龙 | Production method of crystallized water threose |
| CN104621436A (en) * | 2014-10-10 | 2015-05-20 | 浙江玛卡人生生物工程研究所 | Maca extract sugar-removing technology |
| CN105017339A (en) * | 2015-07-01 | 2015-11-04 | 浙江大学 | Method for preparing raffinose and stachyose by simulated-moving-bed chromatographic separation |
| CN106632527A (en) * | 2016-12-19 | 2017-05-10 | 西安源森生物科技有限公司 | Stachyose preparation method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104262418A (en) * | 2014-09-26 | 2015-01-07 | 何龙 | Production method of crystallized water threose |
| CN104621436A (en) * | 2014-10-10 | 2015-05-20 | 浙江玛卡人生生物工程研究所 | Maca extract sugar-removing technology |
| CN104621436B (en) * | 2014-10-10 | 2017-12-15 | 浙江玛卡人生生物工程研究所 | A kind of Maca extract removes sugared technique |
| CN105017339A (en) * | 2015-07-01 | 2015-11-04 | 浙江大学 | Method for preparing raffinose and stachyose by simulated-moving-bed chromatographic separation |
| CN105017339B (en) * | 2015-07-01 | 2018-03-09 | 浙江大学 | A kind of method that SMBC separation prepares raffinose and stachyose |
| CN106632527A (en) * | 2016-12-19 | 2017-05-10 | 西安源森生物科技有限公司 | Stachyose preparation method |
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