CN109232287A - A kind of isolation and purification method of fructus lycii glycine betaine - Google Patents
A kind of isolation and purification method of fructus lycii glycine betaine Download PDFInfo
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- CN109232287A CN109232287A CN201810886819.0A CN201810886819A CN109232287A CN 109232287 A CN109232287 A CN 109232287A CN 201810886819 A CN201810886819 A CN 201810886819A CN 109232287 A CN109232287 A CN 109232287A
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- fructus lycii
- glycine betaine
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
Abstract
The present invention discloses a kind of isolation and purification method of fructus lycii glycine betaine, the specific steps are as follows: fructus lycii dries in the shade indoors first, shreds, is centrifuged obtained leaching liquor after water-bath extraction, obtains supernatant I；After I vacuum-concentrcted of supernatant, dehydrated alcohol precipitating is added except sugar, obtains mixed liquor, mixed liquor is centrifuged, and obtains supernatant II, after II vacuum-concentrcted of supernatant, obtains medicinal extract；Appropriate distilled water dissolution is added in the medicinal extract, obtains sample solution；Sample solution is successively obtained after cation exchange resin, anion exchange resin to fructus lycii glycine betaine crude product；The glycine betaine crude product is obtained into supernatant III after ethanol washing, centrifugation, separation；The supernatant III is placed in sample bottle and is concentrated to dryness, fructus lycii glycine betaine is obtained.The present invention provides a kind of low in cost, good fructus lycii glycine betaine isolation and purification method of purification effect.
Description
Technical field
The invention belongs to the purification technique fields of glycine betaine, and in particular to a kind of side of isolating and purifying of fructus lycii glycine betaine
Method.
Background technique
Glycine betaine is found in Europe first, it is primarily present in the molasses of beet sugar, so gain the name.Glycine betaine is general
All over being formed in the bodies of aminal and plant, it is the intermediate product of animal metabolism, is played a very important role in the metabolism of nutriment,
It is widely used in feed for livestock, using also very universal in aquatic feeds and animal for display feed.In addition, beet
Alkali also acts as food additives, and the food such as manufacture textured vegetable protein have good promotion to care of aged and upgrowth and development of children
Effect.Glycine betaine is also the raw material of pharmaceuticals industry, can be used for producing the drug for the treatment of hepatopathy.
Fructus lycii is the traditional Chinese medicine in China, is the dry of Lycium barbarum L. of solanaceae (Lycium barbarum L.)
Dry ripening fruits, alias beet.Fructus lycii has enhancing and adjusts immune function, reduce blood pressure, promote uterus weight and resist
Cancer, antifatigue and growth stimulation.Fructus lycii main component is polysaccharides, carrotene, glycine betaine etc..Glycine betaine is Chinese holly
One of main component of matrimony vine, pharmacology and clinical research in recent years show that the compound has and promote fat metabolism, anti-cellulite
The multiple pharmacological effects such as liver, protection kidney, decompression, mitigation stress, improve a poor appetite, stable vitamin.
The research of content assaying method is concentrated mainly on to betaine in lycium Chinese at present, and fructus lycii glycine betaine is divided
It is less from purifying report.Glycine betaine trophic function is abundant, healthy and safe, few side effects.Foreign countries have been widely used in health
In raw-food material and dietary supplements, such as ursodeoxycholic acid, South Korea's liver-protecting preparation pharmaceutical and energy drink, the cream system in the U.S.
The foodstuffs such as product；Additionally using its as function raw material flavour enhancer, preservative, in terms of in apply.Therefore,
The market prospects of glycine betaine are boundless.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of low in cost, the good fructus lycii glycine betaine of purification effect point
From purification process.
To solve the above problems, a kind of isolation and purification method of fructus lycii glycine betaine of the present invention, including following step
It is rapid:
Step 1: it will dry in the shade in fructus lycii room, obtain fructus lycii dry sample；
Step 2: fructus lycii dry sample is shredded, and obtains the broken sample of fructus lycii；
Step 3: by the broken sample of fructus lycii and water by mass volume ratio 1:5g/mL~1:100g/mL of feed liquid in 10~70 DEG C of items
After water-bath extracts 0.5~4 h under part, leaching liquor is obtained；
Step 4: after the leaching liquor that step 3 is obtained is centrifuged, supernatant I and filter residue I are obtained；
Step 5: by the supernatant I under the conditions of 45~60 DEG C after vacuum-concentrcted, 6 times of volumes are added in concentrate
Dehydrated alcohol mixing obtains mixed liquor except sugar；
Step 6: the mixed liquor is centrifuged, and obtains supernatant II and filter residue II；
Step 7: the supernatant II after vacuum-concentrcted, is obtained into medicinal extract under the conditions of 45~60 DEG C；
Step 8: suitable distilled water is added in the medicinal extract and is dissolved, sample solution is obtained；
Step 9: by the sample solution after cationic exchange resin adsorption, being first washed till eluent with Enough Dl water is in
It is faint yellow or colourless, then the glycine betaine being adsorbed on cation exchange resin is eluted with the ammonium hydroxide of 2 ~ 6 times of bed volumes, contained
The eluent of fructus lycii glycine betaine；
Step 10: by the eluent of the glycine betaine containing fructus lycii after anion exchange resin adsorbs, with 2 ~ 6 times of bed volumes
Deionized water elution after collect efflux, and by efflux after vacuum-concentrcted, obtain fructus lycii glycine betaine concentrate；
Step 11: the fructus lycii glycine betaine concentrate is lyophilized, fructus lycii glycine betaine crude product is obtained；
Step 12: by the fructus lycii glycine betaine crude product through ethanol washing, centrifugation, separation, supernatant III and filter residue III are obtained；
Step 13: the supernatant III is placed in sample bottle and is concentrated to dryness, fructus lycii glycine betaine is obtained.
The condition of drying in the shade of interior described in the step 1 is that room temperature dries in the shade one week and is rolled into section to fructus lycii.
Preferably, cation exchange resin described in step 9 is 732 type cation exchange resins.
Preferably, the volumetric concentration of ammonium hydroxide described in step 9 is 5%.
Preferably, anion exchange resin described in step 10 is 717 type anion exchange resin.
Compared with prior art, the beneficial effects of the present invention are: (1) this method is easy to operate, and required reagent price is low
Honest and clean, gained fructus lycii glycine betaine purity is higher, can be used for industrial production；(2) preparation process is noiseless dry with toxic reagent
In advance, and energy consumption is lower, and technique is ideal.
Specific embodiment
Embodiment 1
A kind of isolation and purification method of fructus lycii glycine betaine, comprising the following steps:
(1) fructus lycii normal temperature laboratory is dried in the shade one week and is rolled into section to get fructus lycii dry sample to fructus lycii.
(2) fructus lycii dry sample is shredded, obtains the broken sample of fructus lycii.
(3) the broken sample of the fructus lycii is mixed with water by the feed liquid mass volume ratio of 1:20g/mL, after 60 DEG C of extraction 4h,
Obtain leaching liquor.
(4) leaching liquor is obtained into supernatant I and filter residue I after 8000r/min is centrifuged 15min；
(5) by the supernatant I after 60 DEG C of vacuum-concentrcteds, 6 times of volume dehydrated alcohol mixing is added in concentrate and remove
Sugar obtains mixed liquor；
(6) mixed liquor is obtained into supernatant II and filter residue II after 8000r/min is centrifuged 15min.
(7) supernatant II after vacuum-concentrcted, is obtained into medicinal extract at 60 DEG C, appropriate double steamings is added in the medicinal extract
Water dissolution, obtains sample solution.
(8) sample solution is first washed till elution with Enough Dl water after 732 type cationic exchange resin adsorptions
Liquid is in beet that is faint yellow or colourless, then being adsorbed on 732 type cation exchange resins with the ammonium hydroxide elution of 4 times of bed volumes
Alkali obtains the eluent of the glycine betaine containing fructus lycii, and the volumetric concentration of ammonium hydroxide is 5% herein.
(9) by the eluent of the glycine betaine containing fructus lycii after the absorption of 717 type anion exchange resin, with 2 times of beds
The deionized water of volume elutes, and collects efflux.The efflux obtains the concentration of fructus lycii glycine betaine after vacuum-concentrcted
Liquid.
(10) the fructus lycii glycine betaine concentrate is lyophilized, obtains fructus lycii glycine betaine crude product.
(11) by the fructus lycii glycine betaine crude product through ethanol washing twice, 8000r/min be centrifuged 15min after, obtain supernatant
The supernatant III is placed in sample bottle and is concentrated to dryness, obtains fructus lycii glycine betaine by liquid III and filter residue.
Through high performance liquid chromatography detection, the content of the fructus lycii glycine betaine is 87.94%.
Embodiment 2
A kind of isolation and purification method of fructus lycii glycine betaine, comprising the following steps:
(1) fructus lycii normal temperature laboratory is dried in the shade one week and is rolled into section to get fructus lycii dry sample to fructus lycii.
(2) fructus lycii dry sample is shredded, obtains the broken sample of fructus lycii.
(3) the broken sample of the fructus lycii is mixed with water by the feed liquid mass volume ratio of 1:5g/mL, in 10 DEG C of 0.5 h of extraction
Afterwards, leaching liquor is obtained.
(4) leaching liquor is obtained into supernatant I and filter residue I after 8000r/min is centrifuged 15min；
(5) by the supernatant I after 45 DEG C of vacuum-concentrcteds, 6 times of volume dehydrated alcohol mixing is added in concentrate and remove
Sugar obtains mixed liquor；
(6) mixed liquor is obtained into supernatant II and filter residue II after 8000r/min is centrifuged 15min.
(7) supernatant II after vacuum-concentrcted, is obtained into medicinal extract at 45 DEG C, appropriate double steamings is added in the medicinal extract
Water dissolution, obtains sample solution.
(8) sample solution is first washed till elution with Enough Dl water after 732 type cationic exchange resin adsorptions
Liquid is in beet that is faint yellow or colourless, then being adsorbed on 732 type cation exchange resins with the ammonium hydroxide elution of 2 times of bed volumes
Alkali obtains the eluent of the glycine betaine containing fructus lycii, and the volumetric concentration of ammonium hydroxide is 5% herein.
(9) by the eluent of the glycine betaine containing fructus lycii after the absorption of 717 type anion exchange resin, with 4 times of beds
The deionized water of volume elutes, and collects efflux.The efflux obtains the concentration of fructus lycii glycine betaine after vacuum-concentrcted
Liquid.
(10) the fructus lycii glycine betaine concentrate is lyophilized, obtains fructus lycii glycine betaine crude product.
(11) by the fructus lycii glycine betaine crude product through ethanol washing twice, 8000r/min be centrifuged 15min after, obtain supernatant
The supernatant III is placed in sample bottle and is concentrated to dryness, obtains fructus lycii glycine betaine by liquid III and filter residue.
Through high performance liquid chromatography detection, the content of the fructus lycii glycine betaine is 81.54%.
Embodiment 3
A kind of isolation and purification method of fructus lycii glycine betaine, comprising the following steps:
(1) fructus lycii normal temperature laboratory is dried in the shade one week and is rolled into section to get fructus lycii dry sample to fructus lycii.
(2) fructus lycii dry sample is shredded, obtains the broken sample of fructus lycii.
(3) the broken sample of the fructus lycii is mixed with water by the feed liquid mass volume ratio of 1:100g/mL, in 70 DEG C of 3 h of extraction
Afterwards, leaching liquor is obtained.
(4) leaching liquor is obtained into supernatant I and filter residue I after 8000r/min is centrifuged 15min；
(5) by the supernatant I after 50 DEG C of vacuum-concentrcteds, 6 times of volume dehydrated alcohol mixing is added in concentrate and remove
Sugar obtains mixed liquor；
(6) mixed liquor is obtained into supernatant II and filter residue II after 8000r/min is centrifuged 15min.
(7) supernatant II after vacuum-concentrcted, is obtained into medicinal extract at 50 DEG C, appropriate double steamings is added in the medicinal extract
Water dissolution, obtains sample solution.
(8) sample solution is first washed till elution with Enough Dl water after 732 type cationic exchange resin adsorptions
Liquid is in beet that is faint yellow or colourless, then being adsorbed on 732 type cation exchange resins with the ammonium hydroxide elution of 6 times of bed volumes
Alkali obtains the eluent of the glycine betaine containing fructus lycii, and the volumetric concentration of ammonium hydroxide is 5% herein.
(9) by the eluent of the glycine betaine containing fructus lycii after the absorption of 717 type anion exchange resin, with 6 times of beds
The deionized water of volume elutes, and collects efflux.The efflux obtains the concentration of fructus lycii glycine betaine after vacuum-concentrcted
Liquid.
(10) the fructus lycii glycine betaine concentrate is lyophilized, obtains fructus lycii glycine betaine crude product.
(11) by the fructus lycii glycine betaine crude product through ethanol washing twice, 8000r/min be centrifuged 15min after, obtain supernatant
The supernatant III is placed in sample bottle and is concentrated to dryness, obtains fructus lycii glycine betaine by liquid III and filter residue.
Through high performance liquid chromatography detection, the content of the fructus lycii glycine betaine is 88.36%.
Claims (5)
1. a kind of isolation and purification method of fructus lycii glycine betaine, which is characterized in that this method specifically includes the following steps:
Step 1: it will dry in the shade in fructus lycii room, obtain fructus lycii dry sample；
Step 2: fructus lycii dry sample is shredded, and obtains the broken sample of fructus lycii；
Step 3: by the broken sample of fructus lycii and water by mass volume ratio 1:5g/mL~1:100g/mL of feed liquid in 10~70 DEG C of items
After water-bath extracts 0.5~4 h under part, leaching liquor is obtained；
Step 4: after the leaching liquor that step 3 is obtained is centrifuged, supernatant I and filter residue I are obtained；
Step 5: by the supernatant I under the conditions of 45~60 DEG C after vacuum-concentrcted, 6 times of volumes are added in concentrate
Dehydrated alcohol mixing obtains mixed liquor except sugar；
Step 6: the mixed liquor is centrifuged, and obtains supernatant II and filter residue II；
Step 7: the supernatant II after vacuum-concentrcted, is obtained into medicinal extract under the conditions of 45~60 DEG C；
Step 8: suitable distilled water is added in the medicinal extract and is dissolved, sample solution is obtained；
Step 9: by the sample solution after cationic exchange resin adsorption, being first washed till eluent with Enough Dl water is in
It is faint yellow or colourless, then the glycine betaine being adsorbed on cation exchange resin is eluted with the ammonium hydroxide of 2 ~ 6 times of bed volumes, contained
The eluent of fructus lycii glycine betaine；
Step 10: by the eluent of the glycine betaine containing fructus lycii after anion exchange resin adsorbs, with 2 ~ 6 times of bed volumes
Deionized water elution after collect efflux, and by efflux after vacuum-concentrcted, obtain fructus lycii glycine betaine concentrate；
Step 11: the fructus lycii glycine betaine concentrate is lyophilized, fructus lycii glycine betaine crude product is obtained；
Step 12: by the fructus lycii glycine betaine crude product through ethanol washing, centrifugation, separation, supernatant III and filter residue III are obtained；
Step 13: the supernatant III is placed in sample bottle and is concentrated to dryness, fructus lycii glycine betaine is obtained.
2. a kind of isolation and purification method of fructus lycii glycine betaine according to claim 1, which is characterized in that institute in step 1
Stating interior condition of drying in the shade is that room temperature dries in the shade one week and is rolled into section to fructus lycii.
3. a kind of isolation and purification method of fructus lycii glycine betaine according to claim 1, which is characterized in that institute in step 9
Stating cation exchange resin is 732 type cation exchange resins.
4. a kind of isolation and purification method of fructus lycii glycine betaine according to claim 1, which is characterized in that institute in step 9
The volumetric concentration for stating ammonium hydroxide is 5%.
5. a kind of isolation and purification method of fructus lycii glycine betaine according to claim 1, which is characterized in that institute in step 10
The anion exchange resin stated is 717 type anion exchange resin.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111202688A (en) * | 2020-01-23 | 2020-05-29 | 青海大学 | Moisturizing cosmetic containing lycium barbarum betaine and preparation method thereof |
| CN115554183A (en) * | 2022-09-23 | 2023-01-03 | 江苏华汀生物科技股份有限公司 | Facial skin care product and preparation method thereof |
| CN115779017A (en) * | 2022-12-28 | 2023-03-14 | 青海大学 | Medlar betaine effervescent tablet with liver protection effect and preparation method and application thereof |
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| WO1981002420A1 (en) * | 1980-02-29 | 1981-09-03 | Suomen Sokeri Oy | Betaine recovery process |
| CN104829474A (en) * | 2015-05-27 | 2015-08-12 | 中国科学院西北高原生物研究所 | Method for preparing glycine betaine chemical reference substances from boxthorn leaves |
| CN106242986A (en) * | 2016-07-30 | 2016-12-21 | 成都薇诺娜生物科技有限公司 | Fructus Lycii root is used to extract the preparation method of glycine betaine |
| CN108358822A (en) * | 2018-02-14 | 2018-08-03 | 西北农林科技大学 | A method of continuously extracting a variety of active ingredients from matrimony vine cull fruit |
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2018
- 2018-08-06 CN CN201810886819.0A patent/CN109232287A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1981002420A1 (en) * | 1980-02-29 | 1981-09-03 | Suomen Sokeri Oy | Betaine recovery process |
| CN104829474A (en) * | 2015-05-27 | 2015-08-12 | 中国科学院西北高原生物研究所 | Method for preparing glycine betaine chemical reference substances from boxthorn leaves |
| CN106242986A (en) * | 2016-07-30 | 2016-12-21 | 成都薇诺娜生物科技有限公司 | Fructus Lycii root is used to extract the preparation method of glycine betaine |
| CN108358822A (en) * | 2018-02-14 | 2018-08-03 | 西北农林科技大学 | A method of continuously extracting a variety of active ingredients from matrimony vine cull fruit |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111202688A (en) * | 2020-01-23 | 2020-05-29 | 青海大学 | Moisturizing cosmetic containing lycium barbarum betaine and preparation method thereof |
| CN115554183A (en) * | 2022-09-23 | 2023-01-03 | 江苏华汀生物科技股份有限公司 | Facial skin care product and preparation method thereof |
| CN115779017A (en) * | 2022-12-28 | 2023-03-14 | 青海大学 | Medlar betaine effervescent tablet with liver protection effect and preparation method and application thereof |
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