CN1504473A - Resin adsorption process for preparing tannin from sea-buckthorn leaf - Google Patents
Resin adsorption process for preparing tannin from sea-buckthorn leaf Download PDFInfo
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- CN1504473A CN1504473A CNA021539197A CN02153919A CN1504473A CN 1504473 A CN1504473 A CN 1504473A CN A021539197 A CNA021539197 A CN A021539197A CN 02153919 A CN02153919 A CN 02153919A CN 1504473 A CN1504473 A CN 1504473A
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- tannin
- folium hippophae
- resin
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- aqueous ethanolic
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Abstract
The invention relates to a process for preparing tannin from sea-buckthorn leaves through resin adsorption method which comprises the steps of, (1) extracting sea-buckthorn leaves using 40-95% ethanol aqueous solution as dissolvent at the temperature of 20-90 deg.C, combining the extract liquid, filtering the reclaimed ethanol, obtaining extract liquid by centrifugation, (2) going through the disposed large hole adsorption resin tower, (3) water scrubbing until the driving off liquid becomes colorless, elution and reclaiming ethanol, vacuum drying to obtain brown to light brown extract. The invention realizes simple process thus can be applied in mass production.
Description
Technical field
The present invention relates to a kind of method that from Folium Hippophae, prepares tannin with resin adsorption method.
Technical background
Do not see the report that from Folium Hippophae, extracts tannin at present both at home and abroad as yet.Our current research has been found activeconstituents---tannin class material new in the Folium Hippophae.The Folium Hippophae tannin all has remarkable pharmacological action at anti peroxidation of lipid, detoxifcation, anti-mutation, anti-inflammatory, aspect such as hypotensive, and DEVELOPMENT PROSPECT is very wide.We have determined the method that is equipped with the Folium Hippophae tannin with the macroporous adsorbent resin legal system.
Summary of the invention
Technical problem to be solved by this invention provide a kind of technology simple, be easy to suitability for industrialized production from Folium Hippophae, prepare the method for tannin with resin adsorption method.
The technical solution used in the present invention is as follows: (1) is that solvent extracts Folium Hippophae down at 20～90 ℃ with 40～95% aqueous ethanolic solutions, the weight ratio of Folium Hippophae and solvent is 1: 8～15, extracts more than 2 times or 2 times united extraction liquid, filtered and recycled ethanol, the centrifugal extracting solution that gets; (2) make flow velocity the macroporous adsorbent resin tower by handle of said extracted liquid with 0.5～3BV/h; (3) clean resin tower with pure water, colourless to effluent liquid, carry out wash-out with 40～95% aqueous ethanolic solutions with the flow velocity of 0.5～3BV/h then, after collecting elutriant and reclaiming ethanol, vacuum-drying, brown to the light brown extract.
In the technical solution of the present invention, can be at first with the Folium Hippophae coarse reduction, the most handy 50～60% aqueous ethanolic solution is a solvent, 80 ℃ of refluxing extraction three times.
In the technical solution of the present invention, ethanol extract can add finings after reclaiming ethanol, leaves standstill to wait to precipitate the centrifugal precipitation of removing in complete back, gets clear liquor, the macroporous resin tower by handling well again.
Finings of the present invention can adopt chitosan, ZTC finings, 101 finingss, JA finings or the sun 1+1 of section finings, and the add-on of finings is 0.05～0.2% (the best is 0.15～0.18%) of filtrate weight.
Macroporous adsorbent resin of the present invention can be nonpolar, Semi-polarity or strong polar macroporous adsorption resin.
In the technical solution of the present invention, the most handy 50～60% aqueous ethanolic solution carries out wash-out.
Be that solvent extracts Folium Hippophae with 40～95% aqueous ethanolic solutions in the technical solution of the present invention, extract more than 2 times or 2 times that each extraction time is 40 minutes to 8 hours.
In the technical solution of the present invention during macroporous adsorbent resin tower of extracting solution by handling well flow velocity be preferably 0.6～1.2BV/h.
In the technical solution of the present invention, when carrying out wash-out with aqueous ethanolic solution, flow velocity preferably is controlled at 0.6～1.2BV/h.
Positively effect of the present invention is as follows: adopt technology of the present invention can extract activeconstituents new in the Folium Hippophae---tannin class material, the Folium Hippophae tannin all has remarkable pharmacological action at anti peroxidation of lipid, detoxifcation, anti-mutation, anti-inflammatory, aspect such as hypotensive, DEVELOPMENT PROSPECT is very wide, the present invention is simple for process, is easy to suitability for industrialized production.
Embodiment
Technology of the present invention is as follows: Folium Hippophae → extraction using alcohol → filtration → filtrate recycling ethanol → centrifugal → extracting solution → go up macroporous adsorbent resin tower → ethanolic soln wash-out → elutriant to reclaim ethanol → vacuum-drying → finished product.
Also can adopt following technological process: Folium Hippophae → extraction using alcohol → filtration → filtrate recycling ethanol → add finings → centrifugal → clear liquor → last macroporous adsorbent resin tower → ethanolic soln wash-out → elutriant to reclaim ethanol → vacuum-drying → finished product.
Below in conjunction with embodiment technology of the present invention is described in detail.
Embodiment 1:
The Folium Hippophae coarse reduction of (1) drying in the shade, aqueous ethanolic solution with 40% (the most handy 60%) is a solvent, and 20 ℃ are soaked extraction down, and the weight ratio of Folium Hippophae and solvent is 1: 8, lixiviate 4 times, for the first time 8h, 6h, 4h for the third time for the second time, the 4th 2h, united extraction liquid filters through the duplex filter, gets filtrate.
(2) with the centrifugal extracting solution that gets behind the above-mentioned filtrate recycling ethanol, or will add chitosan or ZTC finings behind the filtrate recycling ethanol, its add-on is 0.05% of a filtrate weight, the best is 0.15%, stir, leave standstill and wait to precipitate the centrifugal precipitation of removing in complete back, get clear liquor.
(3) said extracted liquid (or clear liquor) is with the strong polar macroporous adsorption resin tower of 0.5BV/h flow velocity by handling well, it is colourless to be washed till effluent liquid with pure water, carry out wash-out with 40% aqueous ethanolic solution with the 2BV/h flow velocity then, collect elutriant, reclaim ethanol final vacuum drying, temperature is controlled at 60 ℃, gets the light brown extract, content of tannin 38.2%.
Embodiment 2:
The Folium Hippophae coarse reduction of (1) drying in the shade, aqueous ethanolic solution with 70% (being preferably 50%) is that solvent soaks the extraction Folium Hippophae down three times 50 ℃ (being preferably 80 ℃), 2h for the first time, twice is each 40 minutes in addition, the weight ratio of Folium Hippophae and solvent is 1: 15, united extraction liquid filters through the duplex filter, gets filtrate.
(2) with the centrifugal extracting solution that gets behind the above-mentioned filtrate recycling ethanol, or will add chitosan or 101 finingss behind the filtrate recycling ethanol, its add-on is 0.20% of a filtrate weight, the best is 0.15%, stir, leave standstill and wait to precipitate the centrifugal precipitation of removing in complete back, get clear liquor.
(3) said extracted liquid (or clear liquor) is with the 3BV/h flow velocity, by the AB-8 type Semi-polarity macroporous adsorbent resin tower of handling well, it is colourless to be washed till effluent liquid with pure water, carry out wash-out with 60% aqueous ethanolic solution with the 3BV/h flow velocity then, collect elutriant, reclaim ethanol final vacuum drying, temperature is controlled at 55 ℃, gets the light brown extract, content of tannin 41.5%.
Embodiment 3:
The Folium Hippophae coarse reduction of (1) drying in the shade is a solvent with the aqueous ethanolic solution of 95% (being preferably 55%), at 90 ℃ of following refluxing extraction Folium Hippophae secondaries, 1.5h for the first time, 1h for the second time, the weight ratio of Folium Hippophae and solvent is 1: 12, united extraction liquid filters through the duplex filter, gets filtrate.
(2) with the centrifugal extracting solution that gets behind the above-mentioned filtrate recycling ethanol, or will add chitosan or JA finings or the sun 1+1 of section finings behind the filtrate recycling ethanol, its add-on is 0.11% of a filtrate weight, the best is 0.18%, stirs, and leaves standstill, wait to precipitate the centrifugal precipitation of removing in complete back, get clear liquor.
(3) said extracted liquid (or clear liquor) is with the 1.8BV/h flow velocity, by the ZTC type polar macroporous adsorption resin tower of handling well, it is colourless to be washed till effluent liquid with pure water, carry out wash-out with 95% aqueous ethanolic solution with the 0.5BV/h flow velocity then, collect elutriant, reclaim ethanol final vacuum drying, temperature is controlled at 65 ℃, gets the light brown extract, content of tannin 54.3%.
Embodiment 4:
The Folium Hippophae coarse reduction of (1) drying in the shade, the aqueous ethanolic solution with 50% are solvent, and 80 ℃ of following refluxing extraction, the weight ratio of Folium Hippophae and solvent are 1: 8, lixiviate 3 times, 3h, 2h, 1h for the third time for the second time for the first time, united extraction liquid filters through the duplex filter, gets filtrate.
(2) with the centrifugal extracting solution that gets behind the above-mentioned filtrate recycling ethanol, or will add ZTC finings or 101 finingss behind the filtrate recycling ethanol, its add-on is 0.15% of a filtrate weight, stirs, and leaves standstill to wait to precipitate the centrifugal precipitation of removing in complete back, gets clear liquor.
(3) said extracted liquid (or clear liquor) is with the nonpolar macroporous adsorption resin of 0.6BV/h flow velocity by handling well, it is colourless to be washed till effluent liquid with pure water, carry out wash-out with 50% aqueous ethanolic solution with the 0.6BV/h flow velocity then, collect elutriant, reclaim ethanol final vacuum drying, temperature is controlled at 55 ℃, gets the light brown extract, content of tannin 52.6%.
Embodiment 5:
The Folium Hippophae coarse reduction of (1) drying in the shade, the aqueous ethanolic solution with 55% are solvent, and 40 ℃ are soaked extraction down, and the weight ratio of Folium Hippophae and solvent is 1: 12, lixiviate 3 times, 6h, 4h, 2h for the third time for the second time for the first time, united extraction liquid filters through the duplex filter, gets filtrate.
(2) with the centrifugal extracting solution that gets behind the above-mentioned filtrate recycling ethanol, or will add ZTC finings or the sun 1+1 of section finings behind the filtrate recycling ethanol, its add-on is 0.17% of a filtrate weight, stirs, and leaves standstill to wait to precipitate the centrifugal precipitation of removing in complete back, gets clear liquor.
(3) said extracted liquid (or clear liquor) is with the Semi-polarity macroporous adsorbent resin tower of 1.2BV/h flow velocity by handling well, it is colourless to be washed till effluent liquid with pure water, carry out wash-out with 60% aqueous ethanolic solution with the 1.2BV/h flow velocity then, collect elutriant, reclaim ethanol final vacuum drying, temperature is controlled at 60 ℃, gets the light brown extract, content of tannin 49%.
Embodiment 6:
The Folium Hippophae coarse reduction of (1) drying in the shade, the aqueous ethanolic solution with 60% are solvent, and 60 ℃ are soaked extraction down, and the weight ratio of Folium Hippophae and solvent is 1: 15, lixiviate 3 times, 4h, 2h, 1h for the third time for the second time for the first time, united extraction liquid filters through the duplex filter, gets filtrate.
(2) with the centrifugal extracting solution that gets behind the above-mentioned filtrate recycling ethanol, or will add chitosan or JA finings behind the filtrate recycling ethanol, its add-on is 0.18% of a filtrate weight, stirs, and leaves standstill to wait to precipitate the centrifugal precipitation of removing in complete back, gets clear liquor.
(3) said extracted liquid (or clear liquor) is with the strong polar macroporous adsorption resin tower of 0.9BV/h flow velocity by handling well, it is colourless to be washed till effluent liquid with pure water, carry out wash-out with 55% aqueous ethanolic solution with the 0.9BV/h flow velocity then, collect elutriant, reclaim ethanol final vacuum drying, temperature is controlled at 65 ℃, gets the light brown extract, content of tannin 48.2%.
Claims (10)
1, a kind of method that from Folium Hippophae, prepares tannin with resin adsorption method, it is characterized in that it comprises the steps: that (1) is that solvent extracts Folium Hippophae down at 20～90 ℃ with 40～95% aqueous ethanolic solutions, the weight ratio of Folium Hippophae and solvent is 1: 8～15, extract more than 2 times or 2 times, united extraction liquid, filtered and recycled ethanol, the centrifugal extracting solution that gets; (2) make flow velocity the macroporous adsorbent resin tower by handle of said extracted liquid with 0.5～3BV/h; (3) it is colourless to effluent liquid to clean resin tower with pure water, carries out wash-out with 40～95% aqueous ethanolic solutions with the flow velocity of 0.5～3BV/h then, and after collecting elutriant and reclaiming ethanol, vacuum-drying must be brown to the light brown extract.
2, a kind of method that from Folium Hippophae, prepares tannin with resin adsorption method according to claim 1, it is characterized in that to add finings after ethanol extract reclaims ethanol, leave standstill and wait to precipitate the centrifugal precipitation of removing in complete back, get clear liquor, macroporous resin tower again by handling well.
3, a kind of method that from Folium Hippophae, prepares tannin with resin adsorption method according to claim 2, it is characterized in that described finings can adopt chitosan, ZTC finings, 101 finingss, JA finings or the sun 1+1 of section finings, the add-on of finings is 0.05～0.2% (the best is 0.15～0.18%) of filtrate weight.
4, describedly a kind ofly from Folium Hippophae, prepare the method for tannin according to claim 1,2 or 3, it is characterized in that at first with the Folium Hippophae coarse reduction, the most handy 50～60% aqueous ethanolic solution is a solvent, 80 ℃ of refluxing extraction three times with resin adsorption method.
5, describedly a kind ofly from Folium Hippophae, prepare the method for tannin according to claim 1,2 or 3, it is characterized in that described macroporous adsorbent resin can be nonpolar, Semi-polarity or strong polar macroporous adsorption resin with resin adsorption method.
6, describedly a kind ofly from Folium Hippophae, prepare the method for tannin according to claim 1,2 or 3, it is characterized in that the most handy 50～60% aqueous ethanolic solution carries out wash-out with resin adsorption method.
7, according to claim 1,2 or 3 described a kind of methods that from Folium Hippophae, prepare tannin with resin adsorption method, it is characterized in that with 40～95% aqueous ethanolic solutions being that solvent extracts Folium Hippophae, extract more than 2 times or 2 times, each extraction time is 40 minutes～8 hours.
8, describedly a kind ofly prepare the method for tannin with resin adsorption method from Folium Hippophae according to claim 1,2 or 3, flow velocity is preferably 0.6～1.2BV/h when it is characterized in that the macroporous adsorbent resin tower of extracting solution by handling well.
9, describedly a kind ofly prepare the method for tannin with resin adsorption method from Folium Hippophae according to claim 1,2 or 3, when it is characterized in that carrying out wash-out with aqueous ethanolic solution, flow velocity preferably is controlled at 0.6～1.2BV/h.
10, according to claim 1,2 or 3 described a kind of methods that from Folium Hippophae, prepare tannin with resin adsorption method, it is characterized in that carrying out after wash-out reclaims ethanol with aqueous ethanolic solution, vacuum-drying, temperature are controlled between 55～65 ℃, get brown to the light brown extract.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA021539197A CN1504473A (en) | 2002-12-05 | 2002-12-05 | Resin adsorption process for preparing tannin from sea-buckthorn leaf |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA021539197A CN1504473A (en) | 2002-12-05 | 2002-12-05 | Resin adsorption process for preparing tannin from sea-buckthorn leaf |
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| CN1504473A true CN1504473A (en) | 2004-06-16 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102058631A (en) * | 2010-12-22 | 2011-05-18 | 天津泰阳制药有限公司 | Seabuckthorn leaf extract preparation and preparation method thereof |
| CN102451251A (en) * | 2011-12-26 | 2012-05-16 | 中国科学院新疆理化技术研究所 | Method for preparing effective hypoglycemic parts of quince fruits and application of effective hypoglycemic parts |
| CN102532209A (en) * | 2010-12-24 | 2012-07-04 | 苏州宝泽堂医药科技有限公司 | Preparation method of oleaster tannin |
| CN109694394A (en) * | 2018-12-07 | 2019-04-30 | 兰州大学 | The preparation method and its usage of tannin extract in a kind of sea-buckthorn |
-
2002
- 2002-12-05 CN CNA021539197A patent/CN1504473A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102058631A (en) * | 2010-12-22 | 2011-05-18 | 天津泰阳制药有限公司 | Seabuckthorn leaf extract preparation and preparation method thereof |
| CN102058631B (en) * | 2010-12-22 | 2012-10-03 | 天津泰阳制药有限公司 | Seabuckthorn leaf extract preparation and preparation method thereof |
| CN102532209A (en) * | 2010-12-24 | 2012-07-04 | 苏州宝泽堂医药科技有限公司 | Preparation method of oleaster tannin |
| CN102451251A (en) * | 2011-12-26 | 2012-05-16 | 中国科学院新疆理化技术研究所 | Method for preparing effective hypoglycemic parts of quince fruits and application of effective hypoglycemic parts |
| CN102451251B (en) * | 2011-12-26 | 2014-03-12 | 中国科学院新疆理化技术研究所 | Method for preparing effective hypoglycemic parts of quince fruits and application of effective hypoglycemic parts |
| CN109694394A (en) * | 2018-12-07 | 2019-04-30 | 兰州大学 | The preparation method and its usage of tannin extract in a kind of sea-buckthorn |
| CN109694394B (en) * | 2018-12-07 | 2022-08-09 | 兰州大学 | Preparation method and application of tannin extract in sea buckthorn |
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