CN103232502A - Catalpol preparation method - Google Patents
Catalpol preparation method Download PDFInfo
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- CN103232502A CN103232502A CN 201310179292 CN201310179292A CN103232502A CN 103232502 A CN103232502 A CN 103232502A CN 201310179292 CN201310179292 CN 201310179292 CN 201310179292 A CN201310179292 A CN 201310179292A CN 103232502 A CN103232502 A CN 103232502A
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- catalpol
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- crude extract
- ethyl acetate
- preparing
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- 0 *C(C[C@@]1O)[C@](OC(C2[C@@]3(C=O)O[C@]33)OC=C[C@]2C3(*)O)O[C@](*)*1=O Chemical compound *C(C[C@@]1O)[C@](OC(C2[C@@]3(C=O)O[C@]33)OC=C[C@]2C3(*)O)O[C@](*)*1=O 0.000 description 1
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Abstract
The invention discloses a simple and efficient catalpol preparation method. The simple and efficient catalpol preparation method comprises the following steps of: a. smashing fresh radix rehmanniae, juicing, adding the same volume of 95% alcohol to obtained juice, fully stirring, centrifuging, concentrating centrifugate by a nanofiltration membrane, and carrying out spray drying on a concentrated solution to obtain a crude extract; b. adding the crude extract to ethyl acetate and completely dissolving; filtrating, processing filtrate by an aluminium oxide column, purifying a reagent, which is recycled from liquid processed by column, by adopting high-speed counter-current chromatography, carrying out online monitoring by an ultraviolet detector, collecting a target component according to an atlas, recovering the reagent, and drying under reduced pressure to obtain the catalpol. The simple and efficient catalpol preparation method has the advantages that the process operation is simple, the product yield is high, and the industrial amplification is easy.
Description
Technical field
The invention belongs to the Natural Medicine Chemistry field, particularly relate to a kind of method for preparing Catalpol.
Background technology
Catalpol is iridoid glycoside, molecular formula C
15H
22O
10, molecular weight 362.33, CAS work song 2415-24-9, structural formula:
Catalpol is effective constituent in the scrophulariaceae glutinous rehmannia, and physiologically actives such as anticancer, neuroprotective, anti-inflammatory, diuresis, hypoglycemic and hepatitis virus resisting are arranged.
The existing method for preparing the high purity Catalpol adopts silicagel column to separate or the preparation liquid phase separation.(application number: 200810016005.8) " method of separating Catalpol in the Rehmannia Root " disclosed method is the sample liquid that the broken homogenate of Rehmannia Root must contain Catalpol as patent; Macroporous adsorbent resin separates, and silica gel column chromatography or re-crystallization step realize.Owing to silicagel column separates to the dead absorption of product seriously, reagent dosage is big, and the industrialization amplification is difficult to reappear, and causes existing high purity Catalpol production cost height.And the production of preparation liquid phase, quantum of output is less, and cost is higher.
Summary of the invention
The technical problem that will solve of the present invention provides a kind of efficient, short-cut method for preparing Catalpol.
In order to solve the problems of the technologies described above, the present invention realizes by the following technical solutions:
A kind of method for preparing Catalpol is characterized in that following steps:
The new Rehmannia Root of a is pulverized, and squeezes the juice, and gained juice adds equal-volume 95% ethanol, fully stirs, and is centrifugal, and centrifugate concentrates with nanofiltration membrane, and the concentrated solution spraying drying gets crude extract;
The above-mentioned crude extract of b adds ethyl acetate and fully dissolves, filters, and filtrate peroxidation aluminium post, lower column liquid reclaims reagent and adopts the high speed adverse current chromatogram purifying, and the UV-detector on-line monitoring is collected target component according to collection of illustrative plates, reclaims reagent, and drying under reduced pressure is namely.
Described nanofiltration membrane is the hollow cellulose film of molecular weight cut-off 200-300.
The optional ethyl acetate of solvent systems, methyl alcohol, water solvent system that described high speed adverse current chromatogram separates, blending ratio 1-10:1-7:1-9 gets the phase that fixes mutually, does moving phase down mutually.
Utilize the present invention to prepare Catalpol, method is simple to operate, the product yield height, and solvent utilization ratio height is easy to realize suitability for industrialized production.
Embodiment:
Further specify the present invention below in conjunction with embodiment.
Embodiment 1:
New Rehmannia Root is pulverized 10kg, squeeze the juice, gained juice adds equal-volume 95% ethanol, fully stirs, centrifugal, the nanofiltration membrane that centrifugate adds molecular retention amount 200 concentrates, and the concentrated solution spraying drying gets crude extract 430g, getting the 4000ml ethyl acetate fully dissolves, filter, filtrate is crossed the neutral alumina post, lower column liquid concentrate medicinal extract 35g.Get ethyl acetate, methyl alcohol, water by the 3:1:3 mixed, fully after the layering, get and inject the high speed adverse current chromatogram pipe phase that fixes mutually, start main frame, rotating speed 900rpm pumps into down and do moving phase mutually simultaneously, after the balance, flow velocity 2ml/min is set, dissolves concentrated solution with moving phase simultaneously, inject high-speed counter-current chromatograph, flow point is collected in the online detection of UV-detector, preparation continuously, drying under reduced pressure gets white powder 12g, detect content 98.1% through HPLC.
Embodiment 2:
New Rehmannia Root is pulverized 10kg, squeeze the juice, gained juice adds equal-volume 95% ethanol, fully stirs, centrifugal, the nanofiltration membrane that centrifugate adds molecular retention amount 300 concentrates, and the concentrated solution spraying drying gets crude extract 340g, getting the 3000ml ethyl acetate fully dissolves, filter, filtrate is crossed the neutral alumina post, lower column liquid concentrate medicinal extract 27g.Get ethyl acetate, methyl alcohol, water by the 5:2:7 mixed, fully after the layering, get and inject the high speed adverse current chromatogram pipe phase that fixes mutually, start main frame, rotating speed 800rpm pumps into down and do moving phase mutually simultaneously, after the balance, flow velocity 3ml/min is set, dissolves concentrated solution with moving phase simultaneously, inject high-speed counter-current chromatograph, flow point is collected in the online detection of UV-detector, preparation continuously, drying under reduced pressure gets white powder 16.7g, detect content 98.9% through HPLC.
Embodiment 3:
New Rehmannia Root is pulverized 10kg, squeeze the juice, gained juice adds equal-volume 95% ethanol, fully stirs, centrifugal, the nanofiltration membrane that centrifugate adds molecular retention amount 200 concentrates, and the concentrated solution spraying drying gets crude extract 450g, getting the 3000ml ethyl acetate fully dissolves, filter, filtrate is crossed the neutral alumina post, lower column liquid concentrate medicinal extract 31g.Get ethyl acetate, methyl alcohol, water by the 6:2:9 mixed, fully after the layering, get and inject the high speed adverse current chromatogram pipe phase that fixes mutually, start main frame, rotating speed 700rpm pumps into down and do moving phase mutually simultaneously, after the balance, flow velocity 1ml/min is set, dissolves concentrated solution with moving phase simultaneously, inject high-speed counter-current chromatograph, flow point is collected in the online detection of UV-detector, preparation continuously, drying under reduced pressure gets white powder 13.1g, detect content 97.2% through HPLC.
Claims (3)
1. method for preparing Catalpol is characterized in that following steps:
The new Rehmannia Root of a is pulverized, and squeezes the juice, and gained juice adds equal-volume 95% ethanol, fully stirs, and is centrifugal, and centrifugate concentrates with nanofiltration membrane, and the concentrated solution spraying drying gets crude extract;
The above-mentioned crude extract of b adds ethyl acetate and fully dissolves, filters, and filtrate peroxidation aluminium post, lower column liquid reclaims reagent and adopts the high speed adverse current chromatogram purifying, and the UV-detector on-line monitoring is collected target component according to collection of illustrative plates, reclaims reagent, and drying under reduced pressure is namely.
2. the method for preparing Catalpol according to claim 1 is characterized in that the nanofiltration membrane described in the step a is the hollow cellulose film of molecular weight cut-off 100-300.
3. the method for preparing Catalpol according to claim 1, it is characterized in that the optional ethyl acetate of solvent systems, methyl alcohol, water solvent system that the high speed adverse current chromatogram described in the step b separates, blending ratio 1-10:1-7:1-9 gets the phase that fixes mutually, does moving phase down mutually.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201310179292 CN103232502A (en) | 2013-05-15 | 2013-05-15 | Catalpol preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201310179292 CN103232502A (en) | 2013-05-15 | 2013-05-15 | Catalpol preparation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103232502A true CN103232502A (en) | 2013-08-07 |
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ID=48880581
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201310179292 Pending CN103232502A (en) | 2013-05-15 | 2013-05-15 | Catalpol preparation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113480581A (en) * | 2021-07-21 | 2021-10-08 | 湖南朗林生物资源股份有限公司 | Method for extracting iridoid glycoside from rehmannia |
-
2013
- 2013-05-15 CN CN 201310179292 patent/CN103232502A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113480581A (en) * | 2021-07-21 | 2021-10-08 | 湖南朗林生物资源股份有限公司 | Method for extracting iridoid glycoside from rehmannia |
| CN113480581B (en) * | 2021-07-21 | 2022-05-24 | 湖南朗林生物资源股份有限公司 | Method for extracting iridoid glycoside from rehmannia |
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| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130807 |