CN100564392C - A kind of extraction of triterpene compound, preparation method - Google Patents
A kind of extraction of triterpene compound, preparation method Download PDFInfo
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- CN100564392C CN100564392C CNB2006100257923A CN200610025792A CN100564392C CN 100564392 C CN100564392 C CN 100564392C CN B2006100257923 A CNB2006100257923 A CN B2006100257923A CN 200610025792 A CN200610025792 A CN 200610025792A CN 100564392 C CN100564392 C CN 100564392C
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Abstract
The invention discloses extraction, the preparation method of a kind of triterpene compound Colosolic acid (CRA).CRA has the effect of controlling blood sugar, can be used for treating glycosuria, fat-reducing etc.With the Banaba leaf through nontoxic lower alcohol extraction, extracting solution after filtration, filtrate is by the macroporous type polymeric adsorbent, use the hydrophilic solvent desorb, collect CRA desorb position, through vacuum concentration, obtain product after the lyophilize, detecting the CRA product purity by high performance liquid chromatography is 20%～60%.The inventive method has that technology is simple, product purity is high, with short production cycle, advantage that cost is cheap relatively, meets environmental protection and safe requirement, is suitable for the scale suitability for industrialized production.
Description
Technical field
The invention belongs to the vegetable chemistry technical field, be specifically related to extraction, the preparation method of a kind of triterpene compound Colosolicacid (CRA).
Background technology
Colosolic acid (CRA) is a kind of natural product, and it mainly is present in the leaf of plant Lagerstroemiaspeciosa.In South East Asia, the leaf of this kind of plant is used as herbtherapy diabetes, controlling obesity always and is extensive use of.Filipine Tagalog claims that this plant is Banaba, thereby gain the name " Ba Naba ".Show that after deliberation CRA is the main active ingredient of Banaba, relevant report proof CRA can reduce the blood sugar of test white mouse and the test white mouse that suffers from hereditary diabetes is had hypoglycemic activity, CRA can activate the transmission of glucose, therefore can lowering blood glucose, effect with treatment diabetes, fat-reducing, praise promising glucokinin one title, can be applicable to fields such as medicine, food, protective foods.Therefore the extraction preparation method who researchs and develops CRA has important practical significance.
Extract present report seldom about the preparation of CRA, the Banaba plant is used as local herbal medicine to some extent in South East Asia, but in international academic research, not to the pharmacokinetic of CRA, report is not relevant yet tests the human body effect.CRA has confirmed its pharmaceutical use as the pure natural plants extract in the people's prolonged application of South East Asia, but the preparation extraction of CRA is not still had effective means.
Summary of the invention:
Technical problem to be solved by this invention is to study a kind ofly extracts the production method of CRA product from Banaba, and Environmental Safety, cycle are short, simple to operate, the technology of energy suitability for industrialized production.
The invention provides the extraction preparation method of a kind of triterpene compound Colosolic acid (CRA).
The inventive method with the Banaba leaf through water carry, alcohol extracting, extract CRA to greatest extent, extracting solution filters through 1-0.45 micron membranes strainer, removes undissolved impurity.Adopt the nonpolar or low-pole resin of macroporous type to adorn post as stopping composition, under 20～60 ℃, CRA in the extracting solution is adsorbed, and with between gradient zones in 40%～95% low-alcohol solution desorb, collection contains the cut of CRA, and cut vacuum concentration to the solid content that collection is obtained is to carry out lyophilize at 25% o'clock, and concentrated solution is carried out making finished product after the lyophilize, this finished product detects through HPLC, and the CRA product content is 20～60%.
Method of the present invention specifically comprises the following steps:
(1) the Banaba leaf is immersed in the nontoxic rudimentary (C that 8-10 doubly measures
2-C
3) extract 3 times each 2-3 hour in the alcohol;
(2) extracting solution is used 0.1-0.5 μ micro-filtrate membrane filtration, filtrate merga pass macroporous adsorbent resin;
(3) will adsorb the nontoxic lower alcohol flushing of saturated macroporous adsorbent resin with gradient, dominant discharge 4-5BV/h desorbs CRA, and stripping liquid detects by HPLC, collects to be rich in the CRA part;
(4) stripping liquid obtains the CRA product through 80 ℃ of vacuum concentration, lyophilize, detects with HPLC, and content is 20～60%.
Present method adopts is to adopt the nonpolar or low-pole polymeric adsorbent of macroporous type that CRA is carried out fractionation by adsorption, utilizes the absorption of the nonpolar or low-pole resin CRA of team of macropore and can wash-out under the lower alcohol condition of suitable concn goes out the principle of CRA.Effectively enrichment CRA, the CRA content in the products obtained therefrom can be risen to 20～60%, theoretical yield is 80%～90%.
The inventive method has that technology is simple, product purity is high, with short production cycle, advantage that cost is low.It is 20%～60% that the CRA product that adopts the inventive method to extract preparation detects purity through HPL.
Description of drawings:
The HPLC of Fig. 1 CRA product detects, and retention time is that the peak of 12.146min is the CRA signal among the figure.
Specific embodiment
Embodiment one.
Take by weighing Banaba leaf 500g, with 8 times of 4 liters of 40% ethanol of amount, refluxing extraction 4 times is used ethanol 4L at every turn, and each extracted 60 minutes, united extraction liquid, with extracting solution with 0.1 μ micro-filtrate membrane filtration.Get the D101 resin 300g dress post that cleans up, extracting solution is passed through this resin, flow velocity 3BV/h.At first use 40% ethanol of 1L, the flushing resin; Use the flow velocity wash-out CRA of 80% ethanol of 1.5L then, collect this stream part with 3BV/h.With elutriant under 60 vacuum concentration to about 500ml, then with the concentrated solution lyophilize.Obtain the CRA powder, be weighed as 9.72g, detect through the HPLC external standard method, CRA content is 21.06%, and the rate of recovery is 81.9%.
Embodiment two.
Take by weighing Banaba leaf 300g, with 6 times of amount 60% n-propyl alcohol 3L, refluxing extraction 3 times is used n-propyl alcohol 3L at every turn, and each extracted 80 minutes, united extraction liquid, with extracting solution with 0.2 μ film vacuum filtration.Get the ADS-5 resin 300g dress post that cleans up, by this resin, flow velocity is 3BV/h with extracting solution.At first the n-propyl alcohol with 1L60% washes resin; Use the flow velocity wash-out CRA of 80% n-propyl alcohol of 1.5L then, collect this flow point with 2BV/h.With elutriant under 70 vacuum concentration to 500ml, then with the concentrated solution lyophilize.The CRA powder weighing that obtains is 2.72g, detects through the HPLC external standard method, and CRA content is 29.58%, and the rate of recovery is 53.7%.
Embodiment three.
Take by weighing Banaba leaf 200g, with 6 times of amount 70% Virahol 4L, refluxing extraction 3 times is used Virahol 4L at every turn, and each extracted 80 minutes, and united extraction liquid is with extracting solution 8000 rev/mins of processing of whizzer.Get the HP20 resin 100g dress post that cleans up, by this resin, flow velocity is 3BV/h with centrifugal gained extracting solution.At first with 600ml 70% Virahol flushing resin; Use the flow velocity wash-out CRA of the Virahol of 800ml 90% then, collect this flow point with 2BV/h.With elutriant under 70 vacuum concentration to 300ml, then with the concentrated solution lyophilize.Obtain the CRA powder, be weighed as 0.654g, detect through the HPLC external standard method, CRA content is 51.38%, the rate of recovery 33.6%.
Claims (4)
1, the present invention discloses extraction, the preparation method of a kind of triterpene compound Colosolic acid, it is characterized in that this method comprises the following steps:
(1) the Banaba leaf is immersed in the C of 8-10 times of raw material weight
2-C
3Extract in the alcohol, extract 3 times, each 2-3 hour;
(2) extracting solution is used 0.1-0.5 μ micro-filtrate membrane filtration, filtrate merga pass macroporous adsorbent resin;
(3) will adsorb the C of saturated macroporous adsorbent resin with gradient
2-C
3The alcohol flushing, dominant discharge 4-5BV/h, desorb Colosolic acid, stripping liquid detects by HPLC appearance method, collects to be rich in Colosolic acid part;
(4) be 20～25% o'clock with stripping liquid through 80 ℃ of vacuum concentration to solids content, lyophilize obtains Colosolic acid product, detects with HPLC appearance method, and content is 20～60%.
2, extraction, the preparation method of a kind of triterpene compound Colosolic acid according to claim 1 is characterized in that wherein said raw material must select for use Colosolic acid content at the plant Banaba leaf more than 0.5%.
3, extraction, the preparation method of a kind of triterpene compound Colosolic acid according to claim 1 is characterized in that wherein said macroporous adsorbent resin is styrene tyle macroporous nonpolar or low-pole resin: macroporous resin D series, ADS series, HP series or Amberlite XAD.
4, extraction, the preparation method of a kind of triterpene compound Colosolic acid according to claim 1 is characterized in that described hydrophilic organic solvent is ethanol or propyl alcohol.
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| CNB2006100257923A CN100564392C (en) | 2006-04-18 | 2006-04-18 | A kind of extraction of triterpene compound, preparation method |
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| CN101058596A CN101058596A (en) | 2007-10-24 |
| CN100564392C true CN100564392C (en) | 2009-12-02 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1578669A (en) * | 2001-08-31 | 2005-02-09 | 俄亥俄州立大学 | Compositions and methods for treating subjects with hyperglycemia |
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| CN1578669A (en) * | 2001-08-31 | 2005-02-09 | 俄亥俄州立大学 | Compositions and methods for treating subjects with hyperglycemia |
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