CN102863439A - Method for extracting yohimbine hydrochloride from yohimbe barks - Google Patents
Method for extracting yohimbine hydrochloride from yohimbe barks Download PDFInfo
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- CN102863439A CN102863439A CN 201110188916 CN201110188916A CN102863439A CN 102863439 A CN102863439 A CN 102863439A CN 201110188916 CN201110188916 CN 201110188916 CN 201110188916 A CN201110188916 A CN 201110188916A CN 102863439 A CN102863439 A CN 102863439A
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Abstract
The invention discloses a method for extracting refined yohimbine hydrochloride with high content from yohimbe (Pausinystalia Yohimbe) barks, which comprises the following steps of: (1) grinding yohimbe barks into powder, and heating and extracting with a mixed solvent of acid and alcohol aqueous solution; (2) filtrating an extracting solution to remove impurities, carrying out medium absorption on a resin column, eluting with 5-60% ethanol aqueous solution, and concentrating and drying in vacuum; (3) recrystallizing with 5-75% ethanol or methanol aqueous solution with 10-30 times of weight of the extracting solution to obtain a product with content of 95-100% and color from yellow to light yellow; and (4) decoloring through an adsorbing medium to obtain whitish yohimbine hydrochloride with high content and off-white color. The method fills the blank of a technology of domestic large-scale production of yohimbine hydrochloride, turns waste of the wild plants native to the West Africa region into wealth, serves human health, and creates good economic and social benefits.
Description
Technical field
The present invention relates to a kind of method of from yohimbe bark, extracting refining high-content Yomax, related in particular to a kind of high-content, color is the preparation method of the Yomax of off-white color.
Background technology
Yohimbe formal name used at school Pausinystalia Yohimbe, it is a kind of plant that is grown in West Africa, contain abundant alkaloid, Yohimbine (Yohimbine) is first by FDA by becoming the prescription drugs for the treatment of impotence, its Main Function comes from the α of blocking-up on the nervus centralis-2adrenergic susceptor, can expand reproductive organ periphery blood vessel, so that the fully congested infull problem of erecing that solves has 34%-43% user therefrom to benefit in the clinical experiment in 1987.
The johimbine sterling is white powder, is slightly soluble in water, is dissolved in ethanol, chloroform, and hot benzene is slightly soluble in ether.The johimbine that extracts from Ghana's yohimbe bark can effectively improve male sexual disorder, it is reported in the Pansinystalia Yohimba bark that dries, mix the content of Yohimbine biology total alkali up to more than 6.1%, its major portion is johimbine, so plant extract has greatly the prospect of exploitation.In the formulation of the johimbine medicine that has gone on the market, only have two kinds of formulations of Tablet and Capsula.The pharmacological action of johimbine is strong, dosage is little, molecular weight is little, and becomes Yomax behind the hydrochloric acid salify, and it is water-soluble to improve greatly, easily sees through the characteristics such as keratoderma, meets and makes transdermal therapeutic system.
In the at present external patent report, the plant extraction process of Yohimbine is comparatively simple, and the extraction of its extracting method and other biology total alkali is similar, and main leaching process comprises: the adding extraction of solvent; Alkaloidal precipitation; Separation and refining.The lyase that uses mostly is greatly the larger organic solvents of toxicity such as industrial naptha, chloroform or benzene, although the pigment magazine is less in the extract, dissolvent residual serious harm user's is healthy.Separate and refiningly usually can use Physical or chemical method.When content is larger, the method such as can adopt alkaloidal crystallization process or distill; When content is low, can adopt ion-exchange-resin process etc., the method heavy by acid can transform into johimbine water-soluble better Yomax.The Yomax sterling is white powder, is slightly soluble in water, is dissolved in ethanol, chloroform, and hot benzene is slightly soluble in ether.And it is at present domestic and have no the patent report of the extraction process for purification of relevant Yomax.After isolating johimbine in 1900, the medicine workers have carried out years of researches to aspects such as the chemical structure of johimbine and character always, have finally determined the steric configuration of its structural formula in nineteen forty-three, and clear and definite its degradation pathway.WoodWard has at first synthesized johimbine in 1958 with chemical process, after this, constantly has the people that this synthetic route is improved.
Summary of the invention
The invention provides a kind of simple and easy, with low cost, as to be fit to suitability for industrialized production high purity Yomax extraction process for purification that operates.
The technical solution used in the present invention is:
1. one kind is extracted the method made from extra care the high-content Yomax from yohimbe bark, it is characterized in that may further comprise the steps:
(1) yohimbe bark being broken into granularity is 10 to 100 purpose small-particles, extracts with the pure mixed solvent of the water of pH=1～6, extracts temperature and is controlled at 40～100 ℃, and extraction time is 0.5～72 hour,
(2) extracting liquid filtering is removed impurity after, upper resin column carries out medium absorption, the aqueous ethanolic solution wash-out effective constituent with 5～60%, vacuum concentration is dry,
(3) with 10～30 times of ethanol or methanol aqueous solution recrystallizations of 5%～75% to its weight, obtain content 95～100%, color is yellow～lurid product,
(4) use the adsorption mediums such as gac or neutral alumina to decolour, obtain content 97～100%, color is the high-content Yomax of off-white color.
4. the breaking method in the above-mentioned steps (1) adopts the medicinal material crusher to carry out fragmentation, and particle size after cracking is preferably 20～60 orders.
5. the water that be used for the to extract alcohol mixed solvent in the above-mentioned steps (1) can be that 0～60% aqueous ethanolic solution or 0～40% methanol aqueous solution or the two are according to 1:(0.5～2) the mixing solutions of ratio proportioning, its pH value is preferably 2～4.
6. the adsorption medium in the above-mentioned steps (2) can be one or more series connection uses of strongly-acid gel type cation exchange resin, slightly acidic large pores cation exchange resin, macroporous absorption type resin.
7. the aqueous ethanolic solution that is used for wash-out effective constituent in the above-mentioned steps (2), its volume fraction is preferably 20 ~ 50%.
8. be used for the ethanol of recrystallization or the volume fraction of methanol aqueous solution in the above-mentioned steps (3) and be preferably 15～65%.
In the above-mentioned steps (4) method of decolouring for yellow～lurid product in the above-mentioned steps (3) being dissolved in 20～30 times in 30～80% ethanol or methanol aqueous solution of its weight, add gac or the neutral alumina of lyase weight 0.1～0.5%, 40～60 ℃ of lower whip attachment 0.5～4 hour.
10. the method for decolouring is that with the sorbent material filtering, clear liquid was concentrated into 10～20% of original volume after whip attachment finished in the above-mentioned steps (4), and cooling is left standstill, centrifuging and taking crystallization, decompression or constant pressure and dry.
The invention has the beneficial effects as follows:
The present invention has filled up the technological gap of domestic large-scale production Yomax, and the wild plant that originates in the area, West Africa is turned waste into wealth, and serves human health, has created good economic and social benefit.
Embodiment
Embodiment 1:
1) pre-treatment: yohimbe bark is ground into 20～60 order powderies;
2) extract: place the PH=3 of 20 times of raw material weights, 30% ethanol solution hydrochloride to extract 2 times the raw material after the fragmentation, temperature is 85 ℃;
3) filter to get clear liquid, put to room temperature;
4) column chromatography: with 3) adsorbing with the macroporous type polymeric adsorbent, is colourless with washed with de-ionized water resin to effluent liquid, carries out wash-out with 50% ethanol and separates, and 50% alcohol moiety is evaporated to without ethanol, leaves standstill;
5) with 4) centrifugal, 70 ~ 75 ℃ of normal pressure oven dry of gained precipitation get 80% Yomax;
6) recrystallization: with 5) with 15 times of 60% ethanol heating for dissolving, let cool crystallization, the oven dry of crystallization normal pressure gets 98% light yellow Yomax.
7) decolouring: with 6) with 15 times of 50% ethanol heating for dissolving, the gac of adding 0.2%, 45 ~ 48 ℃ of whip attachment 2h filter to get clear liquid, let cool crystallization, and 98% Yomax of off-white color is dried to get in crystallization.
Embodiment 2:
1) pre-treatment: yohimbe bark is ground into 20～60 order powderies;
2) extract: place the PH=2 of 20 times of raw material weights, 50% ethanol solution hydrochloride to extract 2 times the raw material after the fragmentation, temperature is 70 ℃;
3) filter to get clear liquid, put to room temperature;
4) column chromatography: with 3) adsorb with the macroporous type polymeric adsorbent, it is colourless cleaning resin to effluent liquid with 30% ethanol, carries out wash-out with 55% ethanol and separates, and 55% alcohol moiety is evaporated to without ethanol, leaves standstill;
5) with 4) centrifugal, 70 ~ 75 ℃ of normal pressure oven dry of gained precipitation get 80% Yomax;
6) recrystallization: with 5) with 15 times of 60% ethanol heating for dissolving, let cool crystallization, the oven dry of crystallization normal pressure gets 98% yellow Yomax.
7) decolouring: with 6) with 15 times of 50% ethanol heating for dissolving, the gac of adding 0.5%, 45 ~ 48 ℃ of whip attachment 1h filter to get clear liquid, let cool crystallization, and 98% Yomax of off-white color is dried to get in crystallization.
Embodiment 3:
1) pre-treatment: yohimbe bark is ground into 20～60 order powderies;
2) extract: place the PH=2 hydrochloric acid soln of 20 times of raw material weights to extract 2 times the raw material after the fragmentation, temperature is 70 ℃;
3) filter to get clear liquid, put to room temperature;
4) column chromatography: with 3) adsorbing with the macroporous type polymeric adsorbent, is colourless with washed with de-ionized water resin to effluent liquid, carries out wash-out with 55% ethanol and separates, and 55% alcohol moiety is evaporated to without ethanol, leaves standstill;
5) with 4) centrifugal, 70 ~ 75 ℃ of normal pressure oven dry of gained precipitation get 75% Yomax;
6) recrystallization: with 5) with 15 times of 60% ethanol heating for dissolving, let cool crystallization, the oven dry of crystallization normal pressure gets 98% yellow Yomax.
7) decolouring: with 6) with 15 times of 50% ethanol heating for dissolving, the neutral alumina of adding 0.2%, 55 ~ 58 ℃ of whip attachment 2h filter to get clear liquid, let cool crystallization, and 98% Yomax of off-white color is dried to get in crystallization.
Claims (8)
1. one kind is extracted the method made from extra care the high-content Yomax from yohimbe bark, it is characterized in that may further comprise the steps:
The first step, it is 10 to 100 purpose small-particles that yohimbe bark is broken into granularity, extracts with the pure mixed solvent of the water of pH=1～6, extracts temperature and is controlled at 40～100 ℃, extraction time is 0.5～72 hour;
Second step, extracting liquid filtering removed impurity after, upper resin column carries out medium absorption, the aqueous ethanolic solution wash-out effective constituent with 5～60%, vacuum concentration is dry;
The 3rd step with 10～30 times of ethanol or methanol aqueous solution recrystallizations of 5%～75% to its weight, obtained content 95～100%, and color is yellow～lurid product;
The 4th step, use the adsorption mediums such as gac or neutral alumina to decolour, obtain content 97～100%, color is the high-content Yomax of off-white color.
2. the method for extracting refining high-content Yomax from yohimbe bark according to claim 1 it is characterized in that the breaking method in the first step adopts the medicinal material crusher to carry out fragmentation, and particle size after cracking is preferably 20～60 orders.
3. the method for from yohimbe bark, extracting refining high-content Yomax according to claim 1, it is characterized in that the water that be used for to extract alcohol mixed solvent in the first step can be that 0～60% aqueous ethanolic solution or 0～40% methanol aqueous solution or the two are according to 1:(0.5～2) the mixing solutions of ratio proportioning, its pH value is preferably 2～4.
4. the method for extracting refining high-content Yomax from yohimbe bark according to claim 1 is characterized in that the adsorption medium in the second step can be one or more series connection uses of strongly-acid gel type cation exchange resin, slightly acidic large pores cation exchange resin, macroporous absorption type resin.
5. the method for extracting refining high-content Yomax from yohimbe bark according to claim 1 is characterized in that the aqueous ethanolic solution that is used for wash-out effective constituent in the second step, and its volume fraction is preferably 20 ~ 50%.
6. the method for extracting refining high-content Yomax from yohimbe bark according to claim 1 is characterized in that being preferably 15～65% for the ethanol of recrystallization or the volume fraction of methanol aqueous solution in the 3rd step.
7. the method for from yohimbe bark, extracting refining high-content Yomax according to claim 1, it is characterized in that the method for decolouring in the 4th step is for being dissolved in 20～30 times in 30～80% ethanol or methanol aqueous solution of its weight with yellow～lurid product in the 3rd step, add gac or the neutral alumina of lyase weight 0.1～0.5%, 40～60 ℃ of lower whip attachment 0.5～4 hour.
According to claim 1 with the 7 described methods of from yohimbe bark, extracting refining high-content Yomax, the method that it is characterized in that decolouring in the 4th step is after whip attachment finishes, with the sorbent material filtering, clear liquid is concentrated into 10～20% of original volume, cooling is left standstill, the centrifuging and taking crystallization, decompression or constant pressure and dry.
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| CN 201110188916 CN102863439A (en) | 2011-07-07 | 2011-07-07 | Method for extracting yohimbine hydrochloride from yohimbe barks |
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| CN 201110188916 CN102863439A (en) | 2011-07-07 | 2011-07-07 | Method for extracting yohimbine hydrochloride from yohimbe barks |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015172399A1 (en) * | 2014-05-12 | 2015-11-19 | 四川圣湖生物科技有限公司 | Pharmaceutical composition for improving male sexual dysfunction |
| CN111777606A (en) * | 2020-06-05 | 2020-10-16 | 太阳树（厦门）生物工程有限公司 | Method for extracting yohimbine from yohimbine bark |
| CN112999156A (en) * | 2021-03-03 | 2021-06-22 | 宁波御坊堂生物科技有限公司 | Yohimbine hydrochloride synergistic erection-assisting time-delay essential oil spray and preparation method thereof |
-
2011
- 2011-07-07 CN CN 201110188916 patent/CN102863439A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015172399A1 (en) * | 2014-05-12 | 2015-11-19 | 四川圣湖生物科技有限公司 | Pharmaceutical composition for improving male sexual dysfunction |
| CN111777606A (en) * | 2020-06-05 | 2020-10-16 | 太阳树（厦门）生物工程有限公司 | Method for extracting yohimbine from yohimbine bark |
| CN111777606B (en) * | 2020-06-05 | 2021-10-15 | 太阳树（厦门）生物工程有限公司 | Method for extracting yohimbine from yohimbine bark |
| CN112999156A (en) * | 2021-03-03 | 2021-06-22 | 宁波御坊堂生物科技有限公司 | Yohimbine hydrochloride synergistic erection-assisting time-delay essential oil spray and preparation method thereof |
| CN112999156B (en) * | 2021-03-03 | 2023-09-08 | 宁波御坊堂生物科技有限公司 | Erection-assisting time-delay essential oil spray with synergistic yohimbine hydrochloride and preparation method thereof |
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Application publication date: 20130109 |