CN102274319A - Preparation method of rhomotoxine hydrolysis product - Google Patents
Preparation method of rhomotoxine hydrolysis product Download PDFInfo
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- CN102274319A CN102274319A CN2011102068999A CN201110206899A CN102274319A CN 102274319 A CN102274319 A CN 102274319A CN 2011102068999 A CN2011102068999 A CN 2011102068999A CN 201110206899 A CN201110206899 A CN 201110206899A CN 102274319 A CN102274319 A CN 102274319A
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Abstract
The invention provides a preparation method of a rhomotoxine hydrolysis product. The method comprises the following steps of: performing ester hydrolysis, amide hydrolysis and acidification on rhomotoxine serving as a reaction substrate; and performing resin desalination and a subsequent process to obtain the rhomotoxine hydrolysis product. The preparation method has the advantage that: the obtained rhomotoxine hydrolysis product is water-soluble and is easy for a human body to absorb. On the other hand, the rhomotoxine hydrolysis product can be adsorbed on resin, so that the hydrolysis product can be purified by using resin; and the resin can be recycled without being regenerated, so that the production process is simplified, the production cost is lowered, and the realization of continuous production is facilitated. The method has the advantages of simple reaction process, high efficiency, easiness for controlling, simple process, low energy consumption and high product purity. The rhomotoxine hydrolysis product prepared with the method has characteristic absorption at the position of 224 nanometers, high water solubility and low toxicity, and can well keep the drug action.
Description
Technical field
The present invention relates to a kind of preparation method of Rhomotoxine hydrolyzate.
Background technology
The Chinese medicine Ramulus Uncariae Cum Uncis is the buckle branch of Maguireothamnus speciosus Ramulus Uncariae Cum Uncis.Ramulus Uncariae Cum Uncis (
Uncaria rhynchophylla) various in style, comprise 15 kinds of Ramulus Uncariae Cum Uncis, Ramulus Uncariae macrophyllae, Ramulus Uncariae Cum Uncis, Uncaria sinensis (Oliv.) Havil. or stockless fruit Ramulus Uncariae Cum Uncis etc., be distributed widely in China west and south, be a kind of can tame medicinal plants, aboundresources.Rhomotoxine is the deep processed product of Ramulus Uncariae Cum Uncis, can be used for diseases such as hypertension, dizzy, the dysphoric cold of headache.Yet along with the continuous popularization that Rhomotoxine is used, its water-fast characteristics have limited the application of Rhomotoxine to a certain extent.
Chinese invention patent application 200710098441 and 20071009990 discloses a kind of production method of Ramulus Uncariae Cum Uncis total alkaloids, utilizes cation exchange resin separating uncaria rhynchophylla total alkaloids from Chinese medicine extraction liquid.The former adopts cation exchange resin column absorption to be neutral Ramulus Uncariae Cum Uncis extracting solution, reuse 0.5%～15% acid solution eluting, and eluent prepares the Ramulus Uncariae Cum Uncis total alkaloids through neutralization, desalination, drying process again; The latter soaks cation exchange resin column with 0.5%～20% saline solution, again containing acid or alcoholic acid 0.5%～20% saline solution eluting, eluent again through desalination, concentrate, drying process makes the Ramulus Uncariae Cum Uncis total alkaloids.Though these two patents have been improved the production technology of Rhomotoxine, the Rhomotoxine that makes is water insoluble, is unfavorable for absorption of human body.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of Rhomotoxine hydrolyzate, this method is passed through preparation Rhomotoxine hydrolyzate, thereby improves water solublity, widens the application of Rhomotoxine.
The present invention is reaction substrate with the Rhomotoxine, carries out ester hydrolysis, amide hydrolysis and acidify, then by desalination and subsequent technique, and preparation Rhomotoxine hydrolyzate.
The present invention is achieved through the following technical solutions:
Because the main effective ingredient of Rhomotoxine is a Ramulus Uncariae cum Uncis alkali, thus following be the realization that example illustrates technical scheme with the Ramulus Uncariae cum Uncis alkali.
At first, aqueous slkali joined carry out alkaline hydrolysis in the container that Rhomotoxine is housed, reaction disconnects the amido link of Ramulus Uncariae cum Uncis alkali and ester bond, sloughs aniline and methanol groups, generates carboxylate soluble in water.Because amide, ester hydrolysis can be reacted in excessive aqueous slkali thoroughly, therefore final Ramulus Uncariae cum Uncis alkali is with complete hydrolysis.Its reaction equation is as follows:
Alkaline hydrolysis adds acid for adjusting pH after finishing in system, make the carboxylate acidify of generation generate carboxylic acid, and acidifying solution is pumped in the container that resin is housed, and comes the purified water hydrolysis products by absorption and alcohol desorption.Subsequent techniques such as the ethanolysis imbibition warp of collecting concentrates, drying obtain Ramulus Uncariae cum Uncis alkali hydrolyzate powder.Its reaction equation is as follows:
The Ramulus Uncariae cum Uncis alkali hydrolyzate
The preparation method of a kind of Rhomotoxine hydrolyzate of the present invention comprises the steps:
1. reaction substrate: Rhomotoxine;
2. alkaline hydrolysis: in reaction substrate, add aqueous slkali and carry out alkaline hydrolysis;
3. acidify: after alkaline hydrolysis finishes, filter, collect alkali solution liquid, add acid solution and carry out acidify, regulator solution is to pH2.0～pH5.0;
4. desalination: after acidify finishes, filter, collect acidifying solution, acidifying solution is pumped in the container that resin is housed adsorb, the resin after saturated is through alcohol desorption;
5. dry, pulverizing: the ethanolysis imbibition that 4. step is obtained concentrates, dried, and the dried powder that obtains is the Rhomotoxine hydrolyzate.
The step 2. concentration of described aqueous slkali is 0.1mol/L～5.0mol/L; The alkaline hydrolysis temperature is 30 ℃～100 ℃; The alkaline hydrolysis time is 10min～60min; The alkali that adopts in the described aqueous slkali comprises one or more the mixture in sodium hydroxide, ammonium hydroxide, sodium carbonate, potassium carbonate, potassium hydroxide, sodium bicarbonate, ammonium bicarbonate, the potassium bicarbonate.
The step 3. concentration of described acid solution is 0.1mol/L～5.0mol/L; Souring temperature is 10 ℃～80 ℃; The acid of adopting in the described acid solution comprises one or more the mixture in acetic acid, hydrochloric acid, carbonic acid, lactic acid, phosphoric acid, adipic acid, sulphuric acid, tartaric acid, the citric acid.
The 4. described resin of step is nonpolar porous polymeric resin, comprises one or more the mixture among macroporous resin HPD100, HPD100A, HPD300, HPD700, D101, X-5, XAD-2, XAD-4, HP20 and the ion exchange resin D301; Described ethanol is that volume ratio is 40%～100% ethanol; Adsorption time is 5 h～24h, and desorption time is 5 h～24h.
The preparation method of described Rhomotoxine is as follows:
After Ramulus Uncariae Cum Uncis raw material stoving, pulverizing, extract 1～3 time in 4 ℃～80 ℃ with ethanol, filter, obtain the Rhomotoxine extracting solution; The Rhomotoxine extracting solution alkalizes to pH9～pH10 through concentrating, be acidified to pH1～pH3, filtration, filtrate, and through chloroform extraction 1～3 time, standing demix is collected chloroform solution to the alkaline solution that obtains, and obtains Rhomotoxine after concentrated again.Ethanol is that volume ratio is 40%～100% ethanol described in the Rhomotoxine preparation.
The present invention is chemically derived by Rhomotoxine is carried out, preparation Rhomotoxine hydrolyzate, and product is soluble in water, can keep drug effect preferably, and toxicity is lower, and technology is simple, is convenient to promote, so that satisfy the wilderness demand in market.
Find that by comparison diagram 2 and Fig. 3 with respect to the infrared absorpting light spectra of Rhomotoxine, the Rhomotoxine hydrolyzate is at 1383.54cm
-1, 1246.21 cm
-1, 1191.40 cm
-1, 1147.79 cm
-1, 918.96 cm
-1The place does not absorb, at 3182.82 cm
-1, 796.37 cm
-1But there is absorption at the place; The INFRARED ABSORPTION of Rhomotoxine hydrolyzate and Rhomotoxine does not exist together and mainly concentrates finger print region, and Rhomotoxine hydrolyzate and Rhomotoxine structural similarity are described.The Rhomotoxine hydrolyzate is at 3182.82 cm
-1Absorption is arranged, illustrate in its structure to have hydroxy-acid group, water-soluble relevant with it; And at 1400 cm
-1-900 cm
-1Be C-O, C-N of bonding absorption region in the scope,, Rhomotoxine be described behind alkaline hydrolysis, amido link, ester linkage breaking have taken place, sloughed aniline group and methanol groups in conjunction with alkaline hydrolysis, acidifying principle.Therefore, Rhomotoxine is after alkaline hydrolysis, acidification, and some variations have taken place structure, but its pharmacophore still exists, so the Rhomotoxine hydrolyzate can keep drug effect preferably.
The present invention compares with traditional method, has the following advantages:
1, providing a kind of is raw material with the Rhomotoxine, by to its alkaline hydrolysis, acidify and desalination, prepares the method for Rhomotoxine hydrolyzate, can improve the water solublity of Rhomotoxine.
2, resin recycles, and the resin desalting effect is good, and it is few to contain impurity in the Rhomotoxine hydrolyzate that obtains, and then simplifies production technology and reduce production costs.
3, the Rhomotoxine hydrolyzate of the present invention's preparation, product has characteristic absorption at the 224nm place, has good water-solubility.
Description of drawings
Fig. 1 is the spectrogram of Rhomotoxine hydrolyzate of the present invention.
Fig. 2 is the infrared spectrogram of Rhomotoxine.
Fig. 3 is the infrared spectrogram of Rhomotoxine hydrolyzate.
The specific embodiment
The preparation of Rhomotoxine of the present invention, step is as follows:
After Ramulus Uncariae Cum Uncis raw material stoving, pulverizing, extract 1～3 time in 4 ℃～80 ℃ with 40%～100% ethanol, solid-liquid ratio is 1:10～1:50, extraction time is 6 h～36h, filters, and obtains the Rhomotoxine extracting solution; The Rhomotoxine extracting solution is concentrated into extractum, add acid solution then and be acidified to pH1～pH3, filtration, filtrate and alkalize to pH9～pH10, the alkaline solution that obtains is again through chloroform extraction 1～3 time, standing demix, collect chloroform solution, after concentrated, drying, obtain the Rhomotoxine powder.The concentration of described acid solution is 0.1 mol/L～5.0mol/L; Souring temperature is 10 ℃～80 ℃; The acid of adopting in the described acid solution comprises one or more the mixture in acetic acid, hydrochloric acid, carbonic acid, lactic acid, phosphoric acid, adipic acid, sulphuric acid, tartaric acid, the citric acid.
Secondly, the preparation of relevant Rhomotoxine hydrolyzate further describes the present invention by following examples, but the present invention is not limited only to this.
After Ramulus Uncariae Cum Uncis raw material stoving, pulverizing, be 70% ethanol extraction 3 times with volume ratio, solid-liquid ratio is 1:30, extraction time is 12h, filters, and obtains the Rhomotoxine extracting solution; The Rhomotoxine extracting solution is concentrated into extractum, adds 0.1 mol/L dissolving with hydrochloric acid, is acidified to pH2～pH3, filtration, filtrate are alkalized to pH9～pH10 then, the alkaline solution that obtains is again through chloroform extraction 3 times, standing demix, collect chloroform solution, after concentrated, spray drying, obtain the Rhomotoxine powder.
Take by weighing 0.1g Rhomotoxine powder and put in the container, add the sodium hydroxide solution of 50ml 0.1mol/L, about 80 ℃ of control reaction temperature, alkaline hydrolysis 10min.After reaction finishes, collecting alkali solution liquid, with the acetum acidify of 0.2mol/L, is 2.6 until the solution pH value.After acidify finishes, filter, collect acidifying solution, acidifying solution is pumped in the container that 50g ion exchange resin D301 is housed, rate of circulating flow is 5BV/h, and adsorption time is 20h, pumps into the 50% ethanol water desorbing of 100ml again in the container, rate of circulating flow is 8BV/h, desorption time is 18h, collects ethanol water, and ethanol water is concentrated and spray drying through rotating, promptly get the Rhomotoxine hydrolyzate, the product yield is 60%.With the product dissolved in distilled water of gained, found that every 100ml water can dissolve the 10g product, promptly the dissolubility of product is 10g.Take by weighing Rhomotoxine and this product of 50mg, with Rhomotoxine with after the 3% HCl dissolving, with distilled water diluting to 10mg/ml, with this product 50ml dissolved in distilled water, be that concentration is 10mg/ml, these two kinds of solution are injected male Wistar kind rat femoral vein by micro-injection pump with 5ml/kg per hour, observe the variation of the mean arterial pressure (MAP) of rat, change the drug effect of coming side light Rhomotoxine and product with the MAP of rat.The result shows that Rhomotoxine makes MAP reduce by 20.8%, and this product makes MAP reduce by 20.5%, and therefore, the product that this method makes can keep drug effect preferably.
Embodiment 2
Take by weighing 0.3g Rhomotoxine powder and put in the container, add the sodium carbonate liquor of 30ml 0.8mol/L again, about 70 ℃ of control reaction temperature, alkaline hydrolysis 30min.After reaction finishes, collecting alkali solution liquid, with the hydrochloric acid solution acidify of 2mol/L, is 2.0 until the solution pH value.After acidify finishes, filter, collect acidifying solution, acidifying solution is pumped in the container that 20g macroporous resin HPD100 is housed, rate of circulating flow is 10BV/h, and adsorption time is 15h, and 60% ethanol water that pumps into 80ml again in the container carries out desorbing, rate of circulating flow is 12BV/h, desorption time is 20h, collects ethanol water, and ethanol water is concentrated and spray drying through rotating, promptly get the Rhomotoxine hydrolyzate, the product yield is 65%.With the product dissolved in distilled water of gained, found that every 100ml water can dissolve the 12g product, promptly the dissolubility of product is 12g.Take by weighing Rhomotoxine and this product of 50mg, with Rhomotoxine with after the 3% HCl dissolving, with distilled water diluting to 10mg/ml, with this product 50ml dissolved in distilled water, be that concentration is 10mg/ml, these two kinds of solution are injected male Wistar kind rat femoral vein by micro-injection pump with 5ml/kg per hour, observe the variation of the mean arterial pressure (MAP) of rat, change the drug effect of coming side light Rhomotoxine and product with the MAP of rat.The result shows that Rhomotoxine makes MAP reduce by 20.8%, and this product makes MAP reduce by 19.4%, and therefore, the product that this method makes can keep drug effect preferably.
Embodiment 3
Take by weighing 0.5g Rhomotoxine powder and put in the container, add the Ammonia of 40ml 1mol/L again, about 50 ℃ of control reaction temperature, alkaline hydrolysis 40min.After reaction finishes, collecting alkali solution liquid, with the carbon acid solution acidify of 1.5mol/L, is 3.2 until the solution pH value.After acidify finishes, filter, collect acidifying solution, acidifying solution is pumped in the container that 30g macroporous resin HPD100A is housed, and rate of circulating flow is 5 BV/h, and adsorption time is 18h, pump into 70% ethanol water of 120ml again in the container, rate of circulating flow is 10BV/h, and desorption time is 20h, filters, collect ethanol water, ethanol water is concentrated and spray drying through rotating, promptly get the Rhomotoxine hydrolyzate, the product yield is 82%.With the product dissolved in distilled water of gained, found that every 100ml water can dissolve the 10.3g product, promptly the dissolubility of product is 10.3g.Take by weighing Rhomotoxine and this product of 50mg, with Rhomotoxine with after the 3% HCl dissolving, with distilled water diluting to 10mg/ml, with this product 50ml dissolved in distilled water, be that concentration is 10mg/ml, these two kinds of solution are injected male Wistar kind rat femoral vein by micro-injection pump with 5ml/kg per hour, observe the variation of the mean arterial pressure (MAP) of rat, change the drug effect of coming side light Rhomotoxine and product with the MAP of rat.The result shows that Rhomotoxine makes MAP reduce by 20.8%, and this product makes MAP reduce by 20.1%, and therefore, the product that this method makes can keep drug effect preferably.
Embodiment 4
Take by weighing 0.8g Rhomotoxine powder and put in the container, add the potassium hydroxide solution of 60ml 1.5mol/L again, about 100 ℃ of control reaction temperature, alkaline hydrolysis 50min.After reaction finishes, collecting alkali solution liquid, with the phosphoric acid solution acidify of 0.5mol/L, is 4.0 until the solution pH value.After acidify finishes, filter, collect acidifying solution, acidifying solution is pumped in the container that 70g macroporous resin HPD700 is housed, and rate of circulating flow is 13 BV/h, and adsorption time is 10h, pump into 80% ethanol water of 150ml again in the container, rate of circulating flow is 12BV/h, and desorption time is 15h, filters, collect ethanol water, ethanol water is concentrated and spray drying through rotating, promptly get the Rhomotoxine hydrolyzate, the product yield is 70%.With the product dissolved in distilled water of gained, found that every 100ml water can dissolve the 8.7g product, promptly the dissolubility of product is 8.7g.Take by weighing Rhomotoxine and this product of 50mg, with Rhomotoxine with after the 3% HCl dissolving, with distilled water diluting to 10mg/ml, with this product 50ml dissolved in distilled water, be that concentration is 10mg/ml, these two kinds of solution are injected male Wistar kind rat femoral vein by micro-injection pump with 5ml/kg per hour, observe the variation of the mean arterial pressure (MAP) of rat, change the drug effect of coming side light Rhomotoxine and product with the MAP of rat.The result shows that Rhomotoxine makes MAP reduce by 20.8%, and this product makes MAP reduce by 19.6%, and therefore, the product that this method makes can keep drug effect preferably.
Embodiment 5
Take by weighing 0.6g Rhomotoxine powder and put in the container, add the mixed liquor of 50ml 0.5mol/L potassium bicarbonate solution and 0.5mol/L sodium carbonate liquor again, about 90 ℃ of control reaction temperature, alkaline hydrolysis 20min.After reaction finishes, collecting alkali solution liquid, with the lactic acid solution acidify of 0.8mol/L, is 4.5 until the solution pH value.After acidify finishes, filter, collect acidifying solution, acidifying solution is pumped in the container that 45g macroporous resin D101 is housed, and rate of circulating flow is 7 BV/h, and adsorption time is 16h, pump into 45% ethanol water of 110ml again in the container, rate of circulating flow is 11BV/h, and desorption time is 8h, filters, collect ethanol water, ethanol water is concentrated and spray drying through rotating, promptly get the Rhomotoxine hydrolyzate, the product yield is 68%.With the product dissolved in distilled water of gained, found that every 100ml water can dissolve the 9.8g product, promptly the dissolubility of product is 9.8g.Take by weighing Rhomotoxine and this product of 50mg, with Rhomotoxine with after the 3% HCl dissolving, with distilled water diluting to 10mg/ml, with this product 50ml dissolved in distilled water, be that concentration is 10mg/ml, these two kinds of solution are injected male Wistar kind rat femoral vein by micro-injection pump with 5ml/kg per hour, observe the variation of the mean arterial pressure (MAP) of rat, change the drug effect of coming side light Rhomotoxine and product with the MAP of rat.The result shows that Rhomotoxine makes MAP reduce by 20.8%, and this product makes MAP reduce by 18.2%, and therefore, the product that this method makes can keep drug effect preferably.
Claims (6)
1. the preparation method of a Rhomotoxine hydrolyzate is characterized in that comprising the steps:
1. reaction substrate: Rhomotoxine;
2. alkaline hydrolysis: in reaction substrate, add aqueous slkali and carry out alkaline hydrolysis;
3. acidify: after alkaline hydrolysis finishes, filter, collect alkali solution liquid, add acid solution and carry out acidify, regulator solution is to pH2.0～pH5.0;
4. desalination: after acidify finishes, filter, collect acidifying solution, acidifying solution is pumped in the container that resin is housed adsorb, the resin after saturated is through alcohol desorption;
5. dry, pulverizing: the ethanolysis imbibition that 4. step is obtained concentrates, dried, and the dried powder that obtains is the Rhomotoxine hydrolyzate.
2. the preparation method of Rhomotoxine hydrolyzate according to claim 1 is characterized in that: the preparation method of described Rhomotoxine is as follows:
After Ramulus Uncariae Cum Uncis raw material stoving, pulverizing, extract 1～3 time in 4 ℃～80 ℃ with ethanol, filter, obtain the Rhomotoxine extracting solution; The Rhomotoxine extracting solution alkalizes to pH9～pH10 through concentrating, be acidified to pH1～pH3, filtration, filtrate, and through chloroform extraction 1～3 time, standing demix is collected chloroform solution to the alkaline solution that obtains, and obtains Rhomotoxine after concentrated again.
3. the preparation method of Rhomotoxine hydrolyzate according to claim 2 is characterized in that: ethanol is that volume ratio is 40%～100% ethanol described in the Rhomotoxine preparation.
4. the preparation method of Rhomotoxine hydrolyzate according to claim 1 is characterized in that: the step 2. concentration of described aqueous slkali is 0.1mol/L～5.0mol/L; The alkaline hydrolysis temperature is 30 ℃～100 ℃; The alkaline hydrolysis time is 10min～60min; The alkali that adopts in the described aqueous slkali comprises one or more the mixture in sodium hydroxide, ammonium hydroxide, sodium carbonate, potassium carbonate, potassium hydroxide, sodium bicarbonate, ammonium bicarbonate, the potassium bicarbonate.
5. the preparation method of Rhomotoxine hydrolyzate according to claim 1 is characterized in that: the step 3. concentration of described acid solution is 0.1mol/L～5.0mol/L; Souring temperature is 10 ℃～80 ℃; The acid of adopting in the described acid solution comprises one or more the mixture in acetic acid, hydrochloric acid, carbonic acid, lactic acid, phosphoric acid, adipic acid, sulphuric acid, tartaric acid, the citric acid.
6. the preparation method of Rhomotoxine hydrolyzate according to claim 1, it is characterized in that: the 4. described resin of step is nonpolar porous polymeric resin, comprises one or more the mixture among macroporous resin HPD100, HPD100A, HPD300, HPD700, D101, X-5, XAD-2, XAD-4, HP20 and the ion exchange resin D301; Described ethanol is that volume ratio is 40%～100% ethanol; Adsorption time is 5 h～24h, and desorption time is 5 h～24h.
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| CN113149857A (en) * | 2021-05-10 | 2021-07-23 | 山东中医药大学 | Amide compound and preparation method and application thereof |
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