CN102274319B - Preparation method of rhomotoxine hydrolysis product - Google Patents
Preparation method of rhomotoxine hydrolysis product Download PDFInfo
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- CN102274319B CN102274319B CN 201110206899 CN201110206899A CN102274319B CN 102274319 B CN102274319 B CN 102274319B CN 201110206899 CN201110206899 CN 201110206899 CN 201110206899 A CN201110206899 A CN 201110206899A CN 102274319 B CN102274319 B CN 102274319B
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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 hydrolysis product.
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 Southwestern China section, be a kind of can tame medicinal plants, aboundresources.Rhomotoxine is the deep processed product of Ramulus Uncariae Cum Uncis, can be used for the 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 uncaria 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, then uses 0.5%～15% acid solution eluting, and eluent prepares uncaria total alkaloids through neutralization, desalination, drying process again; Latter is to soak cation exchange resin column with 0.5%～20% saline solution, then containing 0.5%～20% saline solution eluting of acid or ethanol, and eluent makes uncaria total alkaloids through desalination, concentrated, drying process again.Although 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 hydrolysis product, the method is passed through the preparation rhomotoxine hydrolysis product, thereby improves water solublity, widens the application of Rhomotoxine.
The present invention carries out ester hydrolysis, amide hydrolysis and acidify take Rhomotoxine as reaction substrate, then by desalination and subsequent technique, and the preparation rhomotoxine hydrolysis product.
The present invention is achieved through the following technical solutions:
Because the main effective ingredient of Rhomotoxine is Ramulus Uncariae cum Uncis alkali, therefore the following realization of explanation technical scheme as an example of Ramulus Uncariae cum Uncis alkali example.
At first, aqueous slkali is 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, acidifying solution is pumped in the container that resin is housed, and comes the purified water hydrolysis products by absorption and ethanol desorbing.The subsequent techniques such as the ethanolysis imbibition warp of collecting is concentrated, dry 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 hydrolysis product of the present invention comprises the steps:
1. reaction substrate: Rhomotoxine;
2. alkaline hydrolysis: add aqueous slkali to carry out alkaline hydrolysis in reaction substrate;
3. acidify: after alkaline hydrolysis finishes, filter, collect alkali solution liquid, add acid solution to 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 the ethanol desorbing;
5. dry, pulverizing: the ethanolysis imbibition that 4. step is obtained concentrates, dried, and the dried powder that obtains is rhomotoxine hydrolysis product.
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 described aqueous slkali comprises one or more the mixture in sodium hydroxide, ammonium hydroxide, sodium carbonate, potassium carbonate, potassium hydroxide, sodium bicarbonate, ammonium bicarbonate, 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 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, citric acid.
Step 4. described resin is nonpolar porous polymeric resin, comprises one or more the mixture in macroporous resin HPD100, HPD100A, HPD300, HPD700, D101, X-5, XAD-2, XAD-4, HP20 and 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 concentrating again.Described in the Rhomotoxine preparation, ethanol is that volume ratio is 40%～100% ethanol.
The present invention is chemically derived by Rhomotoxine is carried out, the preparation rhomotoxine hydrolysis product, and product is soluble in water, can keep preferably drug effect, and toxicity is lower, and technique is simple, is convenient to promote, so that the wilderness demand of satisfying the market.
Find by comparison diagram 2 and Fig. 3, with respect to the infrared absorpting light spectra of Rhomotoxine, rhomotoxine hydrolysis product 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 hydrolysis product and Rhomotoxine does not exist together and mainly concentrates finger print region, and rhomotoxine hydrolysis product and Rhomotoxine structural similarity are described.Rhomotoxine hydrolysis product 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 scope, in conjunction with the principle of alkaline hydrolysis, acidify, Rhomotoxine be described after alkaline hydrolysis, amido link, ester linkage breaking have occured, sloughed aniline group and methanol groups.Therefore, Rhomotoxine is after alkaline hydrolysis, acidification, and some variations have occured structure, but its pharmacophore still exists, therefore rhomotoxine hydrolysis product can keep drug effect preferably.
The present invention compares with traditional method, has the following advantages:
1, provide a kind of take Rhomotoxine as raw material, by to its alkaline hydrolysis, acidify and desalination, prepared the method for rhomotoxine hydrolysis product, can improve the water solublity of Rhomotoxine.
2, resin recycles, and the resin desalting effect is good, contains impurity in the rhomotoxine hydrolysis product that obtains few, and then simplifies production technology and reduce production costs.
3, the rhomotoxine hydrolysis product of the present invention preparation, product has characteristic absorption at the 224nm place, has good water solublity.
Description of drawings
Fig. 1 is the spectrogram of rhomotoxine hydrolysis product of the present invention.
Fig. 2 is the infrared spectrogram of Rhomotoxine.
Fig. 3 is the infrared spectrogram of rhomotoxine hydrolysis product.
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, then add acid solution to 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, through concentrating, obtaining the Rhomotoxine powder after drying.The concentration of described acid solution is 0.1 mol/L～5.0mol/L; Souring temperature is 10 ℃～80 ℃; The acid of adopting in 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, citric acid.
Secondly, the preparation of relevant rhomotoxine hydrolysis product 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, then filtration, filtrate are alkalized to pH9～pH10, the alkaline solution that obtains is again through chloroform extraction 3 times, standing demix, collect chloroform solution, through concentrating, obtaining the Rhomotoxine powder after spray drying.
Take 0.1g Rhomotoxine powder and put in container, add the sodium hydroxide solution of 50ml 0.1mol/L, control reaction temperature 80 ℃ of left and right, alkaline hydrolysis 10min.After reaction finishes, collect alkali solution liquid, with the acetum acidify of 0.2mol/L, until pH is 2.6.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, then pumps into the 50% ethanol water desorbing of 100ml 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, namely get rhomotoxine hydrolysis product, the product yield is 60%.The product of gained is dissolved with distilled water, found that every 100ml water can dissolve the 10g product, namely the dissolubility of product is 10g.Take Rhomotoxine and this product of 50mg, after Rhomotoxine is dissolved with 3% HCl, with distilled water diluting to 10mg/ml, this product is dissolved with the 50ml 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 with the MAP of rat the drug effect of coming side light Rhomotoxine and product.Result demonstration, Rhomotoxine make MAP reduce by 20.8%, and this product makes MAP reduce by 20.5%, and therefore, the product that the method makes can keep drug effect preferably.
Embodiment 2
Take 0.3g Rhomotoxine powder and put in container, then add the sodium carbonate liquor of 30ml 0.8mol/L, control reaction temperature 70 ℃ of left and right, alkaline hydrolysis 30min.After reaction finishes, collect alkali solution liquid, with the hydrochloric acid solution acidify of 2mol/L, until pH is 2.0.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, then 60% ethanol water that pumps into 80ml 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, namely get rhomotoxine hydrolysis product, the product yield is 65%.The product of gained is dissolved with distilled water, found that every 100ml water can dissolve the 12g product, namely the dissolubility of product is 12g.Take Rhomotoxine and this product of 50mg, after Rhomotoxine is dissolved with 3% HCl, with distilled water diluting to 10mg/ml, this product is dissolved with the 50ml 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 with the MAP of rat the drug effect of coming side light Rhomotoxine and product.Result demonstration, Rhomotoxine make MAP reduce by 20.8%, and this product makes MAP reduce by 19.4%, and therefore, the product that the method makes can keep drug effect preferably.
Embodiment 3
Take 0.5g Rhomotoxine powder and put in container, then add the Ammonia of 40ml 1mol/L, control reaction temperature 50 ℃ of left and right, alkaline hydrolysis 40min.After reaction finishes, collect alkali solution liquid, with the carbon acid solution acidify of 1.5mol/L, until pH is 3.2.After acidify finishes, filter, collect acidifying solution, acidifying solution is pumped in the container that 30g macroporous resin HPD100A is housed, rate of circulating flow is 5 BV/h, and adsorption time is 18h, pump into again 70% ethanol water of 120ml in the container, rate of circulating flow is 10BV/h, and desorption time is 20h, filters, collect ethanol water, ethanol water through rotating concentrated and spray drying, is namely got rhomotoxine hydrolysis product, and the product yield is 82%.The product of gained is dissolved with distilled water, found that every 100ml water can dissolve the 10.3g product, namely the dissolubility of product is 10.3g.Take Rhomotoxine and this product of 50mg, after Rhomotoxine is dissolved with 3% HCl, with distilled water diluting to 10mg/ml, this product is dissolved with the 50ml 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 with the MAP of rat the drug effect of coming side light Rhomotoxine and product.Result demonstration, Rhomotoxine make MAP reduce by 20.8%, and this product makes MAP reduce by 20.1%, and therefore, the product that the method makes can keep drug effect preferably.
Embodiment 4
Take 0.8g Rhomotoxine powder and put in container, then add the potassium hydroxide solution of 60ml 1.5mol/L, control reaction temperature 100 ℃ of left and right, alkaline hydrolysis 50min.After reaction finishes, collect alkali solution liquid, with the phosphoric acid solution acidify of 0.5mol/L, until pH is 4.0.After acidify finishes, filter, collect acidifying solution, acidifying solution is pumped in the container that 70g macroporous resin HPD700 is housed, rate of circulating flow is 13 BV/h, and adsorption time is 10h, pump into again 80% ethanol water of 150ml in the container, rate of circulating flow is 12BV/h, and desorption time is 15h, filters, collect ethanol water, ethanol water through rotating concentrated and spray drying, is namely got rhomotoxine hydrolysis product, and the product yield is 70%.The product of gained is dissolved with distilled water, found that every 100ml water can dissolve the 8.7g product, namely the dissolubility of product is 8.7g.Take Rhomotoxine and this product of 50mg, after Rhomotoxine is dissolved with 3% HCl, with distilled water diluting to 10mg/ml, this product is dissolved with the 50ml 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 with the MAP of rat the drug effect of coming side light Rhomotoxine and product.Result demonstration, Rhomotoxine make MAP reduce by 20.8%, and this product makes MAP reduce by 19.6%, and therefore, the product that the method makes can keep drug effect preferably.
Embodiment 5
Take 0.6g Rhomotoxine powder and put in container, then add the mixed liquor of 50ml 0.5mol/L potassium bicarbonate solution and 0.5mol/L sodium carbonate liquor, control reaction temperature 90 ℃ of left and right, alkaline hydrolysis 20min.After reaction finishes, collect alkali solution liquid, with the lactic acid solution acidify of 0.8mol/L, until pH is 4.5.After acidify finishes, filter, collect acidifying solution, acidifying solution is pumped in the container that 45g macroporous resin D101 is housed, rate of circulating flow is 7 BV/h, and adsorption time is 16h, pump into again 45% ethanol water of 110ml in the container, rate of circulating flow is 11BV/h, and desorption time is 8h, filters, collect ethanol water, ethanol water through rotating concentrated and spray drying, is namely got rhomotoxine hydrolysis product, and the product yield is 68%.The product of gained is dissolved with distilled water, found that every 100ml water can dissolve the 9.8g product, namely the dissolubility of product is 9.8g.Take Rhomotoxine and this product of 50mg, after Rhomotoxine is dissolved with 3% HCl, with distilled water diluting to 10mg/ml, this product is dissolved with the 50ml 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 with the MAP of rat the drug effect of coming side light Rhomotoxine and product.Result demonstration, Rhomotoxine make MAP reduce by 20.8%, and this product makes MAP reduce by 18.2%, and therefore, the product that the method makes can keep drug effect preferably.
Claims (6)
1. the preparation method of a rhomotoxine hydrolysis product, is characterized in that comprising the steps:
1. reaction substrate: Rhomotoxine;
2. alkaline hydrolysis: add aqueous slkali to carry out alkaline hydrolysis in reaction substrate;
3. acidify: after alkaline hydrolysis finishes, filter, collect alkali solution liquid, add acid solution to 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 the ethanol desorbing;
5. dry, pulverizing: the ethanolysis imbibition that 4. step is obtained concentrates, dried, and the dried powder that obtains is rhomotoxine hydrolysis product.
2. the preparation method of rhomotoxine hydrolysis product according to claim 1, it 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 concentrating again.
3. the preparation method of rhomotoxine hydrolysis product according to claim 2 is characterized in that: described in the Rhomotoxine preparation, ethanol is that volume ratio is 40%～100% ethanol.
4. the preparation method of rhomotoxine hydrolysis product according to claim 1, it 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 described aqueous slkali is one or more the mixture in sodium hydroxide, ammonium hydroxide, sodium carbonate, potassium carbonate, potassium hydroxide, sodium bicarbonate, ammonium bicarbonate, potassium bicarbonate.
5. the preparation method of rhomotoxine hydrolysis product according to claim 1, it 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 described acid solution is one or more the mixture in acetic acid, hydrochloric acid, carbonic acid, lactic acid, phosphoric acid, adipic acid, sulphuric acid, tartaric acid, citric acid.
6. the preparation method of rhomotoxine hydrolysis product according to claim 1 is characterized in that: step 4. described resin is one or more mixture in macroporous resin HPD100, HPD100A, HPD300, HPD700, D101, X-5, XAD-2, XAD-4, HP20 and 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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