CN101735214B - Method for extracting ajmaline from devilpepper waste liquor - Google Patents
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Abstract
The invention discloses a method for extracting ajmaline from devilpepper waste liquor. The ajmaline is obtained by extracting a raffinate of devilpepper with extracted reserpine and adopting methods, i.e. stepped extraction, decoloration sedimentation, washing crystallization, and the like, i.e. the ajmaline is separated when the reserpine is produced by using devilpepper medicinal materials, thereby realizing the effective utilization of plant resources, solving the problem that the reserpine and the ajmaline are produced at the same time by using the devilpepper, enhancing the utility ratio of resources, increasing the types of products and generating new profit growth points. The invention adopts simple and easy extracting method and refining method, can conveniently and fast obtain the ajmaline according with the specifications of a pharmacopeia and is suitable for large-scale production.
Description
Technical field
The invention belongs to natural drug separation and purification field, particularly a kind of method of from devilpepper waste, extracting Ajmaline.
Background technology
Contain the multiple vegeto-alkali that pharmacologically active is arranged in the Radix Rauvolfiae, isolated reaching more than hundred kinds.The more vegeto-alkali of content is serpentine, Ajmaline, Serpophite and Yohimbine etc.; Wherein the main clinical effect of serpentine is hypotensive; The content of serpentine in Radix Rauvolfiae is generally about 1.2%; Account for about 30% of Radix Rauvolfiae total alkali, therefore, people extract serpentine usually from Radix Rauvolfiae.
The main clinical effect of Ajmaline is an arrhythmia, and its content generally accounts for about 15% of Radix Rauvolfiae total alkali, because of the vegeto-alkali of existence in the Radix Rauvolfiae with the Ajmaline similar, from Radix Rauvolfiae, separates comparatively difficulty of Ajmaline.The method of existing separation and purification Ajmaline mainly contains: the back is pulverized with benzene, ETHYLE ACETATE, acidic methanol, acidic ethanol equal solvent soaking and extracting repeatedly with the rauwolfiae,radix skin in (1); Extract with acidic solution behind the concentrated extracting solution; Transfer the pH to 8.5 of remainder water solution to extract with benzene or chloroform equal solvent to 9 backs; Purified crystals obtains Ajmaline; (2) with after the pulverizing of rauwolfiae,radix skin; With benzene, ETHYLE ACETATE equal solvent extract obtain liquid concentrator after; With the dissolving of acetic acid or phosphoric acid, with the potential of hydrogen branch extraction of ammoniacal liquor, yellow soda ash or sodium hydrate regulator solution, obtain pH 9-10 extraction liquid partly after purified crystals obtain Ajmaline; (3) the rauwolfiae,radix skin is pulverized the back with benzene, ETHYLE ACETATE, acidic methanol, acidic ethanol equal solvent soaking and extracting repeatedly; Extract with acidic solution behind the concentrated extracting solution; The pH to 8.5 that transfers remainder water solution extracts preparation liquid phase post after 9, separation of pure dissolves Ajmaline.The main deficiency of these separation purification method is: (1) radix rauvolfia total extracting solution transfers to aqueous solution part behind the acid extract, and to be transferred in the extraction liquid that alkaline extraction obtains impurity more more, and the subsequent purification difficulty is difficult to such an extent that reach the Ajmaline of qualified purity; During (2) with the extraction of the branch after the acid dissolving, the salt concn of extraction liquid is excessive, and the yield of separation and purification is had bigger influence, is unfavorable for producing and amplifies; (3) the preparation liquid phase method can be used for research but can not be used for amplifying production; (4) from Radix Rauvolfiae, directly extract Ajmaline, will waste serpentine, can not effectively utilize the Radix Rauvolfiae resource.
Summary of the invention
In order to solve the weak point of above-mentioned existing stripping technique, realize making full use of of Radix Rauvolfiae medicinal material, the object of the present invention is to provide a kind of method of from devilpepper waste, extracting Ajmaline.
The object of the invention is realized through following technical proposals: a kind of method of from devilpepper waste, extracting Ajmaline may further comprise the steps:
(1) extraction concentrates: the pH value of devilpepper waste is adjusted to 6～7, uses organic solvent extraction, repeat 2～3 times; PH value with extraction liquid is adjusted to 9～10 again, uses organic solvent extraction, until aqueous phase lifeless matter alkali reaction; The merging organic phase is concentrated into when just having one deck solids to separate out on bottle wall and stops; Be placed into room temperature solids is separated out fully, filter out the solids drying, filtrating is recycled;
(2) purifying: the solids dissolving fully just with the Hydrogen chloride of mass percent 3～6% obtains step (1), then add gac, in 60～70 ℃ of decolouring 15～20min, filter; Then pH value of filtrate is adjusted to 9～10, uses organic solvent extraction again, use the water washing extraction liquid; Dry with siccative, the solids that obtains obtains the white solid thing with the acetone crystallization, and the white solid thing is used methanol crystallization again; Filter, the crystallization that obtains in 60～70 ℃ of dryings, is obtained Ajmaline;
Described devilpepper waste is the raffinate behind the extraction serpentine from Radix Rauvolfiae;
Described raffinate preferably obtains through following steps: after the rauwolfiae,radix skin is pulverized; Methyl alcohol/glacial acetic acid solution with 4～6 times of weight at room temperature soaks; Percolating extract to serpentine extracts fully repeatedly; Extracting solution obtains Radix Rauvolfiae medicinal extract behind concentrating under reduced pressure, the concentrating under reduced pressure temperature is controlled at below 60 ℃; Then use concentration as the hydrochloric acid of mass percent 5～20% the dissolving of Radix Rauvolfiae medicinal extract, the pH value of regulator solution is 4～5, it is complete to be taken to the extraction serpentine with organic solvent extracting then, remaining water partly is the raffinate behind the extraction serpentine;
The degree that said rauwolfiae,radix skin is pulverized is preferably and is crushed to 30～60 orders;
The concentration of Glacial acetic acid min. 99.5 is 0.5～1% by mass percentage in said methyl alcohol/glacial acetic acid solution;
The adjusting of said pH value is regulated with acid or alkali; Acid is hydrochloric acid, sulfuric acid or phosphoric acid; Alkali is ammoniacal liquor, yellow soda ash, sodium hydroxide or Pottasium Hydroxide;
The concentration of described acid is preferably mass percent 3～6%;
The concentration of described alkali is preferably mass percent 10～20%;
Described organic solvent comprises ethylene dichloride, chloroform, methylene dichloride, benzene, toluene and ETHYLE ACETATE etc.;
Said drying comprises drying meanss such as drying, vacuum-drying or fluidized drying in the loft drier;
The consumption of gac is equivalent to 1～6% of said solids quality described in the step (2);
Be preferably with the water washing that is equivalent to extraction liquid volume 1/4～1/3 1～2 time with the water washing extraction liquid described in the step (2);
The preferred Anhydrous potassium carbonate of siccative, SODIUM SULPHATE ANHYDROUS 99PCT or anhydrous magnesium sulfate described in the step (2).
The present invention has following advantage and effect with respect to prior art:
1. the present invention extracts through the raffinate that from Radix Rauvolfiae, extracts behind the serpentine, through concentrating directly purified method of extraction back, obtains Ajmaline; Promptly be to isolate Ajmaline when utilizing the Radix Rauvolfiae medicinal material to produce serpentine; Realize effective utilization of plant resources, meaned to have solved the problem of utilizing Radix Rauvolfiae to produce serpentine and Ajmaline simultaneously, improved efficiency of resource; Increase product type, produced new profit growth point.
2. the present invention adopts easy extracting process and process for purification, can obtain conforming with the Ajmaline of pharmacopeia regulation easily and quickly, is fit to amplify produce.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail, but embodiment of the present invention is not limited thereto.
Embodiment 1
(1) extraction concentrates: get 100 liters of remaining aqueous solutions after having extracted serpentine, with the pH value to 6.5 of ammoniacal liquor (concentration is mass percent 25～28%) accent remaining aqueous solution, follow with (30 liters/inferior of 90 liters extracted in toluene; 3 times), again after the pH value to 9.5 with ammoniacal liquor accent remaining aqueous solution, with extracted in toluene to lifeless matter alkali reaction (confirming) with vegeto-alkali characteristic developer-bismuth potassium iodide solution colour developing is qualitative; The combining methylbenzene phase is concentrated into when just separating out one deck solids in the bottle and stops, and is placed into room temperature solids is separated out fully; Filter out solids; In 60～65 ℃ of dryings 3 hours, obtain bullion 291 grams, filtrate is recycled.
(2) purifying: use concentration to be 1550 milliliters of dissolvings of the Hydrogen chloride of mass percent 5% bullion, add 10 gram active carbon powders in 65 ℃ of decolourings 20 minutes, filtrate filtered uses ammoniacal liquor to regulate after the pH value is 9.5, with (300 milliliters/inferior of 1200 milliliters of extracted in toluene; 4 times), the combining methylbenzene phase is with (200 milliliters/inferior of 400 ml waters washings; 2 times) the toluene phase, concentrate the toluene phase, obtain solids; With 850 milliliters of acetone heating for dissolving solidss, crystallization obtains the white solid thing, uses methanol crystallization again; Filter, the crystallization that obtains was put into 60 ℃ of dryings of loft drier 3 hours, (calculate by the Radix Rauvolfiae bark conversion back promptly to get Ajmaline 140 grams; The yield of Ajmaline is that per mille puts four or five), fusing point is 158～160 ℃ (with after this laboratory sample mixes, the fusing point of biased sample is identical with standard substance with the Ajmaline standard substance).This sample is the white powder crystal, and nothing is smelt, and little hardship is soluble in diacetyl oxide and chloroform, is slightly soluble in methyl alcohol, ethanol (95), acetone and ether, is insoluble in water, and the character description that is dissolved in diluted hydrochloric acid aqueous solution and Japanese Pharmacopoeia coincide.Perchloric acid titration quantivative approach by Japanese pharmacopeia version in 2007 detects, and purity is 98.6%, meets the pharmacopeia specified standards.
Embodiment 2
(1) extraction concentrates: get 200 liters of remaining aqueous solutions after having extracted serpentine, with the pH value to 7 of ammoniacal liquor (concentration is mass percent 25～28%) accent remaining aqueous solution, follow with (40 liters/inferior of 160 liters chloroform extractions; 4 times), again after the pH value to 10 with ammoniacal liquor accent remaining aqueous solution, with chloroform extraction to lifeless matter alkali reaction (confirming) with vegeto-alkali characteristic developer-bismuth potassium iodide solution colour developing is qualitative; The combined chloroform phase is concentrated into when just separating out one deck solids in the bottle and stops, and is placed into room temperature solids is separated out fully; Filter out solids, in 65～70 ℃ of dryings 3 hours; Obtain bullion 623 grams, filtrate is recycled.
(2) purifying: use concentration to be 2700 milliliters of dissolvings of the Hydrogen chloride of mass percent 5% bullion, add 15 gram active carbon powders in 70 ℃ of decolourings 20 minutes, filtrate filtered uses ammoniacal liquor to regulate after the pH value is 9.0, with (500 milliliters/inferior of 2000 milliliters of chloroform extractions; 4 times), the combined chloroform phase is with (300 milliliters/inferior of 600 ml waters washings; 2 times) the chloroform phase, concentrate the chloroform phase, obtain solids; With 1350 milliliters of acetone heating for dissolving solidss, crystallization obtains the white solid thing, uses methanol crystallization again; Filter, the crystallization that obtains was put into 65 ℃ of dryings of loft drier 3 hours, (calculate by the Radix Rauvolfiae bark conversion back promptly to get Ajmaline 310 grams; The yield of Ajmaline is a per mille point five), fusing point is 159～161 ℃ (with after this laboratory sample mixes, the fusing point of biased sample is identical with standard substance with the Ajmaline standard substance).This sample is the white powder crystal, and nothing is smelt, and little hardship is soluble in diacetyl oxide and chloroform, is slightly soluble in methyl alcohol, ethanol (95), acetone and ether, is insoluble in water, and the character description that is dissolved in diluted hydrochloric acid aqueous solution and Japanese Pharmacopoeia coincide.Perchloric acid titration quantivative approach by Japanese pharmacopeia version in 2007 detects, and purity is 98.2%, meets the pharmacopeia specified standards.
Embodiment 3
(1) extraction concentrates: get 300 liters of remaining aqueous solutions after having extracted serpentine, with the pH value to 6.0 of ammoniacal liquor (concentration is mass percent 25～28%) accent remaining aqueous solution, follow with (60 liters/inferior of 240 liters ethyl acetate extractions; 4 times), again after the pH value to 9.5 with ammoniacal liquor accent remaining aqueous solution, with ethyl acetate extraction to lifeless matter alkali reaction (confirming) with vegeto-alkali characteristic developer-bismuth potassium iodide solution colour developing is qualitative; The combined ethyl acetate phase is concentrated into when just separating out one deck solids in the bottle and stops, and is placed into room temperature solids is separated out fully; Filter out solids; In 60 ℃ of dryings 3 hours, obtain bullion 815 grams, filtrate is recycled.
(2) purifying: use concentration to be 3260 milliliters of dissolvings of the Hydrogen chloride of mass percent 5% bullion, add 21 gram active carbon powders in 70 ℃ of decolourings 25 minutes, filtrate filtered uses ammoniacal liquor to regulate after the pH value is 9.0; With 2400 milliliters of ethyl acetate extractions (600 milliliters/inferior, 4 times), combined ethyl acetate phase; With 800 ml waters washing (400 milliliters/inferior, 2 times) ETHYLE ACETATE phase, concentrate the ETHYLE ACETATE phase; Obtain solids, with 1880 milliliters of acetone heating for dissolving solidss, crystallization obtains the white solid thing; Use methanol crystallization again, filter, the crystallization that obtains was put into 60 ℃ of dryings of loft drier 3 hours; (calculate by the Radix Rauvolfiae bark conversion back promptly to get Ajmaline 380 grams; The yield of Ajmaline is a per mille point three), fusing point is 158～160 ℃ (with after this laboratory sample mixes, the fusing point of biased sample is identical with standard substance with the Ajmaline standard substance).This sample is the white powder crystal, and nothing is smelt, and little hardship is soluble in diacetyl oxide and chloroform, is slightly soluble in methyl alcohol, ethanol (95), acetone and ether, is insoluble in water, and the character description that is dissolved in diluted hydrochloric acid aqueous solution and Japanese Pharmacopoeia coincide.Perchloric acid titration quantivative approach by Japanese pharmacopeia version in 2007 detects, and purity is 98.3%, meets the pharmacopeia specified standards.
Embodiment 4
(1) extraction concentrates: get 250 liters of remaining aqueous solutions after having extracted serpentine, with the pH value to 6.5 of ammoniacal liquor (concentration is mass percent 25～28%) accent remaining aqueous solution, the ethylene dichloride of following with 200 liters extracts (50 liters/inferior; 4 times), after the pH value to 9.0 with ammoniacal liquor accent remaining aqueous solution, be extracted to lifeless matter alkali reaction (confirming) again with vegeto-alkali characteristic developer-bismuth potassium iodide solution colour developing is qualitative with ethylene dichloride; Merge the ethylene dichloride phase, be concentrated into when just separating out one deck solids in the bottle and stop, being placed into room temperature solids is separated out fully; Filter out solids; In 65 ℃ of dryings 3 hours, obtain bullion 742 grams, filtrate is recycled.
(2) purifying: use concentration to be 3020 milliliters of dissolvings of the Hydrogen chloride of mass percent 5% bullion, add 18 gram active carbon powders in 60～65 ℃ of decolourings 20 minutes, filtrate filtered uses ammoniacal liquor to regulate after the pH value is 9.5; With 2400 milliliters of ethylene dichloride extractions (600 milliliters/inferior, 4 times), merge the ethylene dichloride phase; With 800 ml waters washing (400 milliliters/inferior, 2 times) ethylene dichloride phase, concentrate the ethylene dichloride phase; Obtain solids, with 1600 milliliters of acetone heating for dissolving solidss, crystallization obtains the white solid thing; Use methanol crystallization again, filter, the crystallization that obtains was put into 65～68 ℃ of dryings of loft drier 3 hours; (calculate by the Radix Rauvolfiae bark conversion back promptly to get Ajmaline 353 grams; The yield of Ajmaline is a per mille point four), fusing point is 159～160 ℃ (with after this laboratory sample mixes, the fusing point of biased sample is identical with standard substance with the Ajmaline standard substance).This sample is the white powder crystal, and nothing is smelt, and little hardship is soluble in diacetyl oxide and chloroform, is slightly soluble in methyl alcohol, ethanol (95), acetone and ether, is insoluble in water, and the character description that is dissolved in diluted hydrochloric acid aqueous solution and Japanese Pharmacopoeia coincide.Perchloric acid titration quantivative approach by Japanese pharmacopeia version in 2007 detects, and purity is 98.5%, meets the pharmacopeia specified standards.
Embodiment 5
(1) extracts serpentine: 200kg rauwolfiae,radix skin comminuted powder is broken to 30～60 orders; Use 800kg methyl alcohol/glacial acetic acid solution (concentration of Glacial acetic acid min. 99.5 is mass percent 1%) under room temperature, to soak then; Percolating extract repeatedly; Through thin-layer chromatography detect extract fully to serpentine till, extracting solution obtains Radix Rauvolfiae medicinal extract behind concentrating under reduced pressure, the concentrating under reduced pressure temperature is controlled at below 60 ℃; Then use concentration as the hydrochloric acid of mass percent 10% the dissolving of Radix Rauvolfiae medicinal extract, the pH value of regulator solution is 4, uses ethyl acetate extraction then 4 times; Thin-layer chromatography detects the serpentine extraction fully, and combining extraction liquid is concentrated into glue with extraction liquid; Add an amount of mass percent 95% ethanol; Heating is dissolved jelly fully, places and separates out solids, obtains the serpentine coarse-grain.The serpentine coarse-grain of separating out is filtered, and with the trichloromethane dissolving, the filtering insolubles concentrates the back with mass percent 95% dissolve with ethanol, places and separates out crystallization, and is dry in 60 ℃ of thermostatic drying chambers with 95% washing, obtains serpentine finished product 1.2kg.Through thin-layer chromatographic analysis and fusing point test and the comparison of serpentine standard model, confirm that the serpentine finished product purity that obtains is high, reach more than 99%.
(2) extract Ajmaline: get 250 liters of the raffinates that step (1) obtains; Extraction step is with embodiment 4 steps (2); Difference only is to use concentration to transfer alkali as the sodium hydroxide solution of mass percent 10%, obtains Ajmaline 302 grams (calculate by the Radix Rauvolfiae bark conversion back, and the yield of Ajmaline is a per mille point five); Fusing point is 158～160 ℃ (with after this laboratory sample mixes, the fusing point of biased sample is identical with standard substance with the Ajmaline standard substance).This sample is the white powder crystal, and nothing is smelt, and little hardship is soluble in diacetyl oxide and chloroform, is slightly soluble in methyl alcohol, ethanol (95), acetone and ether, is insoluble in water, and the character description that is dissolved in diluted hydrochloric acid aqueous solution and Japanese Pharmacopoeia coincide.Perchloric acid titration quantivative approach by Japanese pharmacopeia version in 2007 detects, and purity is 98.5%, meets the pharmacopeia specified standards.
The foregoing description is a preferred implementation of the present invention; But embodiment of the present invention is not restricted to the described embodiments; Other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; All should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (9)
1. method of from devilpepper waste, extracting Ajmaline is characterized in that may further comprise the steps:
(1) extraction concentrates: the pH value of devilpepper waste is adjusted to 6～7, uses organic solvent extraction, repeat 2～3 times; PH value with extraction liquid is adjusted to 9～10 again, uses organic solvent extraction, until aqueous phase lifeless matter alkali reaction; The merging organic phase is concentrated into when just having one deck solids to separate out on bottle wall and stops; Be placed into room temperature solids is separated out fully, filter out the solids drying, filtrating is recycled;
(2) purifying: the solids dissolving fully just with the Hydrogen chloride of mass percent 3～6% obtains step (1), then add gac, in 60～70 ℃ of decolouring 15～20min, filter; Then pH value of filtrate is adjusted to 9～10, uses organic solvent extraction again, use the water washing extraction liquid; Dry with siccative, the solids that obtains obtains the white solid thing with the acetone crystallization, and the white solid thing is used methanol crystallization again; Filter, the crystallization that obtains in 60～70 ℃ of dryings, is obtained Ajmaline;
Described devilpepper waste is for extracting the remaining aqueous solution behind the serpentine from Radix Rauvolfiae;
Described organic solvent is a kind of in ethylene dichloride, chloroform, methylene dichloride, benzene, toluene or the ETHYLE ACETATE.
2. according to the said method of from devilpepper waste, extracting Ajmaline of claim 1; It is characterized in that: the raffinate of described devilpepper waste: after the rauwolfiae,radix skin is pulverized for obtaining through following steps; Methyl alcohol/glacial acetic acid solution with 4～6 times of weight at room temperature soaks; Percolating extract to serpentine extracts fully repeatedly, and extracting solution obtains Radix Rauvolfiae medicinal extract behind concentrating under reduced pressure, and the concentrating under reduced pressure temperature is controlled at below 60 ℃; Then use concentration as the hydrochloric acid of mass percent 5～20% the dissolving of Radix Rauvolfiae medicinal extract, the pH value of regulator solution is 4～5, it is complete to be taken to the extraction serpentine with organic solvent extracting then, the merging raffinate obtains extracting the raffinate behind the serpentine;
Described organic solvent is ethylene dichloride, chloroform, methylene dichloride, benzene, toluene or ETHYLE ACETATE.
3. according to the said method of from devilpepper waste, extracting Ajmaline of claim 2, it is characterized in that:
The degree that said rauwolfiae,radix skin is pulverized is for being crushed to 30～60 orders;
The concentration of Glacial acetic acid min. 99.5 is 0.5～1% by mass percentage in said methyl alcohol/glacial acetic acid solution.
4. according to claim 1 or the 2 said methods of from devilpepper waste, extracting Ajmaline, it is characterized in that: the adjusting of said pH value is regulated with acid or alkali; Acid is hydrochloric acid, sulfuric acid or phosphoric acid; Alkali is ammoniacal liquor, yellow soda ash, sodium hydroxide or Pottasium Hydroxide.
5. according to the said method of from devilpepper waste, extracting Ajmaline of claim 4, it is characterized in that: the concentration of described acid is mass percent 3～6%; The concentration of described alkali is mass percent 10～20%.
6. according to the said method of from devilpepper waste, extracting Ajmaline of claim 1, it is characterized in that: said drying comprises drying, vacuum-drying or fluidized drying in the loft drier.
7. according to the said method of from devilpepper waste, extracting Ajmaline of claim 1, it is characterized in that: the consumption of gac is equivalent to 1～6% of said solids quality described in the step (2).
8. according to the said method of from devilpepper waste, extracting Ajmaline of claim 1, it is characterized in that: use the water washing extraction liquid for the water washing that is equivalent to extraction liquid volume 1/4～1/3 1～2 time described in the step (2).
9. according to the said method of from devilpepper waste, extracting Ajmaline of claim 1, it is characterized in that: siccative is Anhydrous potassium carbonate, SODIUM SULPHATE ANHYDROUS 99PCT or anhydrous magnesium sulfate described in the step (2).
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