CN101732451A - Preparation method capable of enhancing content of amino acid of Qingkailing - Google Patents
Preparation method capable of enhancing content of amino acid of Qingkailing Download PDFInfo
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- CN101732451A CN101732451A CN200810079708A CN200810079708A CN101732451A CN 101732451 A CN101732451 A CN 101732451A CN 200810079708 A CN200810079708 A CN 200810079708A CN 200810079708 A CN200810079708 A CN 200810079708A CN 101732451 A CN101732451 A CN 101732451A
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Abstract
The invention discloses a preparation method capable of enhancing the content of the amino acid of Qingkailing, which comprises the following steps: (a) hydrolyzing buffalo horn powder; (b) hydrolyzing mother-of-pearl powder; (c) adding a right amount of concentrated H2SO4 into buffalo horn hydrolysate and mother-of-pearl hydrolysate, regulating the pH value to 3.0-5.0 and mixing; (d) concentrating the mixed supernatant liquid, chilling, adding high-concentration ethanol, refrigerating and filtering; (e) processing filtrate in the procedure of the step (d) by styrene series cation exchange resin, desorbing by using 1.0-4.0% of ammonia and collecting ammonia lotion; and (f) carrying out water bath on the ammonia lotion, drying by distillation, adding 4.0-8.0% of active carbon after adding distilled water and dissolving, and carrying out decarburization treatment. The content of various Qingkailing medicine preparations prepared by mixing a buffalo horn and mother-of-pearl mixed extract prepared by adopting the method and other medicinal materials and medicinal material extracts in a Qingkailing medicine formula and the amino acid thereof can be enhanced by 10-15%.
Description
Technical field
The present invention relates to the production technology of Chinese medicine preparation, specifically a kind of preparation method that improves content of amino acid of Qingkailing.
Background technology
The QINGKAILING medicine is made up of Flos Lonicerae, Radix Isatidis, Fructus Gardeniae, Cornu Bubali, Concha Margaritifera, baicalin, cholic acid and Hyodeoxycholic Acid eight flavor medical materials and extract, the function that it has heat-clearing and toxic substances removing, eleminating phlegm and freeing channels, consciousness and resuscitation restoring is widely used in diseases such as treatment calentura coma, apoplectic hemiplegia, obnubilation, upper respiratory tract infection, acute, chronic hepatitis, hepatitis B, pneumonia, hyperpyrexia and cerebral thrombosis, cerebral hemorrhage.Patent application about the QINGKAILING medicine at present has a lot, discloses a kind of preparation method of Qingkailing freeze-drying powder preparation as CN1724023; CN1513505 discloses a kind of new method for preparing the Qingkailing granule agent; The CN1586587 disclosure of the Invention a kind of Qingkailing oral disintegration tablet and preparation method thereof.As can be seen, the research at the QINGKAILING medicine at present mainly concentrates on the improvement that pharmaceutical dosage form is carried out, and rarely has at improving the innovation and creation that effective ingredient carries out from these disclosed patent applications.Modern pharmacology studies show that polypeptide, amino acids are important active constituents of medicine.And all contain a large amount of taurines and several amino acids such as valine, methionine, methionine, glutamic acid and isoleucine in Cornu Bubali in the QINGKAILING ingredient and the Concha Margaritifera, and it plays an important role at aspects such as the demented infantile convulsion of treatment, the vertigo, tinnitus cardiopalmus, hematemesis and epistaxis, metrorrhagias.Amino acid content in the effort raising QINGKAILING medicine can further strengthen the curative effect of medicine undoubtedly.Existing QINGKAILING pharmaceutical preparation, for Cornu Bubali in the drug component and the common extracting method that adopts of Concha Margaritifera be: Cornu Bubali powder barium hydroxide solution, Concha Margaritifera powder with sulphuric acid difference hydrolysis 7～9 hours, are filtered merging filtrate, regulate pH value to 3.5～4.0, filter, filtrate adds ethanol makes pure content reach 60%, cold preservation, filter, filtrate recycling ethanol adds water, and cold preservation is standby.This method whole process of production is fairly simple, but the component separating specificity is not strong, and the Qingkailing preparation amino acid content of producing is lower.
Summary of the invention
The purpose of this invention is to provide the preparation method that a kind of technology is simple, with low cost, can effectively improve content of amino acid of Qingkailing.
The object of the present invention is achieved like this:
The present invention adopts following steps to extract the Cornu Bubali powder in the QINGKAILING pharmaceutical formulation, Concha Margaritifera powder:
A, Cornu Bubali powder place hydrolytic decomposition pot, add 6～10 times of amount 1.0～3.0mol/L Ba (OH) while stirring
2Solution is heated to 95～100 ℃, and insulation hydrolysis 5～10 hours is cooled to 0～15 ℃, and it is standby to get supernatant;
B, Concha Margaritifera powder place hydrolytic decomposition pot, slowly add 6～10 times of amount 2.0～4.0mol/L H
2SO
4Solution is heated to 95～100 ℃, and insulation hydrolysis 5～10 hours is cooled to 10～25 ℃, and it is standby to get supernatant;
C, with the Cornu Bubali supernatant, under agitation add in the Concha Margaritifera supernatant, add an amount of dense H
2SO
4Leave standstill adjust pH to 3.0～5.0; Get mixing supernatant; With NaOH adjust pH to 6.0～7.5, standby;
D, above-mentioned mixing supernatant is concentrated into when being equivalent to 1～4 times of crude drug total amount amount, puts coldly, under agitation add high concentration ethanol, make to contain the alcohol amount and reach 55～65%, cold preservation 5～10 days is filtered, and reclaims ethanol, filtrate for later use;
E, d is gone on foot the described filtrate of operation handle, when treating that liquid level flow to the resin face, use distilled water drip washing, use 1.0～4.0% ammonia desorbings again instead, collect the ammonia washing liquid by styrene type cation exchange resin;
F, with ammonia washing liquid water bath method, add dissolved in distilled water after, add 4.0～8.0 ‰ active carbons by liquor capacity again, stir, leave standstill, take off charcoal and handle, filtrate is Cornu Bubali, Concha Margaritifera mixed extract.
Adopt method for preparing Cornu Bubali, Concha Margaritifera mixed extract again with the QINGKAILING pharmaceutical formulation in other medical material and the various QINGKAILING pharmaceutical preparatioies that are mixed and made into of medicinal substances extract compare with the QINGKAILING pharmaceutical preparation that conventional method prepares, amino acid whose content can improve 10～15% in the QINGKAILING.
In order further to improve amino acid whose content in the QINGKAILING, e goes on foot the said resin treatment of operation, and its control flow velocity is preferably 0.5～3.0ml/min.Preferred 732 styrene type cation exchange resins of the e step said styrene type cation exchange resin of operation.
The present invention is an object of study at Cornu Bubali in the Qingkailing preparation and Concha Margaritifera merely, and it is simple, with low cost to have production technology, the high characteristics of total amino acids content in the preparation.
The specific embodiment
Following examples are used to be described in further detail the present invention, but do not limit the present invention in any form.
Embodiment 1 QINKAILING ZHUSHEYE
Proportional quantity according to the QINGKAILING pharmaceutical formulation takes by weighing cholic acid, Hyodeoxycholic Acid, baicalin, Concha Margaritifera powder, Cornu Bubali powder, Fructus Gardeniae, Radix Isatidis, Flos Lonicerae;
Fructus Gardeniae, Radix Isatidis, that Flos Lonicerae prepares extracting solution according to conventional method is standby;
Cholic acid powder, Hyodeoxycholic Acid powder, baicalin powder mix, and be standby;
Cornu Bubali powder, Concha Margaritifera powder extract in accordance with the following methods:
A, Cornu Bubali powder is placed hydrolytic decomposition pot, add 6 times of amount 1.0mol/L Ba (OH) while stirring
2Solution,, be heated to 95 ℃, insulation hydrolysis 5 hours to a jar interior no brown granule, is cooled to 0 ℃, and inclining, it is standby to get supernatant.
B, Concha Margaritifera powder place hydrolytic decomposition pot, slowly add the H of 6 times of amount 2.0mol/L
2SO
4Solution is treated bubble collapse, reheat to 95 ℃, and insulation hydrolysis 5 hours transfers the yellow-white precipitation to by Lycoperdon polymorphum Vitt to Concha Margaritifera powder, is cooled to 10 ℃, and inclining, it is standby to get supernatant.
C, with the Cornu Bubali supernatant, under agitation add in the Concha Margaritifera supernatant, after whole Cornu Bubali supernatant are added, add an amount of dense H
2SO
4Adjust pH to 3.0 extracts mixed hydrolysis liquid supernatant, and precipitate filters with an amount of purified water boiling washing twice.Merge hydrolyzed solution and cleaning mixture,, filter, get the clear and bright mixed liquor of brownish red with solid NaOH adjust pH to 6.0.
D, above-mentioned clear and bright mixed liquor is put in the concentration tank, be concentrated into when being equivalent to 2 times of amounts of crude drug total amount, put cold.Under agitation add high concentration ethanol, make to contain alcohol amount and reach 55%, cold preservation 5 days is filtered, and filtrate recycling ethanol is to not having alcohol flavor, filtrate for later use.
E, above-mentioned worry liquid is added on 732 styrene type cation exchange resins upper ends, when treating that liquid level flow to the resin face, use distilled water drip washing, use 1.0% ammonia desorbing again instead, the control flow velocity is 0.5ml/min, collection ammonia washing liquid.
F, with ammonia washing liquid water bath method, add the dissolving of an amount of water for injection after, add 4.0 ‰ active carbons by liquor capacity again, stir, left standstill 3～10 minutes, after taking off charcoal and handling, filtrate is Cornu Bubali, Concha Margaritifera mixed extract.
With Cornu Bubali, Concha Margaritifera mixed extract, make injection according to the preparation method of conventional injection with Fructus Gardeniae, Radix Isatidis, Flos Lonicerae extractive solution and cholic acid powder, Hyodeoxycholic Acid powder, baicalin powder.
The QINKAILING ZHUSHEYE of present embodiment preparation utilizes automatic amino acid analyzer to record that total amino acids content is 35.9% in the preparation.
Embodiment 2 Qingkailing capsules
Proportional quantity according to the QINGKAILING pharmaceutical formulation takes by weighing cholic acid, Hyodeoxycholic Acid, baicalin, Concha Margaritifera powder, Cornu Bubali powder, Fructus Gardeniae, Radix Isatidis, Flos Lonicerae;
Fructus Gardeniae, Radix Isatidis, that Flos Lonicerae prepares extracting solution according to conventional method is standby;
Cholic acid powder, Hyodeoxycholic Acid powder, baicalin powder mix, and be standby;
Cornu Bubali powder, Concha Margaritifera powder extract in accordance with the following methods:
A, Cornu Bubali powder is placed hydrolytic decomposition pot, add 8 times of amount 2.0mol/L Ba (OH) while stirring
2Solution is heated to 98 ℃, and insulation hydrolysis 8 hours to a jar interior no brown granule, is cooled to 10 ℃, and inclining, it is standby to get supernatant.
B, Concha Margaritifera powder place hydrolytic decomposition pot, slowly add the H of 6 times of amount 4.0mol/L
2SO
4Solution is treated bubble collapse, reheat to 95 ℃, and insulation hydrolysis 5 hours transfers the yellow-white precipitation to by Lycoperdon polymorphum Vitt to Concha Margaritifera powder, is cooled to 10 ℃, and inclining, it is standby to get supernatant.
C, with the Cornu Bubali supernatant, under agitation add in the Concha Margaritifera supernatant, after whole Cornu Bubali supernatant are added, add an amount of dense H
2SO
4Adjust pH to 3.0 extracts mixed hydrolysis liquid supernatant, and precipitate filters with an amount of purified water boiling washing twice.Merge hydrolyzed solution and cleaning mixture,, filter, get the clear and bright mixed liquor of brownish red with solid NaOH adjust pH to 6.0.
D, above-mentioned clear and bright mixed liquor is put in the concentration tank, be concentrated into when being equivalent to 2 times of amounts of crude drug total amount, put cold.Under agitation add high concentration ethanol, make to contain alcohol amount and reach 55%, cold preservation 5 days is filtered, and filtrate recycling ethanol is to not having alcohol flavor, filtrate for later use.
E, above-mentioned worry liquid is added on 001 * 12 styrene type cation exchange resin upper end, when treating that liquid level flow to the resin face, use distilled water drip washing, use 4.0% ammonia desorbing again instead, the control flow velocity is 3.0ml/min, collection ammonia washing liquid.
F, with ammonia washing liquid water bath method, add the dissolving of an amount of water for injection after, add 8.0 ‰ active carbons by liquor capacity again, stir, left standstill 30 minutes, after taking off charcoal and handling, filtrate is Cornu Bubali, Concha Margaritifera mixed extract.
With Cornu Bubali, Concha Margaritifera mixed extract, make Qingkailing capsules according to conventional preparation of soft capsule method with Fructus Gardeniae, Radix Isatidis, Flos Lonicerae extractive solution and cholic acid powder, Hyodeoxycholic Acid powder, baicalin powder.
The Qingkailing capsules of present embodiment preparation utilizes automatic amino acid analyzer to record that total amino acids content is 32.2% in the preparation.
Embodiment 3 QINGKAILING liquid preparations
Proportional quantity according to the QINGKAILING pharmaceutical formulation takes by weighing cholic acid, Hyodeoxycholic Acid, baicalin, Concha Margaritifera powder, Cornu Bubali powder, Fructus Gardeniae, Radix Isatidis, Flos Lonicerae;
Fructus Gardeniae, Radix Isatidis, that Flos Lonicerae prepares extracting solution according to conventional method is standby;
Cholic acid powder, Hyodeoxycholic Acid powder, baicalin powder mix, and be standby;
Cornu Bubali powder, Concha Margaritifera powder extract in accordance with the following methods:
A, Cornu Bubali powder is placed hydrolytic decomposition pot, add 10 times of amount 3.0mol/L Ba (OH) while stirring
2Solution,, be heated to 100 ℃, insulation hydrolysis 10 hours to a jar interior no brown granule, is cooled to 15 ℃, and inclining, it is standby to get supernatant.
B, Concha Margaritifera powder place hydrolytic decomposition pot, slowly add the H of 6 times of amount 4.0mol/L
2SO
4Solution is treated bubble collapse, reheat to 100 ℃, and insulation hydrolysis 10 hours transfers the yellow-white precipitation to by Lycoperdon polymorphum Vitt to Concha Margaritifera powder, is cooled to 15 ℃, and inclining, it is standby to get supernatant.
C, with the Cornu Bubali supernatant, under agitation add in the Concha Margaritifera supernatant, after whole Cornu Bubali supernatant are added, add an amount of dense H
2SO
4Adjust pH to 4.0 extracts mixed hydrolysis liquid supernatant, and precipitate filters with an amount of purified water boiling washing twice.Merge hydrolyzed solution and cleaning mixture,, filter, get the clear and bright mixed liquor of brownish red with solid NaOH adjust pH to 7.5.
D, above-mentioned clear and bright mixed liquor is put in the concentration tank, be concentrated into when being equivalent to the total 3 times of amounts of crude drug, put cold.Under agitation add high concentration ethanol, make to contain alcohol amount and reach 60%, cold preservation 8 days is filtered, and filtrate recycling ethanol is to not having alcohol flavor, filtrate for later use.
E, above-mentioned worry liquid is added on 001 * 14 styrene type cation exchange resin upper end, when treating that liquid level flow to the resin face, use distilled water drip washing, use 2.0% ammonia desorbing again instead, the control flow velocity is 1.5ml/min, collection ammonia washing liquid.
F, with ammonia washing liquid water bath method, add the dissolving of an amount of water for injection after, add 6.0 ‰ active carbons by liquor capacity again, stir, left standstill 60 minutes, after taking off charcoal and handling, filtrate is Cornu Bubali, Concha Margaritifera mixed extract.
With Cornu Bubali, Concha Margaritifera mixed extract, make the QINGKAILING liquid preparation according to the preparation method of conventional infusion solutions with Fructus Gardeniae, Radix Isatidis, Flos Lonicerae extractive solution and cholic acid powder, Hyodeoxycholic Acid powder, baicalin powder.
The QINGKAILING liquid preparation of present embodiment preparation utilizes automatic amino acid analyzer to record that total amino acids content is 30.6% in the preparation.
Claims (3)
1. preparation method that can improve content of amino acid of Qingkailing is characterized in that Cornu Bubali powder, the Concha Margaritifera powder in the pharmaceutical formulation adopts following steps to extract:
A, Cornu Bubali powder place hydrolytic decomposition pot, add 6～10 times of amount 1.0～3.0mol/L Ba (OH) while stirring
2Solution is heated to 95～100 ℃, and insulation hydrolysis 5～10 hours is cooled to 0～15 ℃, and it is standby to get supernatant;
B, Concha Margaritifera powder place hydrolytic decomposition pot, slowly add 6～10 times of amount 2.0～4.0mol/L H
2SO
4Solution is heated to 95～100 ℃, and insulation hydrolysis 5～10 hours is cooled to 10～25 ℃, and it is standby to get supernatant;
C, with the Cornu Bubali supernatant, under agitation add in the Concha Margaritifera supernatant, add an amount of dense H
25O
4Leave standstill adjust pH to 3.0～5.0; Get mixing supernatant; With NaOH adjust pH to 6.0～7.5, standby;
D, above-mentioned mixing supernatant is concentrated into when being equivalent to 1～4 times of crude drug total amount amount, puts coldly, under agitation add high concentration ethanol, make to contain the alcohol amount and reach 55～65%, cold preservation 5～10 days is filtered, and reclaims ethanol, filtrate for later use;
E, d is gone on foot the described filtrate of operation handle, when treating that liquid level flow to the resin face, use distilled water drip washing, use 1.0～4.0% ammonia desorbings again instead, collect the ammonia washing liquid by styrene type cation exchange resin;
F, with ammonia washing liquid water bath method, add dissolved in distilled water after, add 4.0～8.0 ‰ active carbons by liquor capacity again, stir, leave standstill, take off charcoal and handle, filtrate is Cornu Bubali, Concha Margaritifera mixed extract.
2. the preparation method of raising content of amino acid of Qingkailing according to claim 1 is characterized in that the said resin treatment of e step operation, and its control flow velocity is 0.5～3.0ml/min.
3. the preparation method of raising content of amino acid of Qingkailing according to claim 1 and 2 is characterized in that the said styrene type cation exchange resin of e step operation is 732 styrene type cation exchange resins.
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| CN105878470A (en) * | 2016-06-19 | 2016-08-24 | 神威药业集团有限公司 | Qingkailing pharmaceutical composition |
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| CN101259181B (en) * | 2008-04-16 | 2011-12-28 | 贵州益佰制药股份有限公司 | Preparation of qinkailing freeze-dried injection |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105878470A (en) * | 2016-06-19 | 2016-08-24 | 神威药业集团有限公司 | Qingkailing pharmaceutical composition |
| CN105878470B (en) * | 2016-06-19 | 2019-07-05 | 神威药业集团有限公司 | A kind of Qing kailing pharmaceutical composition |
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Address after: 051430 Hebei province Luancheng County South Pharmaceutical Company Limited Patentee after: China Shineway Pharmaceutical Group Co., Ltd. Address before: 051430 Hebei province Luancheng County South Pharmaceutical Company Limited Patentee before: Shineway Pharmaceutical Co., Ltd. |