CN1238002C - Method for extracting active ingredient of gastrointestinal diseases drug and application thereof - Google Patents
Method for extracting active ingredient of gastrointestinal diseases drug and application thereof Download PDFInfo
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- CN1238002C CN1238002C CN 03117273 CN03117273A CN1238002C CN 1238002 C CN1238002 C CN 1238002C CN 03117273 CN03117273 CN 03117273 CN 03117273 A CN03117273 A CN 03117273A CN 1238002 C CN1238002 C CN 1238002C
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Abstract
The present invention relates to the extraction of Zuojin total alkaloid and applications the Zuojin total alkaloid. In an extraction method of the present invention, golden thread and evodia rutaecarpa are taken for being used as raw materials according to a Zuojin prescription, after the golden thread and the evodia rutaecarpa are respectively pulverized into coarse powder, the golden thread coarse powder and the evodia rutaecarpa coarse powder are mixed; then, 0.5 to 5% of methanol hydrochloride used as an extraction solvent with the weight which is 5 to 10 times heavier than that of the mixed coarse powder is added, the mixed coarse powder and the methanol hydrochloride are processed through the steps of heating refluxing and filtration, and the amalgamation of filtered solutions is carried out, and a methanol hydrochloride extracting solution is obtained; medicine dregs are decocted by water and filtrated, decoction solutions are amalgamated and concentrated, and a concentrated solution is obtained; the methanol hydrochloride extracting solution and the concentrated solution are mixed, placement, deposition, suction filtration are carried out, and methanol in the filtered solution is recovered; then, neutral aluminum chloride is added to the filtered solution, blending and drying are carried out, and the heating, the reflux and the extraction of the filtered solution are carried out by alcohol. Placement, crystallization, suction filtration and drying are carried out, and an extract-the Zuojin total alkaloid is obtained. The Zuojin total alkaloid can be prepared into various medicaments for clinic according to a general preparation technology. The present invention has the characteristics of easy operation, good operation effect, high extract purity, poor hygroscopicity, easy preparation and good quality.
Description
Technical field
The present invention relates to a kind of application of extracting method and extract thereof of Chinese crude drug active ingredient, the particularly a kind of method of extract total alkaloids and application of total alkaloids from Chinese crude drug.
Background technology
The golden medicine in a left side has curative effect preferably for diseases such as acute or chronic gastritis, enteritis, gastric ulcers.But in the left golden medicine production process, be to adopt decocting extraction method (or directly pulverize and make finished medicines) for the extraction of crude drug, the extract that this method obtains is an extractum, this extract purity is low, draw moist strong, the formulation preparation difficulty, the quality of the pharmaceutical preparations is relatively poor, and dose is big.
Summary of the invention
The objective of the invention is to, the extracting method of a kind of treatment gastrointestinal disease medicine active ingredient (Zuojinzong alkaloid) and the application of extract are provided.The extract that utilizes the present invention to obtain is the total alkaloids that contains pharmaceutical compositions, makes medicament with it, can improve preparation level greatly.
Technical scheme of the present invention.Carry out the Zuojinzong alkaloid extraction according to the following steps, described umber is weight portion;
A, get the raw materials ready: get 6 parts of Rhizoma Coptidis, 1 part of Fructus Evodiae mixes Rhizoma Coptidis, Fructus Evodiae pulverize separately as raw material after becoming coarse powder, the A product;
B, extraction: 0.5～5% the hydrochloric acid methanol that adds 5～10 times of amounts of A product total amount in the A product is as extracting solvent, heating and refluxing extraction 2～3 times, and each 0.5～3 hour, filter, merging filtrate must the hydrochloric acid methanol extracting solution; 4～8 times of water gagings of medicinal residues reuse decoct 2～3 times, and each 0.5～3 hour, filter, merge decoction liquor, be concentrated into relative density 0.9～1.40, get concentrated solution; Hydrochloric acid methanol extracting solution and concentrated solution are mixed, place precipitation, sucking filtration, filtrate gets the B product after reclaiming methanol;
C, in the B product, add the neutral alumina of 1.5～4 times of amounts of A product total amount, mixing again after 60～80 ℃ of dryings, extracts 2～3 times with the alcohol heating reflux of 5～10 times of amounts, each 0.5～2 hour, filter, filtrate recycling ethanol, being concentrated into does not have the alcohol flavor, place crystallization, sucking filtration, crystallization promptly get extract Zuojinzong alkaloid 60～80 ℃ of dryings.
In the above-mentioned Zuojinzong alkaloid extracting method, step b is preferably: 0.5～1.5% of 7～9 times of amounts of adding A product total amount hydrochloric acid methanol is as extracting solvent, heating and refluxing extraction 2～3 times in the A product, each 0.5～3 hour, filter, merging filtrate gets the hydrochloric acid methanol extracting solution; 4～8 times of water gagings of medicinal residues reuse decoct 2～3 times, and each 0.5～3 hour, filter, merge decoction liquor, be concentrated into relative density 0.9～1.1, get concentrated solution; Hydrochloric acid methanol extracting solution and concentrated solution are mixed, place precipitation, sucking filtration, filtrate gets the B product after reclaiming methanol.
In the aforesaid Zuojinzong alkaloid extracting method, step c is preferably: the neutral alumina in the B product more than 50 orders of 2～3 times of amounts of adding A product total amount, mixing, again after 60～80 ℃ of dryings, alcohol heating reflux with 5～10 times of amounts extracts 2～3 times, each 0.5～2 hour, filters, filtrate recycling ethanol, being concentrated into does not have the alcohol flavor, places crystallization, sucking filtration, crystallization promptly gets extract Zuojinzong alkaloid 60～80 ℃ of dryings.
In the aforesaid Zuojinzong alkaloid extracting method, better step c is: add 200～300 purpose neutral aluminas of 2～3 times of amounts of A product total amount in the B product, mixing, again after 60～80 ℃ of dryings, alcohol heating reflux with 5～10 times of amounts extracts 2～3 times, each 0.5～2 hour, filters, filtrate recycling ethanol, being concentrated into does not have the alcohol flavor, places crystallization, sucking filtration, crystallization promptly gets extract Zuojinzong alkaloid 60～80 ℃ of dryings.
The alkaloidal application of Zuojinzong, be Zuojinzong alkaloid that aforesaid Zuojinzong alkaloid extracting method is obtained routinely preparation process make the medicament of clinical usefulness.
In the alkaloidal application of above-mentioned Zuojinzong, the medicament of described clinical usefulness is capsule, soft capsule, tablet, granule.
The present invention compared with the prior art because the present invention adopted a kind of new extracting method, the extract that obtains is the total alkaloids that contains pharmaceutical compositions, makes the preparation of left golden medicine be easy to preparation and the quality of the pharmaceutical preparations improves greatly.That the present invention has is easy to implement, implementation result good, the extract purity height, draws moist poorly, and formulation preparation is easy, the measured characteristics of matter.Can be used in the production of Zuojinzong alkaloid extraction and medicament.
The specific embodiment
Embodiment 1.Carry out the Zuojinzong alkaloid extraction according to the following steps.
A, get the raw materials ready: get Rhizoma Coptidis 6Kg, Fructus Evodiae 1Kg becomes coarse powder as raw material with Rhizoma Coptidis, Fructus Evodiae pulverize separately, mix then, the A product;
B, extraction: in the A product, add 56Kg concentration and be 1% hydrochloric acid methanol as extracting solvent, heating and refluxing extraction 2 times, each 2 hours, filter, merging filtrate, the hydrochloric acid methanol extracting solution; 4～8 times of water gagings of medicinal residues reuse decoct 2 times, and each 2 hours, filter, merge decoction liquor, be concentrated into relative density 1.1, get concentrated solution; Hydrochloric acid methanol extracting solution and concentrated solution are mixed, place precipitation, sucking filtration, filtrate gets the B product after reclaiming methanol;
C, in the B product, add 14Kg200～300 purpose neutral aluminas, mixing again after 60～80 ℃ of dryings, extracts 2 times with the alcohol heating reflux of 5～10 times of amounts, each 1 hour, filter, filtrate recycling ethanol, being concentrated into does not have the alcohol flavor, place crystallization, sucking filtration, crystallization promptly get extract Zuojinzong alkaloid 60～80 ℃ of dryings.
Capsule preparation technology routinely, get extract Zuojinzong alkaloid (in berberine hydrochloride) 90Kg, pregelatinized Starch is an amount of, the Zuojinzong alkaloid was pulverized 80 mesh sieves, standby, accurately take by weighing the Zuojinzong alkaloid and the pregelatinized Starch of recipe quantity, mix homogeneously, be filled in the Capsules shell, get 1,000,000 capsules, every contains total alkaloids (in berberine hydrochloride) 90mg.Oral, every day 2 times, each 2.
Embodiment 2.Carry out the Zuojinzong alkaloid extraction according to the following steps.
A, get the raw materials ready: get Rhizoma Coptidis 6Kg, Fructus Evodiae 1Kg becomes coarse powder as raw material with Rhizoma Coptidis, Fructus Evodiae pulverize separately, mix then, the A product;
B, extraction: in the A product, add 50Kg concentration and be 1.2% hydrochloric acid methanol as extracting solvent, heating and refluxing extraction 2 times, each 1 hour, filter, merging filtrate, the hydrochloric acid methanol extracting solution; 4～8 times of water gagings of medicinal residues reuse decoct 2 times, and each 2 hours, filter, merge decoction liquor, be concentrated into relative density 1.1, get concentrated solution; Hydrochloric acid methanol extracting solution and concentrated solution are mixed, place precipitation, sucking filtration, filtrate gets the B product after reclaiming methanol;
C, in the B product, add 20Kg200～300 purpose neutral aluminas, mixing again after 60～80 ℃ of dryings, extracts 2 times with the alcohol heating reflux of 5～10 times of amounts, each 1 hour, filter, filtrate recycling ethanol, being concentrated into does not have the alcohol flavor, place crystallization, sucking filtration, crystallization promptly get extract Zuojinzong alkaloid 60～80 ℃ of dryings.
Soft capsule preparation technology gets extract Zuojinzong alkaloid (in berberine hydrochloride) 90Kg routinely, and vegetable oil is an amount of, soft capsule material is an amount of, the Zuojinzong alkaloid was pulverized 80 mesh sieves, standby, accurately take by weighing the Zuojinzong alkaloid of recipe quantity, it is an amount of to add vegetable oil, the Zuojinzong alkaloid is suspended in the vegetable oil or with vegetable oil is mixed into the thick paste shape, adopt rolling, be filled in than in the capsule, get 1,000,000 soft capsules, every contains total alkaloids (in berberine hydrochloride) 90mg.Oral, every day 2 times, each 2.
Embodiment 3.Carry out the Zuojinzong alkaloid extraction according to the following steps.
A, get the raw materials ready: get Rhizoma Coptidis 6Kg, Fructus Evodiae 1Kg becomes coarse powder as raw material with Rhizoma Coptidis, Fructus Evodiae pulverize separately, mix then, the A product;
B, extraction: in the A product, add 60Kg concentration and be 0.8% hydrochloric acid methanol as extracting solvent, heating and refluxing extraction 2 times, each 2 hours, filter, merging filtrate, the hydrochloric acid methanol extracting solution; 4～8 times of water gagings of medicinal residues reuse decoct 2 times, and each 2 hours, filter, merge decoction liquor, be concentrated into relative density 0.9, get concentrated solution; Hydrochloric acid methanol extracting solution and concentrated solution are mixed, place precipitation, sucking filtration, filtrate gets the B product after reclaiming methanol;
C, in the B product, add 17Kg200～300 purpose neutral aluminas, mixing again after 60～80 ℃ of dryings, extracts 2 times with the alcohol heating reflux of 5～10 times of amounts, each 2 hours, filter, filtrate recycling ethanol, being concentrated into does not have the alcohol flavor, place crystallization, sucking filtration, crystallization promptly get extract Zuojinzong alkaloid 60～80 ℃ of dryings.
Tablet producing technology is got extract Zuojinzong alkaloid (in berberine hydrochloride) 90Kg, starch 48Kg routinely, microcrystalline Cellulose 33Kg, carboxymethyl starch sodium 6.6Kg, 10%PVP ethanol liquid is an amount of, magnesium stearate 2.2Kg, the Zuojinzong alkaloid was pulverized 80 mesh sieves, standby, accurately take by weighing the Zuojinzong alkaloid of recipe quantity, starch and microcrystalline Cellulose, mixing, add 10%PVP ethanol liquid, the system soft material with 16～20 mesh sieves, is granulated soft material, 40～80 ℃ of dryings, the carboxymethyl starch sodium and the magnesium stearate that add recipe quantity, mixing, 20 mesh sieve granulate, survey granule content, determine that sheet is heavy, tabletting, coating, get 1,000,000, every contains total alkaloids (in berberine hydrochloride) 90mg.Oral, every day 2 times, each 2.
Embodiment 4.Carry out the Zuojinzong alkaloid extraction according to the following steps.
A, get the raw materials ready: get Rhizoma Coptidis 6Kg, Fructus Evodiae 1Kg becomes coarse powder as raw material with Rhizoma Coptidis, Fructus Evodiae pulverize separately, mix then, the A product;
B, extraction: in the A product, add 40Kg concentration and be 2% hydrochloric acid methanol as extracting solvent, heating and refluxing extraction 3 times, each 1 hour, filter, merging filtrate, the hydrochloric acid methanol extracting solution; 4～8 times of water gagings of medicinal residues reuse decoct 2 times, and each 2 hours, filter, merge decoction liquor, be concentrated into relative density 1.3, get concentrated solution; Hydrochloric acid methanol extracting solution and concentrated solution are mixed, place precipitation, sucking filtration, filtrate gets the B product after reclaiming methanol;
C, in the B product, add 26Kg200～300 purpose neutral aluminas, mixing again after 60～80 ℃ of dryings, extracts 2 times with the alcohol heating reflux of 5～10 times of amounts, each 1 hour, filter, filtrate recycling ethanol, being concentrated into does not have the alcohol flavor, place crystallization, sucking filtration, crystallization promptly get extract Zuojinzong alkaloid 60～80 ℃ of dryings.
Granule preparation technology routinely, get extract Zuojinzong alkaloid (in berberine hydrochloride) 180Kg, soluble starch 87.8Kg, saccharin sodium 2.2Kg, 10%PVP ethanol liquid is an amount of, the Zuojinzong alkaloid was pulverized 80 mesh sieves, standby, accurately take by weighing the Zuojinzong alkaloid of recipe quantity, soluble starch and saccharin sodium, mixing, add 10%PVP ethanol liquid, the system soft material with 16～20 mesh sieves, is granulated soft material, 40～80 ℃ of dryings, 20 mesh sieve granulate are surveyed granule content, determine every packed amount, get 1,000,000 bags of granules, every bag contains total alkaloids (in berberine hydrochloride) 180mg.Hot water is taken after mixing it with water, every day 2 times, each 1 bag.
Claims (2)
1, the extracting method of treatment gastrointestinal disease medicine active ingredient is characterized in that carry out according to the following steps, described umber is weight portion;
A, get the raw materials ready: get 6 parts of Rhizoma Coptidis, 1 part of Fructus Evodiae mixes Rhizoma Coptidis, Fructus Evodiae pulverize separately as raw material after becoming coarse powder, the A product;
B, extraction: 0.5～1.5% the hydrochloric acid methanol that adds 7～9 times of amounts of A product total amount in the A product is as extracting solvent, heating and refluxing extraction 2～3 times, and each 0.5～3 hour, filter, merging filtrate must the hydrochloric acid methanol extracting solution; 4～8 times of water gagings of medicinal residues reuse decoct 2～3 times, and each 0.5～3 hour, filter, merge decoction liquor, be concentrated into relative density 0.9～1.1, get concentrated solution; Hydrochloric acid methanol extracting solution and concentrated solution are mixed, place precipitation, sucking filtration, filtrate gets the B product after reclaiming methanol;
C, in the B product, add 200～300 purpose neutral aluminas of 2～3 times of amounts of A product total amount, mixing again after 60～80 ℃ of dryings, extracts 2～3 times with the alcohol heating reflux of 5～10 times of amounts, each 0.5～2 hour, filter, filtrate recycling ethanol, being concentrated into does not have the alcohol flavor, place crystallization, sucking filtration, crystallization promptly get extract Zuojinzong alkaloid 60～80 ℃ of dryings.
2, the application of the extract that obtains according to the extracting method of the described treatment gastrointestinal disease of claim 1 medicine active ingredient, it is characterized in that, with extract Zuojinzong alkaloid routinely preparation process make capsule, soft capsule, tablet, the granule of clinical usefulness.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03117273 CN1238002C (en) | 2003-01-28 | 2003-01-28 | Method for extracting active ingredient of gastrointestinal diseases drug and application thereof |
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| CN 03117273 CN1238002C (en) | 2003-01-28 | 2003-01-28 | Method for extracting active ingredient of gastrointestinal diseases drug and application thereof |
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| CN1431014A CN1431014A (en) | 2003-07-23 |
| CN1238002C true CN1238002C (en) | 2006-01-25 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100375627C (en) * | 2005-08-26 | 2008-03-19 | 上海中医药大学 | Application of match drug Chinese goldthread and evodia fruit extracts in preparation of medicine for preventing and treating cancer |
| CN100563686C (en) * | 2006-11-14 | 2009-12-02 | 南京中医药大学 | A kind of gastric floating capsule of ' Zuo Jin Wan ' and preparation method thereof |
| CN102058703A (en) * | 2011-01-07 | 2011-05-18 | 顺德职业技术学院 | Zuojin helicobacter-pylori-resistant floating tablets and preparation method thereof |
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Owner name: GUIYANG HAOZHEN DRUG DEVELOPMENT CO., LTD. Free format text: FORMER OWNER: GUANGZHOU HONGXIN PHARMACEUTICAL VOCATIONAL TECHNICAL SCHOOL Effective date: 20110130 |
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Free format text: CORRECT: ADDRESS; FROM: 550025 NO.40 (LUOSICHONG), SOUTH SECTION, HUAXI AVENUE, GUIYANG CITY, GUIZHOU PROVINCE TO: 550003 NO.7, UNIT 2, BUILDING 9, ZHAOHUI FACTORY, JINZHU TOWN, XIAOHE DISTRICT, GUIYANG CITY, GUIZHOU PROVINCE |
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Effective date of registration: 20110130 Address after: 550003 Guizhou city of Guiyang Province River District Jin Zhu Zhen Zhaohui Factory nine building two unit 7 Patentee after: Guiyang Haozhen Pharmaceutical Development Co., Ltd. Address before: 550025, No. 40, south section, Huaxi Road, Guiyang, Guizhou Patentee before: Hongxin employment Technology School of Medicine Industry, Guizhou |
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Granted publication date: 20060125 Termination date: 20130128 |