CN103099891A - Preparation method of belladonna extract - Google Patents
Preparation method of belladonna extract Download PDFInfo
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- CN103099891A CN103099891A CN2011103625468A CN201110362546A CN103099891A CN 103099891 A CN103099891 A CN 103099891A CN 2011103625468 A CN2011103625468 A CN 2011103625468A CN 201110362546 A CN201110362546 A CN 201110362546A CN 103099891 A CN103099891 A CN 103099891A
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Abstract
The invention discloses a preparation method of belladonna extract, belongs to the technical field of medicine, and in particular relates to a preparation method of belladonna extract. A preparation method of belladonna extract with short process flow and high purity is provided. The method is free from sewage disposal and environment-friendly. The preparation method comprises the following steps of: using belladonna herb as a raw material, crushing, adding a sulfuric acid or hydrochloric acid solution, stirring, filtering a stirred solution, performing resin adsorption and separation on the filtrate, eluting by an ethanol solution, and concentrating the elution to obtain the belladonna extract. By adopting the normal temperature acid solution extracting method, chlorophyll and impurity digestion is less; belladonna alkaloid is easier to extract in the acid solution, so that the extracted solution has high effective component content and less impurity.
Description
Technical field
The invention belongs to medical technical field, be specifically related to a kind of preparation method of belladonna extract.
Background content
Semen daturae is a kind of Solanaceae herbaceous plant, and effective ingredient is hyoscyamine, acts on identically with atropine, is mainly used in stomach spasm, Stomach duodenum ulcer, biliary colic, the stomachache that ureteral calculus etc. cause, the vomiting that gastritis and stomach spasm cause and diarrhoea.Domestic present extraction process mostly adopts 85% acetic acid percolation to extract belladonna extract, and still, the shortcoming of current technology is that extraction process is long, and chlorophyll is many, and except unclean, the product impurity level is large.
Summary of the invention
The technical problem to be solved in the present invention is to provide the preparation method of the belladonna extract that a kind of technological process is short, purity is high, and the method is without blowdown, and is environment friendly and pollution-free.
The technical scheme of technical solution problem of the present invention is:
Belladonna extract preparation method of the present invention is: take Herba Belladonnae as raw material, be 10 with raw material pulverizing---20 order fine powders, add fine powder sulphuric acid or hydrochloric acid solution to stir, filter and stir liquid, after filtrate is separated with resin absorption, use the alcoholic solution eluting, then eluent be concentrated to the alcohol amount 25 that contains---35%, get belladonna extract.
The described sulfuric acid solution of belladonna extract preparation method of the present invention refers to that concentration is 0.05---0.5% aqueous sulfuric acid.
It is 0.1 that the described hydrochloric acid solution of belladonna extract preparation method of the present invention refers to add concentration---2% aqueous hydrochloric acid solution.
Belladonna extract preparation method of the present invention is described adds sulphuric acid or hydrochloric acid solution stirring to be: add at twice sulphuric acid or hydrochloric acid solution to stir, each time of stirring is 2---4 hours.
The above-mentioned method that adds at twice sulphuric acid or hydrochloric acid solution to stir is: adding for the first time sulphuric acid or hydrochloric acid solution is 10 of raw material weight---12 times, filter; Adding for the second time sulphuric acid or hydrochloric acid solution is 6 of raw material weight---8 times, filter; Merge and stir liquid; Each time of stirring is 2---4 hours.
The described filtrate resin absorption of belladonna extract preparation method of the present invention is to use the D101 macroporous resin adsorption, absorption flow velocity 2---5BV/H, then be washed till PH=6 with the clear water of 6BV---7.
Belladonna extract preparation method of the present invention is described with the alcoholic solution eluting is: with 75%---85% alcoholic solution eluting, elution flow rate are 3BV/H.
The invention has the beneficial effects as follows:
1, because the present invention adopts room temperature acid solution extraction method, chlorophyll and impurity stripping are few, and belladonna alkaloids more easily is extracted in acid solution, so in the solution that extracts, effective component content is high, impurity is few, and energy consumption is low;
2, in method of the present invention, after resin absorption, belladonna alkaloids is selectively adsorbed by resin, other impurity flows out with sour water and is not adsorbed, use again a small amount of alcoholic solution eluting, obtain in belladonna extract belladonna alkaloids content high, therefore, extract purity is relatively high, and cost is lower;
3, the inventive method acid solution used can reuse, next batch extract acid solution used can use last consignment of time through tree refer to adsorb acid solution, so both saved water and acid, non-wastewater discharge again can be to environment.
The specific embodiment
Below in conjunction with embodiment, the present invention is described in further details.
Embodiment 1:
1, get Semen daturae raw material 100kg, pulverizing is 10---20 orders;
2, add 0.5% hydrochloric acid solution to stir twice the Semen daturae raw material of pulverizing, each 3 hours, adding for the first time aqueous hydrochloric acid solution was 10 times of raw material weight, and adding for the second time aqueous hydrochloric acid solution is 6 times of raw material weight, merges and stirs liquid, filters;
3, filtrate is separated at the hole resin absorption through D101, absorption flow velocity 3BV/H, then be washed till PH=6 with the clear water of 6BV---7;
4, with 4BV 75% alcoholic solution eluting, elution flow rate is 3BV/H, collects eluent;
5, eluent is concentrated into the alcohol amount of containing approximately 30%, gets 13.6kg content and be 1.61% belladonna extract, collect rate as 89.4% take material content.
Embodiment 2:
1, get Semen daturae raw material 100kg, pulverizing is 10---20 orders;
2, add 0.1% sulfuric acid solution to stir twice the Semen daturae raw material of pulverizing, each 3 hours, adding for the first time aqueous sulfuric acid was 12 times of raw material weight, and adding for the second time aqueous sulfuric acid is 8 times of raw material weight, merges and stirs liquid, filters;
3, filtrate is separated at the hole resin absorption through D101, absorption flow velocity 3BV/H, then be washed till PH=6 with the clear water of 6BV---7;
4, with 4BV 80% alcoholic solution eluting, elution flow rate is 3BV/H, collects eluent;
5, eluent is concentrated into the alcohol amount of containing approximately 30%, gets 14.9kg content and be 1.53% belladonna extract, collect rate as 93.1% take material content.
The said BV of the present invention is times column volume unit.
Claims (7)
1. the preparation method of a belladonna extract, it is characterized in that: take Herba Belladonnae as raw material, be 10 with raw material pulverizing---20 order fine powders, add fine powder sulphuric acid or hydrochloric acid solution to stir, filter and stir liquid, after filtrate is separated with resin absorption, use the alcoholic solution eluting, again eluent is concentrated to and contains to containing alcohol amount 25---35%, get belladonna extract.
2. said preparation method according to claim 1, it is characterized in that: described sulfuric acid solution refers to that concentration is 0.05---0.5% aqueous sulfuric acid.
3. said preparation method according to claim 1, it is characterized in that: described hydrochloric acid solution refers to that concentration is 0.1---2% aqueous hydrochloric acid solution.
4. said preparation method according to claim 1 is characterized in that: described to add sulphuric acid or hydrochloric acid solution to stir be to add at twice sulphuric acid or hydrochloric acid solution to stir, and each time of stirring is 2---4 hours.
5. said preparation method according to claim 4, it is characterized in that: the described method that adds at twice sulphuric acid or hydrochloric acid solution to stir is: adding for the first time sulphuric acid or hydrochloric acid solution is 10 of raw material weight---12 times, filter; Adding for the second time sulphuric acid or hydrochloric acid solution is 6 of raw material weight---8 times, filter; Merge and stir liquid; Each time of stirring is 2---4 hours.
6. said extract according to claim 1, it is characterized in that: described filtrate resin absorption is to use the D101 macroporous resin adsorption, absorption flow velocity 2---5BV/H, then be washed till PH=6 with the clear water of 6BV---7.
7. said extract according to claim 1 is characterized in that: describedly with the alcoholic solution eluting be: with 75%---85% alcoholic solution eluting, elution flow rate are 3BV/H.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104387380A (en) * | 2013-11-29 | 2015-03-04 | 江苏汉邦科技有限公司 | Preparation method of hyoscyamine in Flos Daturae Innoxiae |
CN111588775A (en) * | 2020-06-15 | 2020-08-28 | 弘美制药(中国)有限公司 | Belladonna extract and belladonna capsule compound preparation |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104387380A (en) * | 2013-11-29 | 2015-03-04 | 江苏汉邦科技有限公司 | Preparation method of hyoscyamine in Flos Daturae Innoxiae |
CN111588775A (en) * | 2020-06-15 | 2020-08-28 | 弘美制药(中国)有限公司 | Belladonna extract and belladonna capsule compound preparation |
CN111588775B (en) * | 2020-06-15 | 2022-01-18 | 弘美制药(中国)有限公司 | Belladonna extract and belladonna capsule compound preparation |
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