CN102657696A - Process for extracting total alkali of sophora alopecuroide - Google Patents
Process for extracting total alkali of sophora alopecuroide Download PDFInfo
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- CN102657696A CN102657696A CN2012101351148A CN201210135114A CN102657696A CN 102657696 A CN102657696 A CN 102657696A CN 2012101351148 A CN2012101351148 A CN 2012101351148A CN 201210135114 A CN201210135114 A CN 201210135114A CN 102657696 A CN102657696 A CN 102657696A
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Abstract
The invention provides a process for extracting total alkali of sophora alopecuroide. The process comprises the following steps of: smashing, drawing, concentrating, extracting and the like. By adopting a continuous backflow water extraction method, the production cost is low, the process is simple, and the method is suitable for industrial large-scale production; organic solvents are not retained in a product; the total sophoridine content is up to 96 percent; and other processes can hardly reach the purity.
Description
Technical field
The present invention relates to a kind of extraction process of Herba Sophorae alopecuroidis total alkali.
Background technology
Herba Sophorae alopecuroidis (sophora alopecuroides L.) is a cassia leguminous plant, has another name called Sophora Alopecuroides L., Herba Astragali Melilotoidis, Radix Sophorae Alopecuroidis, Europe Radix Sophorae Flavescentis etc., is a kind of deleterious herbaceos perennial on China's desert steppe and calacareous soil or the sand dune, in the farmland.Herba Sophorae alopecuroidis is cold in nature, and bitter in the mouth has effects such as clearing away heat-damp and promoting diuresis, pain relieving, parasite killing.Contain multiple alkaloid in the Herba Sophorae alopecuroidis, alkaloid is the main bioactive ingredients of Herba Sophorae alopecuroidis, removes to also have flavonoid, polysaccharide etc. in addition.China's Herba Sophorae alopecuroidis resource is very abundant, mainly is distributed in the ground such as Xinjiang, Ningxia, Gansu, Shaanxi of northern China.
Alkaloid is meant that one type is present in complex structure in the organism, has the very alkaline organic compound of Johnson & Johnson's reason effect.Most of alkaloids are nitrogenous heterocyclic compound, and optically active and tangible biological activity are arranged, and it is morning and one type of maximum natural organic-compound of human research, is one of topmost source of modern medicines.
Herba Sophorae alopecuroidis is of many uses, and China is medicinal to have long history, also is the flavoring agent of special mouthfeel simply; Alkaloid in the Herba Sophorae alopecuroidis belongs to the extraction medicine of pure natural product; Can degrade rapidly, no ecological environmental pollution problem has higher selectivity; To the person poultry safety and do not produce resistance, have no poisoning, plant growth is had stimulation, the insect pest of can doublely curing the disease, improves the advantages such as immunologic function of plant.
At present; Method for distilling about Herba Sophorae alopecuroidis total alkali has water extraction, ethanol extraction method, acid extraction method, resin method etc., and the disclosed Herba Sophorae alopecuroidis total alkali method for distilling of Chinese patent has only ethanol extraction method, as: among the CN1273870A " preparation technology of Herba Sophorae alopecuroidis total alkali liquid "; Adopt the alcohols solvent heating extraction; This method no doubt has its saving grace, but if carry out the large-scale production in the industry, water extraction method will obviously reduce production costs; And make the Herba Sophorae alopecuroidis total alkali yield reach 6.3%～7.2% (with acid-dye colorimetry mensuration total alkaloid contents in the Herba Sophorae alopecuroidis sample is measured, measuring the result is 8.21% for total alkaloid content in the Herba Sophorae alopecuroidis sample).Among the Chinese patent CN1368502A " preparation technology of Herba Sophorae alopecuroidis total alkali ", its process only be from the Herba Sophorae alopecuroidis extracting solution extract, concentrate or hydrogenation after extract, concentrate, promptly get Herba Sophorae alopecuroidis total alkali.This method is simple and feasible no doubt, but wherein contains many other biological alkali or impurity, makes gained Herba Sophorae alopecuroidis total alkali content very low, and the production yield is lower in the industry.The present invention has overcome above technological deficiency, adopts water extraction, concentrates, extraction, recovery, crystalline method, not only reduces production costs, and makes gained Herba Sophorae alopecuroidis total alkali yield high, and Functionality, quality and appealing design meets the requirement of the various medicine preparations of crude drug preparation thus.
Summary of the invention
For realizing this purpose, the concrete processing step that the present invention adopts is following:
(1) pulverize: the Herba Sophorae alopecuroidis that will clean is ground into coarse powder, and moistening is subsequent use;
(2) extract: the coarse powder that moistening is good is put into the Continuous Countercurrent Extraction unit, and temperature is controlled at 80～95 ℃ and carries out the continuous flow upstream water extraction;
(3) concentrate: the concentrated receipts in the cream jar of extracting solution suction economic benefits and social benefits concentrated;
(4) single extraction, neutralization: adding sheet alkali in the concentrated solution, to transfer pH value be 11～12, adds organic solvent extraction, in concentrated solution, do not have or have minute quantity alkaloid colour developing speckle to get final product water-break; Adding the acid neutralization, is 4～5 until a neutralizer pH value;
(5) reextraction, neutralization: adding sheet alkali in the neutralizer, to transfer pH value be 11～12, adds organic solvent extraction, in concentrated solution, do not have or have minute quantity alkaloid colour developing speckle to get final product water-break; Adding the acid neutralization, is 5～6 until secondary neutralizer pH value;
(6) rough: it is 11～12 that the secondary neutralizer adds liquid caustic soda accent pH value, adds other a kind of organic substance extraction, until alkali waste water water-break after detecting inanimate object alkali colour developing speckle;
(7) reclaim: the another kind of Organic substance of heating recovery is to doing, add water stirring, dissolving, evacuation more than 16 hours to the thick paste shape;
(8) refining: add dissolve with ethanol, filter, 85 ± 5 ℃ of heating-up temperatures reclaim ethanol to there not being the ethanol flavor, stir and promptly get sepia paste Herba Sophorae alopecuroidis total alkali elaboration.
In said (2) step, extracting institute's water is drinking water, purified water.
Said (4), (5) are in the step, and sheet alkali is solid sodium hydroxide, potassium hydroxide, sodium carbonate; Acid is hydrochloric acid, sulphuric acid, acetic acid, and organic solvent is a benzene,toluene,xylene.
In said (6) step, liquid caustic soda is sodium hydroxide, potassium hydroxide, sodium carbonate liquor.
Said (6), (7) are in the step, and said other a kind of Organic substance is chloroform, ethanol.
In said (7) step, it is purified water, drinking water that recovery institute adds water.
The characteristics that the present invention gives prominence to adopt water extraction process exactly, can make the Herba Sophorae alopecuroidis total alkali yield reach 6.3%～7.2%, not only reduce production costs, and make simple for processly, do not influence simultaneously the high-quality of product.
Description of drawings
Accompanying drawing 1 is process chart of the present invention.
The specific embodiment
Embodiment 1:
(1) pulverize: the Herba Sophorae alopecuroidis that will clean is ground into coarse powder, and moistening is subsequent use;
(2) extract: the coarse powder that moistening is good is put into the Continuous Countercurrent Extraction unit, and temperature is controlled at 80～95 ℃ and carries out the continuous flow upstream water extraction;
(3) concentrate: the concentrated receipts in the cream jar of extracting solution suction economic benefits and social benefits concentrated;
(4) single extraction, neutralization: add caustic soda in the concentrated solution, transferring pH value is 11～12, adds extracted in toluene, in concentrated solution, does not have or has minute quantity alkaloid colour developing speckle to get final product water-break; Adding the neutralization of 10% hydrochloric acid, is 4～5 until a neutralizer pH value;
(5) reextraction, neutralization: add caustic soda in the neutralizer, transferring pH value is 11～12, adds extracted in toluene, in concentrated solution, does not have or has minute quantity alkaloid colour developing speckle to get final product water-break; Adding the neutralization of 10% hydrochloric acid, is 5～6 until secondary neutralizer pH value;
(6) rough: it is 11～12 that the secondary neutralizer adds 30% sodium hydroxide accent pH value, adds the chloroform extraction, until alkali waste water water-break after detecting inanimate object alkali colour developing speckle;
(7) reclaim: the another kind of Organic substance of heating recovery is to doing, add water stirring, dissolving, evacuation more than 16 hours to the thick paste shape;
(8) add dissolve with ethanol, filter, 85 ℃ of heating-up temperatures reclaim ethanol to there not being the ethanol flavor, stir and promptly get sepia paste Herba Sophorae alopecuroidis total alkali elaboration.
Embodiment 2:
(1) pulverize: the Herba Sophorae alopecuroidis that will clean is ground into coarse powder, and moistening is subsequent use;
(2) extract: the coarse powder that moistening is good is put into the Continuous Countercurrent Extraction unit, and temperature is controlled at 80～95 ℃ and carries out water extraction;
(3) concentrate: the concentrated receipts in the cream jar of extracting solution suction economic benefits and social benefits concentrated;
(4) single extraction, neutralization: adding the solid sodium hydroxide in the concentrated solution, to transfer pH value be 11～12, adds the benzene extraction, in concentrated solution, do not have or have minute quantity alkaloid colour developing speckle to get final product water-break; Adding 10% hydrochloric acid neutralization, is 4 until a neutralizer pH value;
(5) reextraction, neutralization: adding the solid sodium hydroxide in the neutralizer, to transfer pH value be 11, adds the benzene extraction, in concentrated solution, do not have or have minute quantity alkaloid colour developing speckle to get final product water-break; Adding 10% hydrochloric acid neutralization, is 5 until secondary neutralizer pH value;
(6) rough: the secondary neutralizer adds 30% sodium hydroxide, and to transfer pH value be 11, adds the chloroform extraction, until alkali waste water water-break after detecting inanimate object alkali colour developing speckle;
(7) reclaim: heating recovery organic solvent chloroform is to doing, add purified water stirring, dissolving, evacuation more than 16 hours to the thick paste shape;
(8) add dissolve with ethanol, filter, 88 ℃ of heating-up temperatures reclaim ethanol to there not being the ethanol flavor, stir and promptly get sepia paste Herba Sophorae alopecuroidis total alkali elaboration.
Claims (6)
1. the extraction process of a Herba Sophorae alopecuroidis total alkali is characterized in that this method for distilling comprises pulverizing, extraction, concentrates and process such as extraction, and concrete steps are:
(1) pulverize: the Herba Sophorae alopecuroidis that will clean is ground into coarse powder, and moistening is subsequent use;
(2) extract: the coarse powder that moistening is good is put into the Continuous Countercurrent Extraction unit, and temperature is controlled at 80～95 ℃ and carries out the continuous flow upstream water extraction;
(3) concentrate: the concentrated receipts in the cream jar of extracting solution suction economic benefits and social benefits concentrated;
(4) single extraction, neutralization: adding sheet alkali in the concentrated solution, to transfer pH value be 11～12, adds organic solvent extraction, in concentrated solution, do not have or have minute quantity alkaloid colour developing speckle to get final product water-break; Adding the acid neutralization, is 4～5 until a neutralizer pH value;
(5) reextraction, neutralization: adding sheet alkali in the neutralizer, to transfer pH value be 11～12, adds organic solvent extraction, in concentrated solution, do not have or have minute quantity alkaloid colour developing speckle to get final product water-break; Adding the acid neutralization, is 5～6 until secondary neutralizer pH value;
(6) rough: it is 11～12 that the secondary neutralizer adds liquid caustic soda accent pH value, adds other a kind of organic solvent extraction, until alkali waste water water-break after detecting inanimate object alkali colour developing speckle;
(7) reclaim: the another kind of Organic substance of heating recovery is to doing, add water stirring, dissolving, evacuation more than 16 hours to the thick paste shape;
(8) add dissolve with ethanol, filter, 85 ± 5 ℃ of heating-up temperatures reclaim ethanol to there not being the ethanol flavor, stir and promptly get sepia paste Herba Sophorae alopecuroidis total alkali elaboration.
2. according to claim 1 in (2) step, it is characterized in that said extraction institute water is drinking water, purified water.
3. during according to claim 1 (4), (5) go on foot, it is characterized in that said alkali is solid sodium hydroxide, potassium hydroxide, sodium carbonate; Acid is hydrochloric acid, sulphuric acid, acetic acid, and organic solvent is a benzene,toluene,xylene.
4. according to claim 1 in (6) step, it is characterized in that said liquid caustic soda is sodium hydroxide, potassium hydroxide, sodium carbonate liquor.
5. during according to claim 1 (6), (7) go on foot, it is characterized in that said other a kind of organic solvent is chloroform, ethanol.
6. according to claim 1 in (7) step, it is characterized in that it is purified water, drinking water that said recovery adds water.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104825533A (en) * | 2015-05-07 | 2015-08-12 | 江苏天晟药业有限公司 | Preparation method of sophora alopecuroides total alkaloid |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1110339C (en) * | 2000-06-19 | 2003-06-04 | 宁夏药物研究所 | Process for preparing total allooerine liquid |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1110339C (en) * | 2000-06-19 | 2003-06-04 | 宁夏药物研究所 | Process for preparing total allooerine liquid |
Non-Patent Citations (1)
| Title |
|---|
| 张珍明: "水蒸气蒸馏技术在精细化学品生产中的应用", 《化工时刊》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104825533A (en) * | 2015-05-07 | 2015-08-12 | 江苏天晟药业有限公司 | Preparation method of sophora alopecuroides total alkaloid |
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Application publication date: 20120912 |