CN1110339C - Process for preparing total allooerine liquid - Google Patents
Process for preparing total allooerine liquid Download PDFInfo
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- CN1110339C CN1110339C CN00109238A CN00109238A CN1110339C CN 1110339 C CN1110339 C CN 1110339C CN 00109238 A CN00109238 A CN 00109238A CN 00109238 A CN00109238 A CN 00109238A CN 1110339 C CN1110339 C CN 1110339C
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- 239000007788 liquid Substances 0.000 title claims abstract description 39
- 238000004519 manufacturing process Methods 0.000 title abstract description 5
- 238000005516 engineering process Methods 0.000 claims abstract description 26
- 241000219784 Sophora Species 0.000 claims abstract description 18
- 238000010992 reflux Methods 0.000 claims abstract description 17
- 238000000605 extraction Methods 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 13
- 239000003513 alkali Substances 0.000 claims abstract description 10
- 150000003839 salts Chemical class 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims description 35
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 34
- 239000000284 extract Substances 0.000 claims description 33
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 27
- 241001145009 Sophora alopecuroides Species 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 22
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 229930013930 alkaloid Natural products 0.000 claims description 17
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 150000003797 alkaloid derivatives Chemical class 0.000 claims description 15
- 235000012054 meals Nutrition 0.000 claims description 15
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 11
- 150000001350 alkyl halides Chemical class 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 11
- 150000001298 alcohols Chemical class 0.000 claims description 10
- 239000012141 concentrate Substances 0.000 claims description 10
- 150000002148 esters Chemical class 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 8
- 150000001555 benzenes Chemical class 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000007654 immersion Methods 0.000 claims description 5
- 238000012856 packing Methods 0.000 claims description 5
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 5
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical group CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 claims description 3
- 125000001340 2-chloroethyl group Chemical class [H]C([H])(Cl)C([H])([H])* 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 2
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract 1
- 238000009833 condensation Methods 0.000 abstract 1
- 230000005494 condensation Effects 0.000 abstract 1
- 230000007547 defect Effects 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 230000020477 pH reduction Effects 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 238000009736 wetting Methods 0.000 abstract 1
- ZSBXGIUJOOQZMP-UHFFFAOYSA-N Isomatrine Natural products C1CCC2CN3C(=O)CCCC3C3C2N1CCC3 ZSBXGIUJOOQZMP-UHFFFAOYSA-N 0.000 description 4
- ZSBXGIUJOOQZMP-JLNYLFASSA-N Matrine Chemical compound C1CC[C@H]2CN3C(=O)CCC[C@@H]3[C@@H]3[C@H]2N1CCC3 ZSBXGIUJOOQZMP-JLNYLFASSA-N 0.000 description 3
- 229930014456 matrine Natural products 0.000 description 3
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 2
- ZSBXGIUJOOQZMP-BHPKHCPMSA-N sophoridine Chemical compound C1CC[C@@H]2CN3C(=O)CCC[C@@H]3[C@@H]3[C@H]2N1CCC3 ZSBXGIUJOOQZMP-BHPKHCPMSA-N 0.000 description 2
- AAGFPTSOPGCENQ-UHFFFAOYSA-N Sophocarpin I Natural products C1CCC2CN3C(=O)C=CCC3C3C2N1CCC3 AAGFPTSOPGCENQ-UHFFFAOYSA-N 0.000 description 1
- IGXQFUGORDJEST-UHFFFAOYSA-N Sophocarpine Natural products O=C1C=CCC2C3CCCC4CCCC(CN12)C34 IGXQFUGORDJEST-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000003810 ethyl acetate extraction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- AAGFPTSOPGCENQ-JLNYLFASSA-N sophocarpine Chemical compound C1CC[C@H]2CN3C(=O)C=CC[C@@H]3[C@@H]3[C@H]2N1CCC3 AAGFPTSOPGCENQ-JLNYLFASSA-N 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The present invention provides a technology for preparing sophora total alkali liquid, which overcomes the defects of low yield, low practicability and unsuitable commercial production of the existing public technologies. The technology comprises the following technological steps: pulverization, wetting, reflux extraction, condensation, centrifugal filtration, acidification, alkalization, salt conversion, etc. The present invention has the advantages of reasonable technology and high total alkali yield, and is suitable for industrialized large-scale production.
Description
Technical field
The present invention relates to alkaloid extraction in the Sophora alopecuroide, especially the preparation technology of sophora alapecuroides liquid.
Background technology
The Sophora alopecuroide plant in Ningxia, there is very rich in natural resources in province such as Inner Mongol, Gansu and Xinjiang.Contain multiple alkaloids such as matrine, Sophoridine, sophocarpine in the Sophora alopecuroide, because various alkaloids have very high medical value, therefore, extracting alkaloid from Sophora alopecuroide has high economic benefit and social benefit.Various alkaloid extraction are to extract sophora alapecuroides liquid from Sophora alopecuroide at all, could further isolate single alkaloid then." technology for preparing matrine from Sophora alopecuroide " is disclosed among the Chinese patent CN1044475C, directly from the Sophora alopecuroide separating matrine, the compound that utilizes benzene or alkyl halide are disclosed as solvent, the refluxing extraction alkaloid in the technology, but its technology does not have industrial applicibility, and yield is very low.At present, on industrial applications, also there is not to be fit to the technology of large-scale industrial production sophora alapecuroides liquid.
Summary of the invention
It is simple, practical to the purpose of this invention is to provide a kind of technology, is fit to suitability for industrialized production, the preparation technology of the sophora alapecuroides liquid that yield is high.
For achieving the above object, the present invention is by the following technical solutions:
The preparation technology of sophora alapecuroides liquid, concrete processing step is as follows:
(1) pulverize: with the seed of Sophora alopecuroide or/and root, stem, leaf are ground into meal;
(2) moistening with adding water in the Sophora alopecuroide meal, put to seal in the container and place more than 24 hours;
(3) refluxing extraction:, in the refluxing extraction of packing into the device, add alcohols solvent to flooding on the material face with the Sophora alopecuroide meal after moistening, close extractor, soak more than 12 hours, concentration tank is put in immersion liquid, close the return pipe valve, add alcohols solvent in the extractor again to flooding on the material face heating, after treating that solvent begins to reflux, open solvent return pipe valve, extract continuously, extract after 8 hours, check in the extract not contain till the alkaloid that it is standby to reclaim alcohols solvent;
(4) concentrate: extract in the concentration tank is concentrated, and it is standby to reclaim alcohols solvent;
(5) centrifugal filtration: will be acidified with acid centrifugal filtration in the concentrate, get cleaner liquid;
(6) acidifying: cleaner liquid is inserted in the retort, add benzene kind solvent 20% (V/V), stir and extract, emit the sour water layer, it is standby that the way of distillation reclaims benzene kind solvent;
(7) alkalization: the sour water layer adds alkali and alkalizes, and adds again in the retort, extracts for several times with benzene class, alkyl halide, esters solvent, and each benzene class, alkyl halide, esters solvent consumption are 20% (V/V), get extract;
(8) change salt: used benzene class, alkyl halide, esters solvent are changed in 10% aqueous sulfuric acid, stir, the alkaloid salify is changed in the sour water, it is standby to reclaim benzene class, alkyl halide, esters solvent, collects acid liquid promptly.
Described alcohols solvent is methyl alcohol or ethanol.
Described benzene kind solvent is benzene, toluene or ethylbenzene.
The acid that is acidified with acid in the described centrifugal filtration processing step is sulfuric acid or hydrochloric acid.
The alkali that adds the alkali alkalization in the described alkalization process step is caustic soda.
Described alkyl halide is dichloroethanes, chloroethanes, chloroform, carrene or carbon tetrachloride.
Described ester class is an ethyl acetate.
The present invention has following advantage and effect:
(1) raw material is easy to get, and cost is low.
The Sophora alopecuroide plant is widely distributed, gather easily, thereby cost of material is low.
(2) technology is reasonable, total alkali yield height.
Through ten crowdes of production results are tested, the total alkali yield is 3.25,2.90,3.40,2.25,2.95,2.90,3.50,3.30,3.00,2.50, thereby determines that yield is stable at about 2.95, belongs to high level.
(3) technology is practical, is fit to industrial mass production.
Description of drawings
Fig. 1 prepares the process chart of sophora alapecuroides liquid for the present invention.
The specific embodiment
Embodiment one:
The preparation technology of sophora alapecuroides liquid, concrete processing step is as follows:
(1) pulverizes: the seed of Sophora alopecuroide or root, stem, leaf are ground into meal;
(2) moistening with adding water in the Sophora alopecuroide meal, put to seal in the container and place more than 24 hours;
(3) refluxing extraction:, in the refluxing extraction of packing into the device, add methyl alcohol to flooding on the material face with the Sophora alopecuroide meal after moistening, close extractor, soak more than 12 hours, concentration tank is put in immersion liquid, close the return pipe valve, add methyl alcohol in the extractor again to flooding on the material face heating, after treating that solvent begins to reflux, open solvent return pipe valve, extract continuously, extract after 8 hours, check in the extract not contain till the alkaloid that it is standby to reclaim methyl alcohol;
(4) concentrate: extract in the concentration tank is concentrated, and it is standby to reclaim methyl alcohol;
(5) centrifugal filtration: will add sulfuric acid acidation centrifugal filtration in the concentrate, get cleaner liquid;
(6) acidifying: cleaner liquid is inserted in the retort, add toluene 20% (V/V), stir and extract, emit the sour water layer, it is standby that the way of distillation reclaims toluene;
(7) alkalize: the sour water layer adds the caustic soda alkalization, adds again in the retort, extracts for several times with toluene, and each toluene consumption is 20% (V/V), gets extract;
(8) change salt: toluene is changed in 10% aqueous sulfuric acid, stir, the alkaloid salify is changed in the sour water, it is standby to reclaim toluene, collects acid liquid promptly.
Embodiment two:
The preparation technology of sophora alapecuroides liquid, concrete processing step is as follows:
(1) pulverizes: seed and root, stem, the leaf of Sophora alopecuroide are ground into meal;
(2) moistening with adding water in the Sophora alopecuroide meal, put to seal in the container and place more than 24 hours;
(3) refluxing extraction:, in the refluxing extraction of packing into the device, add ethanol to flooding on the material face with the Sophora alopecuroide meal after moistening, close extractor, soak more than 12 hours, concentration tank is put in immersion liquid, close the return pipe valve, add ethanol in the extractor again to flooding on the material face heating, after treating that solvent begins to reflux, open solvent return pipe valve, extract continuously, extract after 8 hours, check in the extract not contain till the alkaloid that it is standby to reclaim ethanol;
(4) concentrate: extract in the concentration tank is concentrated, and it is standby to reclaim ethanol;
(5) centrifugal filtration: will add sulfuric acid acidation centrifugal filtration in the concentrate, get cleaner liquid;
(6) acidifying: cleaner liquid is inserted in the retort, add benzene 20% (V/V), stir and extract, emit the sour water layer, it is standby that the way of distillation reclaims benzene;
(7) alkalize: the sour water layer adds the caustic soda alkalization, adds again in the retort, extracts for several times with chloroform, and each chloroform consumption is 20% (V/V), gets extract;
(8) change salt: chloroform is changed in 10% aqueous sulfuric acid, stir, the alkaloid salify is changed in the sour water, it is standby to reclaim chloroform, collects acid liquid promptly.
Embodiment three:
The preparation technology of sophora alapecuroides liquid, concrete processing step is as follows:
(1) pulverizes: seed and root, stem, the leaf of Sophora alopecuroide are ground into meal;
(2) moistening with adding water in the Sophora alopecuroide meal, put to seal in the container and place more than 24 hours;
(3) refluxing extraction:, in the refluxing extraction of packing into the device, add ethanol to flooding on the material face with the Sophora alopecuroide meal after moistening, close extractor, soak more than 12 hours, concentration tank is put in immersion liquid, close the return pipe valve, add ethanol in the extractor again to flooding on the material face heating, after treating that solvent begins to reflux, open solvent return pipe valve, extract continuously, extract after 8 hours, check in the extract not contain till the alkaloid that it is standby to reclaim ethanol;
(4) concentrate: extract in the concentration tank is concentrated, and it is standby to reclaim ethanol;
(5) centrifugal filtration: will add sulfuric acid acidation centrifugal filtration in the concentrate, get cleaner liquid;
(6) acidifying: cleaner liquid is inserted in the retort, add dimethylbenzene 20% (V/V), stir and extract, emit the sour water layer, it is standby that the way of distillation reclaims dimethylbenzene;
(7) alkalization: the sour water layer adds the caustic soda alkalization, adds again in the retort, and with ethyl acetate extraction for several times, each ethyl acetate consumption is 20% (V/V), gets extract;
(8) change salt: ethyl acetate is changed in 10% aqueous sulfuric acid, stir, the alkaloid salify is changed in the sour water, it is standby to reclaim ethyl acetate, collects acid liquid promptly.
Among above embodiment one, embodiment two and the embodiment three, methyl alcohol, ethanol can exchange, and sulfuric acid and hydrochloric acid can exchange.Toluene can be replaced by benzene, dimethylbenzene among the embodiment one, and the chloroform among the embodiment two can be by a kind of the substituting in dichloroethanes, chloroethanes, carrene, the carbon tetrachloride.
Claims (7)
1. the preparation technology of sophora alapecuroides liquid is characterized in that concrete processing step is as follows:
(1) pulverize: with the seed of Sophora alopecuroide or/and root, stem, leaf are ground into meal;
(2) moistening with adding water in the Sophora alopecuroide meal, put to seal in the container and place more than 24 hours;
(3) refluxing extraction:, in the refluxing extraction of packing into the device, add alcohols solvent to flooding on the material face with the Sophora alopecuroide meal after moistening, close extractor, soak more than 12 hours, concentration tank is put in immersion liquid, close the return pipe valve, add alcohols solvent in the extractor again to flooding on the material face heating, after treating that solvent begins to reflux, open solvent return pipe valve, extract continuously, extract after 8 hours, check in the extract not contain till the alkaloid that it is standby to reclaim alcohols solvent;
(4) concentrate: extract in the concentration tank is concentrated, and it is standby to reclaim alcohols solvent;
(5) centrifugal filtration: will be acidified with acid centrifugal filtration in the concentrate, get cleaner liquid;
(6) acidifying: cleaner liquid is inserted in the retort, add benzene kind solvent 20% (V/V), stir and extract, emit the sour water layer, it is standby that the way of distillation reclaims benzene kind solvent;
(7) alkalize: the sour water layer adds the alkali alkalization, adds again in the retort, and with a kind of extraction in benzene class, alkyl halide, the esters solvent for several times, each benzene class, alkyl halide, esters solvent consumption are 20% (V/V), get extract;
(8) change salt: used benzene class, alkyl halide, esters solvent are changed in 10% aqueous sulfuric acid, stir, the alkaloid salify is changed in the sour water, it is standby to reclaim benzene class, alkyl halide, esters solvent, collects acid liquid promptly.
2. the preparation technology of sophora alapecuroides liquid as claimed in claim 1 is characterized in that described alcohols solvent is methyl alcohol or ethanol.
3. the preparation technology of sophora alapecuroides liquid as claimed in claim 1 is characterized in that described benzene kind solvent is benzene, toluene or dimethylbenzene.
4. the preparation technology of sophora alapecuroides liquid as claimed in claim 1 is characterized in that the acid that is acidified with acid in the described centrifugal filtration processing step is sulfuric acid or hydrochloric acid.
5. the preparation technology of sophora alapecuroides liquid as claimed in claim 1, the alkali that it is characterized in that adding in the described alkalization process step alkali alkalization is caustic soda.
6. the preparation technology of sophora alapecuroides liquid as claimed in claim 1 is characterized in that described alkyl halide is dichloroethanes, chloroethanes, chloroform, carrene or carbon tetrachloride.
7. the preparation technology of sophora alapecuroides liquid as claimed in claim 1 is characterized in that described ester class is an ethyl acetate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00109238A CN1110339C (en) | 2000-06-19 | 2000-06-19 | Process for preparing total allooerine liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00109238A CN1110339C (en) | 2000-06-19 | 2000-06-19 | Process for preparing total allooerine liquid |
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| Publication Number | Publication Date |
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| CN1273870A CN1273870A (en) | 2000-11-22 |
| CN1110339C true CN1110339C (en) | 2003-06-04 |
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| CN00109238A Expired - Fee Related CN1110339C (en) | 2000-06-19 | 2000-06-19 | Process for preparing total allooerine liquid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102657696A (en) * | 2012-05-04 | 2012-09-12 | 宁夏紫荆花制药有限公司 | Process for extracting total alkali of sophora alopecuroide |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100441587C (en) * | 2001-02-10 | 2008-12-10 | 宁夏博尔泰力药业股份有限公司 | Process for preparing general alooerine |
| CN101837044A (en) * | 2010-06-23 | 2010-09-22 | 邱宏亮 | Extraction method of wild herba Sophora alopecuroide and oral medicinal composition |
| CN110025660A (en) * | 2019-04-23 | 2019-07-19 | 中南民族大学 | Application of the sophora alopecuroides extract in the drug that preparation is used for diastole airway smooth muscle |
| CN117018057A (en) * | 2023-08-01 | 2023-11-10 | 新疆维吾尔自治区阿克苏职业技术学院 | An extraction method and composition of sophora sophora alkaloids |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1089846A (en) * | 1993-01-18 | 1994-07-27 | 江西中医学院 | A kind of anticancer drug and preparation method thereof |
| CN1180074A (en) * | 1997-02-18 | 1998-04-29 | 山东农业大学 | Extraction of sophora alopecuroides extract and its composition |
-
2000
- 2000-06-19 CN CN00109238A patent/CN1110339C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1089846A (en) * | 1993-01-18 | 1994-07-27 | 江西中医学院 | A kind of anticancer drug and preparation method thereof |
| CN1180074A (en) * | 1997-02-18 | 1998-04-29 | 山东农业大学 | Extraction of sophora alopecuroides extract and its composition |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102657696A (en) * | 2012-05-04 | 2012-09-12 | 宁夏紫荆花制药有限公司 | Process for extracting total alkali of sophora alopecuroide |
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