CN1456548A - Process for extracting leonuridine from fresh motherwort and leonuridine preparation - Google Patents
Process for extracting leonuridine from fresh motherwort and leonuridine preparation Download PDFInfo
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- CN1456548A CN1456548A CN 03118828 CN03118828A CN1456548A CN 1456548 A CN1456548 A CN 1456548A CN 03118828 CN03118828 CN 03118828 CN 03118828 A CN03118828 A CN 03118828A CN 1456548 A CN1456548 A CN 1456548A
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- 235000000604 Chrysanthemum parthenium Nutrition 0.000 title claims abstract description 64
- 235000000802 Leonurus cardiaca ssp. villosus Nutrition 0.000 title claims abstract description 64
- 241000207925 Leonurus Species 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title claims description 24
- VELYAQRXBJLJAK-MJSCJBMMSA-N Leonuridine Chemical compound C12C(C)(O)CC(O)C2C=COC1O[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O VELYAQRXBJLJAK-MJSCJBMMSA-N 0.000 title 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 98
- 235000011389 fruit/vegetable juice Nutrition 0.000 claims abstract description 43
- 238000001035 drying Methods 0.000 claims abstract description 17
- 238000002347 injection Methods 0.000 claims abstract description 16
- 239000007924 injection Substances 0.000 claims abstract description 16
- 239000002775 capsule Substances 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 58
- 240000007890 Leonurus cardiaca Species 0.000 claims description 46
- 239000003513 alkali Substances 0.000 claims description 46
- 238000005516 engineering process Methods 0.000 claims description 43
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 34
- 238000000605 extraction Methods 0.000 claims description 27
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 26
- 239000000706 filtrate Substances 0.000 claims description 25
- 239000011347 resin Substances 0.000 claims description 23
- 229920005989 resin Polymers 0.000 claims description 23
- 239000000284 extract Substances 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 17
- 239000012141 concentrate Substances 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 14
- 229930013930 alkaloid Natural products 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 12
- 238000004064 recycling Methods 0.000 claims description 12
- 150000003797 alkaloid derivatives Chemical class 0.000 claims description 11
- DUNMULOWUUIQIL-RGMNGODLSA-N (2s)-1,1-dimethylpyrrolidin-1-ium-2-carboxylic acid;chloride Chemical compound Cl.C[N+]1(C)CCC[C@H]1C([O-])=O DUNMULOWUUIQIL-RGMNGODLSA-N 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 10
- 238000010009 beating Methods 0.000 claims description 9
- 238000010828 elution Methods 0.000 claims description 9
- 238000013467 fragmentation Methods 0.000 claims description 9
- 238000006062 fragmentation reaction Methods 0.000 claims description 9
- 239000012535 impurity Substances 0.000 claims description 9
- 238000001556 precipitation Methods 0.000 claims description 9
- 239000002893 slag Substances 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 150000001768 cations Chemical class 0.000 claims description 6
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 5
- 230000002378 acidificating effect Effects 0.000 claims description 5
- 150000001298 alcohols Chemical class 0.000 claims description 5
- 239000003729 cation exchange resin Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 229920001353 Dextrin Polymers 0.000 claims description 4
- 239000004375 Dextrin Substances 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 claims description 4
- 229920002472 Starch Polymers 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 235000019425 dextrin Nutrition 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 229910001415 sodium ion Inorganic materials 0.000 claims description 4
- 239000008107 starch Substances 0.000 claims description 4
- 235000019698 starch Nutrition 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000000741 silica gel Substances 0.000 claims description 3
- 229910002027 silica gel Inorganic materials 0.000 claims description 3
- 229920000168 Microcrystalline cellulose Polymers 0.000 claims description 2
- 229920003081 Povidone K 30 Polymers 0.000 claims description 2
- 230000000274 adsorptive effect Effects 0.000 claims description 2
- 230000001476 alcoholic effect Effects 0.000 claims description 2
- 238000009835 boiling Methods 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- 239000003153 chemical reaction reagent Substances 0.000 claims description 2
- 238000004587 chromatography analysis Methods 0.000 claims description 2
- 230000006837 decompression Effects 0.000 claims description 2
- AZHSSKPUVBVXLK-UHFFFAOYSA-N ethane-1,1-diol Chemical compound CC(O)O AZHSSKPUVBVXLK-UHFFFAOYSA-N 0.000 claims description 2
- 230000002496 gastric effect Effects 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims description 2
- 229940031703 low substituted hydroxypropyl cellulose Drugs 0.000 claims description 2
- 235000019813 microcrystalline cellulose Nutrition 0.000 claims description 2
- 239000008108 microcrystalline cellulose Substances 0.000 claims description 2
- 229940016286 microcrystalline cellulose Drugs 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 238000012856 packing Methods 0.000 claims description 2
- 238000005325 percolation Methods 0.000 claims description 2
- 239000001253 polyvinylpolypyrrolidone Substances 0.000 claims description 2
- 235000013809 polyvinylpolypyrrolidone Nutrition 0.000 claims description 2
- 229920000523 polyvinylpolypyrrolidone Polymers 0.000 claims description 2
- 238000011084 recovery Methods 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 235000014347 soups Nutrition 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 230000001954 sterilising effect Effects 0.000 claims description 2
- 238000004659 sterilization and disinfection Methods 0.000 claims description 2
- 239000010409 thin film Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims 2
- 239000003595 mist Substances 0.000 claims 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims 1
- 235000012239 silicon dioxide Nutrition 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 4
- 239000003826 tablet Substances 0.000 abstract description 4
- WNGSUWLDMZFYNZ-UHFFFAOYSA-N Leonurine Chemical compound COC1=CC(C(=O)OCCCCN=C(N)N)=CC(OC)=C1O WNGSUWLDMZFYNZ-UHFFFAOYSA-N 0.000 abstract 4
- 238000000151 deposition Methods 0.000 abstract 1
- 230000008901 benefit Effects 0.000 description 3
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- 206010030113 Oedema Diseases 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 206010013935 Dysmenorrhoea Diseases 0.000 description 1
- 208000019255 Menstrual disease Diseases 0.000 description 1
- 206010030302 Oliguria Diseases 0.000 description 1
- 241000590428 Panacea Species 0.000 description 1
- 235000019658 bitter taste Nutrition 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
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- 238000007907 direct compression Methods 0.000 description 1
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- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
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- 201000008383 nephritis Diseases 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
Abstract
A process for extracting leonurine from fresh motherwort includes such steps as extracting juice, depositing in alcohol, filtering, column exchanging, eluting, concentrating and drying. Said leonurine can be made into capsule, tablet, or injection for treating gynopathy with hige curative effect.
Description
Technical field
The present invention relates to a kind of extraction process and preparation thereof of Chinese medicine, especially relate to a kind of extraction process and preparation thereof of fresh Herba Leonuri total alkali.
Background technology
Motherwort Herb is a labiate, and Shennong's Herbal is classified as top grade, and the successive dynasties book on Chinese herbal medicine all records, and is traditional gynaecology's good medicine.Clinical application is extensive, be used for menoxenia, dysmenorrhoea, through close, lochiorrhea; The oedema oliguria, diseases such as acute nephritis edema.
" Chinese pharmacopoeia 2000 editions has been recorded Motherwort Herb dry product and two kinds of bright product.Bright product seedling in spring phase to first summer flower is tapped in earlier stage; Dry product cauline leaf in summer is luxuriant, Hua Weikai or tap when just opening, dry, and contained alkaloidal stachydrine hydrochloride meter, dry product must not be less than 0.4%; Bright product must not be less than 1.0%, studies show that Motherwort Herb is a kind of not sun-proof, not long keeping Chinese medicine, and Motherwort Herb its effective active composition alkaloids content after shining dry-storage significantly descends.Fresh Herba Leonuri more dried Motherwort Herb on effective active component content, curative effect has significant advantage.Bright benefit is female to be raw material extraction Motherwort Herb total alkali so the present invention adopts, the Motherwort Herb total alkali active constituent content height of gained, and dose is little, and good effect, and technology simplifies is greatly produced more conveniently, has great realistic meaning and promotional value.
Motherwort Herb is gynaecology's panacea, determined curative effect, be widely used, clinical used preparation variety is numerous, as Herba Leonuri paste, the Motherwort Herb oral liquid, YIMUCAO PIAN etc., general water is carried or aqueous extraction-alcohol precipitation technology all has preparation not refining but be, bitter, consumption is big, the unsettled shortcoming of drug effect, and the motherwort total alkali preparation comprises Motherwort Herb total alkali capsule, Motherwort Herb total alkali sheet, Motherwort Herb total alkali injection liquid, success overcome above-mentioned deficiency, it is refining to have preparation, no bitter taste, and consumption is little, advantages such as efficacy stability, therefore easier have vast market prospect for people accept, and is the ideal product of modern pharmaceutical enterprise.
Summary of the invention
1, the present invention extracts the Motherwort Herb total alkali and is achieved by the following technical solution from fresh Herba Leonuri.
Technology one, fresh Herba Leonuri is cleaned, remove impurity and clean, it is standby to be up to the standards; Get the fresh Herba Leonuri fragmentation, making beating is squeezed the juice, get juice, slag adds the suitable quantity of water mixing squeezes the juice 2-3 time repeatedly, merge juice, under agitation add ethanol and make and contain the alcohol amount and be 40-80%, leave standstill, filter, get filtrate recycling ethanol, transfer pH to 2-3 with hydrochloric acid, filter, acidic cation-exchange resin post on the filtrate, exchange back resin washes with water to water elution liquid pH6-7, discard, continue to be eluted to the alkaloid extraction fully with the ammoniacal liquor of 5-20% acid or 5-20%.Collect elutriant, transfer pH6-7, filter, filtrate concentrates, drying, and dry product uses the extraction using alcohol alkaloid to fully, filters, and behind the filtrate recycling ethanol, concentrates, and drying gets Motherwort Herb total alkali extract.
Technology two, fresh Herba Leonuri is cleaned, remove impurity and clean, it is standby to be up to the standards; Get the fresh Herba Leonuri fragmentation, making beating is squeezed the juice, get juice, slag adds the suitable quantity of water mixing squeezes the juice, and 2-3 time repeatedly, merges juice, under agitation adding ethanol makes the alcohol amount of containing be 40-80%, leave standstill, filter, get filtrate recycling ethanol, transfer pH to 2-3 with hydrochloric acid, filter, acidic cation-exchange resin post on the filtrate, exchange back resin washes with water to water elution liquid pH6-7, discard, continuation is eluted to alkaloid with ammonia alcohol (adding ammoniacal liquor to pH value 9-10 in ethanol) and extracts fully, collects elutriant, behind the recovery ethanol, concentrate drying gets Motherwort Herb total alkali extract.
Technology three, fresh Herba Leonuri is cleaned, remove impurity and clean, it is standby to be up to the standards; Get the fresh Herba Leonuri fragmentation, making beating is squeezed the juice, and gets juice, slag adds the suitable quantity of water mixing squeezes the juice, and 2-3 time repeatedly, merge juice, under agitation add ethanol and make and contain the alcohol amount and be 40-80%, leave standstill, filter, behind the filtrate recycling ethanol, transfer to certain pH value, filter macroporous adsorptive resins on the filtrate, behind distilled water flush away impurity, with certain density ethanol elution, collection elutriant, after elutriant reclaims ethanol, concentrate, drying gets Motherwort Herb total alkali extract.
1,1 technology one, the two i.e. processing of 732 type Zeo-karbs of middle strong acidity 001 * 7 of the present invention can be adopted following any method:
1.1.1 new resin cation (R.C.) fully expands it with distilled water immersion 1-2 days, wash with water to elutant clear and bright colourless till, surplus water is removed, add 2-5 and doubly measure 1-2mol/l hydrochloric acid, constantly stir, soaked 1-3 hour, remove acid solution, wash with water till the elutant pH3-4, incline and remove surplus water.Add 2-5 and doubly measure 1-2mol/lNaOH solution, constantly stir, soaked about 1-3 hour, remove alkali lye, wash with water to elutant pH7 again, Yu Shui inclines.Add 2-5 at last and doubly measured the 1-2mol/lHCl solution soaking 1-3 hour, make resin cation (R.C.) transfer the H type to, the disacidify liquid that inclines, wash with water to pH be 3-5, can adorn post and use.
1.1.2 new resin cation (R.C.) was immersed in the distilled water 1-2 days, make its fully expand wash with water to elutant clear and bright colourless till, in the chromatography column of packing into.Earlier with resin volume 10-20 1-2mol/l hydrochloric acid doubly, exchange with the flow velocity of every square centimeter of 1ml of per minute, make it become Hydrogen, wash with water then to effluent liquid and be neutral.Then the 1-2mol/l sodium hydroxide of doubly measuring with resin volume 5-15 again (or sodium-chlor) exchanges, and makes it reply the sodium type, washes with water to elutant not contain sodium ion (inspect with flame method, if there is sodium ion to exist, flame is yellow during calcination) again.Repeat the processing of hydrochloric acid and sodium hydroxide (or sodium-chlor) again.The 1-2mol/l hydrochloric acid of doubly measuring with resin volume 5-15 exchanges at last, makes it become Hydrogen, is washed to pH3-5 and can supplies usefulness.
The used water of aforesaid operations is distilled water.
1.2 raw materials used among the present invention is fresh Herba Leonuri.
1.3 fresh Herba Leonuri extraction gained juice can directly add the ethanol alcohol precipitation in the technology of the present invention, adds the alcoholic acid alcohol precipitation again after also can suitably concentrating.
1.4 the alcohol concn of alcohol precipitation is 40-80% in the technology of the present invention.
1.5 whether fully available alkaloid extraction alkaloid precipitation reagent detect in the technology of the present invention.
1.6 filter this step also available centrifugal replacement in the technology of the present invention.
1.7 the fresh Herba Leonuri juice extracting method is in the technology of the present invention: get the fresh Herba Leonuri fragmentation, making beating is squeezed the juice, and gets juice, and slag adds the suitable quantity of water mixing squeezes the juice, 2-3 time repeatedly, merge juice, and also can be that fresh Herba Leonuri is got juice through broken boiling.
1.8 in the technology of the present invention, dry drying under reduced pressure or the spraying drying of adopting.
Adopt decompression or thin film concentration 1.9 concentrate in the technology of the present invention.
1.10 in the technology one of the present invention, exchange back resin can adopt the acetic acid of 5%-20%, the sulfuric acid of 5%-20%, perhaps the sodium hydroxide wash-out of the ammoniacal liquor 2%-10% of 5%-20%.
1.11 in the technology one of the present invention, the gained dry product extremely fully can be by adding 3-8 times of 70-95% alcohol reflux 2-3 time with 95% extraction using alcohol alkaloid, each 1-3 hour, or dress post 70-95% ethanol percolation wash-out, or employing adds the ultrasonic wash-out 2 inferior methods realizations of 70-95% ethanol, best for 95% alcohol reflux 2 times, each 2 hours.
1.12 with the pure wash-out alkaloid of ammonia, also can adopt NaOH ethanolic soln (with NaOH liquid adjust pH 9-10) to be elutriant in the technology two of the present invention, elutriant filters with HCL adjust pH 6-7, behind the filtrate recycling ethanol, concentrate drying gets Motherwort Herb total alkali extract.
1.13 exchange back resin washes with water to water elution liquid pH value 6-7 in the technology one, two of the present invention, can continue with after the washing with alcohol, uses acid or basic solvent wash-out again.
1.14 in the technology three of the present invention, be elutriant with certain density ethanol, alcohol concn can be any among the 30-90%, best concentration of ethanol is about 50%.
To transfer to certain pH value can be any among the 3-7 1.15 reclaim soup behind the ethanol in the technology three of the present invention, and optimal ph is 5-6.
2, the preparation of motherwort total alkali preparation of the present invention is achieved by the following technical solution:
2.1 the capsular preparation of Motherwort Herb total alkali:
2.1.1 the capsular prescription of Motherwort Herb total alkali is formed:
Motherwort total alkaline extraction thing (in stachydrine hydrochloride) 10-60g
Right amount of auxiliary materials is made 1000.
Optimum formula is formed:
Motherwort total alkaline extraction thing (in stachydrine hydrochloride) 20g
Right amount of auxiliary materials is made 1000.
2.1.2 the capsular preparation technology of Motherwort Herb total alkali: get motherwort total alkaline extraction thing and pulverize, add right amount of auxiliary materials, mixing, the encapsulated Motherwort Herb total alkali capsule that promptly gets.
2.1.3 used auxiliary material can be any or multiple mixing use in dextrin, starch, the micropowder silica gel etc. in the technology of the present invention.
2.2 the preparation of Motherwort Herb total alkali sheet:
2.2.1 the prescription of Motherwort Herb total alkali sheet is formed:
Motherwort total alkaline extraction thing (in stachydrine hydrochloride) 10-60g
Right amount of auxiliary materials is made 1000.
Optimum formula is formed:
Motherwort total alkaline extraction thing (in stachydrine hydrochloride) 20g
Right amount of auxiliary materials is made 1000.
2.2.2 the preparation technology of Motherwort Herb total alkali sheet:
Get motherwort total alkaline extraction thing and pulverize, add right amount of auxiliary materials, mixing, direct compression or granulation, dry back compressing tablet, dressing, quality inspection promptly gets Motherwort Herb total alkali sheet.
2.2.3 by the made coating tablet of technology, be film coated tablet, its film-coat material adopts gastric soluable film-coat pre-mixture (Opadry).
2.2.4 added auxiliary material can be among the present invention: any or multiple mixing in Microcrystalline Cellulose, polyvinylpolypyrrolidone, carboxymethylstach sodium, 30 POVIDONE K 30 BP/USP 30, low-substituted hydroxypropyl cellulose, starch, dextrin, the micropowder silica gel etc. is used.
2.3 the preparation of Motherwort Herb total alkali injection liquid:
2.3.1 Motherwort Herb total alkali injection formula is formed:
Motherwort total alkaline extraction thing (in stachydrine hydrochloride) 5-30g
It is an amount of to add the injection water, makes 1000ml.
Optimum formula is: motherwort total alkaline extraction thing (in stachydrine hydrochloride) 15g
It is an amount of to add the injection water, makes 1000ml.
2.3.2 preparation technology:
Get motherwort total alkaline extraction thing, add the injection water and dissolve in right amount, regulate the pH value, filter, filtrate adds the injection water to the specified amount embedding, and sterilization promptly gets Motherwort Herb total alkali injection liquid.
2.3.3 filtrate adds the injection water to the specified amount embedding, can add proper amount of active carbon and stir evenly, and after the filtration, adds the injection water again to specified amount, embedding.
Embodiment
The optimum implementation of this invention is that fresh Herba Leonuri is cleaned, and removes impurity and cleans, and it is standby to be up to the standards; Get the fresh Herba Leonuri fragmentation, making beating is squeezed the juice, get juice, slag adds the suitable quantity of water mixing squeezes the juice 2-3 time repeatedly, merge juice, under agitation add ethanol and make and contain the alcohol amount and be 40-80%, leave standstill, filter, get filtrate recycling ethanol, transfer pH to 2-3 with hydrochloric acid, filter, acidic cation-exchange resin post on the filtrate, exchange back resin washes with water to water elution liquid pH6-7, discard, continue to be eluted to the alkaloid extraction fully with the ammoniacal liquor of 5-20% acid or 5-20%.Collect elutriant, transfer pH6-7, filter, filtrate concentrates, drying, dry product, filters, behind the filtrate recycling ethanol to fully with the extraction using alcohol alkaloid, concentrate, drying gets Motherwort Herb total alkali extract, again extract is made capsule, tablet, injection by the requirement of different dosage form batching.
Claims (4)
1, a kind of fresh Herba Leonuri extracts Motherwort Herb total alkali technology and motherwort total alkali preparation, it is characterized in that comprising following technical scheme and realizes:
(1) fresh Herba Leonuri is cleaned, remove impurity and clean, it is standby to be up to the standards; Get the fresh Herba Leonuri fragmentation, making beating is squeezed the juice, get juice, slag adds the suitable quantity of water mixing squeezes the juice 2-3 time repeatedly, merge juice, under agitation add ethanol and make and contain the alcohol amount and be 40-80%, leave standstill, filter, get filtrate recycling ethanol, transfer pH to 2-3 with hydrochloric acid, filter, acidic cation-exchange resin post on the filtrate, exchange back resin washes with water to water elution liquid pH6-7, discard, continue to be eluted to the alkaloid extraction fully with the ammoniacal liquor of 5-20% acid or 5-20%.Collect elutriant, transfer pH6-7, filter, filtrate concentrates, drying, and dry product uses the extraction using alcohol alkaloid to fully, filters, and behind the filtrate recycling ethanol, concentrates, and drying gets Motherwort Herb total alkali extract.
(2) fresh Herba Leonuri is cleaned, remove impurity and clean, it is standby to be up to the standards; Get the fresh Herba Leonuri fragmentation, making beating is squeezed the juice, get juice, slag adds the suitable quantity of water mixing squeezes the juice, and 2-3 time repeatedly, merges juice, under agitation adding ethanol makes the alcohol amount of containing be 40-80%, leave standstill, filter, get filtrate recycling ethanol, transfer pH to 2-3 with hydrochloric acid, filter, acidic cation-exchange resin post on the filtrate, exchange back resin washes with water to water elution liquid pH6-7, discard, continuation is eluted to alkaloid with ammonia alcohol (adding ammoniacal liquor to pH value 9-10 in ethanol) and extracts fully, collects elutriant, behind the recovery ethanol, concentrate drying gets Motherwort Herb total alkali extract.
(3) fresh Herba Leonuri is cleaned, remove impurity and clean, it is standby to be up to the standards; Get the fresh Herba Leonuri fragmentation, making beating is squeezed the juice, and gets juice, slag adds the suitable quantity of water mixing squeezes the juice, and 2-3 time repeatedly, merge juice, under agitation add ethanol and make and contain the alcohol amount and be 40-80%, leave standstill, filter, behind the filtrate recycling ethanol, transfer to certain pH value, filter macroporous adsorptive resins on the filtrate, behind distilled water flush away impurity, with certain density ethanol elution, collection elutriant, after elutriant reclaims ethanol, concentrate, drying gets Motherwort Herb total alkali extract.
2, fresh Herba Leonuri according to claim 1 extracts Motherwort Herb total alkali technology and motherwort total alkali preparation, it is characterized in that the i.e. processing of 732 type Zeo-karbs of strongly-acid 001 * 7 can adopt following any method:
(1) new resin cation (R.C.) fully expands it with distilled water immersion 1-2 days, wash with water to elutant clear and bright colourless till, surplus water is removed, add 2-5 and doubly measure 1-2mol/l hydrochloric acid, constantly stir, soaked 1-3 hour, remove acid solution, wash with water till the elutant pH3-4, incline and remove surplus water, add 2-5 and doubly measure 1-2mol/lNaOH solution, constantly stir, soaked about 1-3 hour, and removed alkali lye, wash with water again to elutant pH7, Yu Shui inclines, add 2-5 at last and doubly measured the 1-2mol/lHCl solution soaking 1-3 hour, make resin cation (R.C.) transfer the H type to, disacidify liquid inclines, wash with water to pH be 3-5, can adorn post and use.
(2) new resin cation (R.C.) is immersed in the distilled water 1-2 days, make its fully expand wash with water to elutant clear and bright colourless till, pack in the chromatography column, earlier with resin volume 10-20 1-2mol/l hydrochloric acid doubly, flow velocity with every cubic centimetre of 1ml of per minute exchanges, make it become Hydrogen, wash with water then to effluent liquid and be neutral, then the 1-2mol/l sodium hydroxide of doubly measuring with resin volume 5-15 again (or sodium-chlor) exchanges, make it reply the sodium type, wash with water again to elutant and do not contain sodium ion (inspect with flame method, if there is sodium ion to exist, flame is yellow during calcination), repeat the processing of hydrochloric acid and sodium hydroxide (or sodium-chlor) again, the 1-2mol/l hydrochloric acid of doubly measuring with resin volume 5-15 exchanges at last, makes it become Hydrogen, is washed to pH3-5 and can supplies usefulness.
3, fresh Herba Leonuri according to claim 1 extracts Motherwort Herb total alkali technology and motherwort total alkali preparation, it is characterized in that:
(1) fresh Herba Leonuri extraction gained juice can directly add the ethanol alcohol precipitation in the technology of the present invention, adds the alcoholic acid alcohol precipitation again after also can suitably concentrating.
(2) alcohol concn of alcohol precipitation is 40-80% in the technology of the present invention.
(3) whether fully available alkaloid extraction alkaloid precipitation reagent detect in the technology of the present invention.
(4) filter this step also available centrifugal replacement in the technology of the present invention.
(5) the fresh Herba Leonuri juice extracting method is in the technology of the present invention: get the fresh Herba Leonuri fragmentation, making beating is squeezed the juice, and gets juice, and slag adds the suitable quantity of water mixing squeezes the juice, and 2-3 time repeatedly, merge juice, also can be that fresh Herba Leonuri is got juice through broken boiling.
(6) in the technology of the present invention, the dry drying under reduced pressure/spraying drying that adopts.
(7) concentrate employing decompression/thin film concentration in the technology of the present invention.
(8) in the technology of the present invention, exchange back resin can adopt the acetic acid of 5%-20%, the sulfuric acid of 5%-20%, the sodium hydroxide wash-out of the ammoniacal liquor 2%-10% of/5%-20%.
(9) in the technology of the present invention, the gained dry product extremely fully can be by adding 3-8 times of 70-95% alcohol reflux 2-3 time with 95% extraction using alcohol alkaloid, each 1-3 hour, / dress post 70-95% ethanol percolation wash-out, / adopt to add the ultrasonic wash-out 2 inferior methods realizations of 70-95% ethanol, best for 95% alcohol reflux 2 times, each 2 hours.
(10) use the pure wash-out alkaloid of ammonia in the technology of the present invention, also can adopt NaOH ethanolic soln (with NaOH liquid adjust pH 9-10) to be elutriant, elutriant HCL adjust pH 6-7, filtration, behind the filtrate recycling ethanol, concentrate drying gets Motherwort Herb total alkali extract.
(11) exchange back resin washes with water to water elution liquid pH value 6-7 in the technology of the present invention, can continue with after the washing with alcohol, uses acid/basic solvent wash-out again.
(12) in the technology of the present invention, be elutriant with certain density ethanol, alcohol concn can be any among the 30-90%, and best concentration of ethanol is about 50%.
(13) reclaiming soup behind the ethanol in the technology of the present invention, to transfer to certain pH value can be any among the 3-7, and optimal ph is 5-6.
4, fresh Herba Leonuri according to claim 1 extracts motherwort total area alkali technology and motherwort total alkali preparation, it is characterized in that the motherwort total alkali preparation also can be achieved through the following technical solutions:
(1) Motherwort Herb total alkali capsule preparation: get motherwort total alkaline extraction thing (in stachydrine hydrochloride) 10-60g, the best is 20g, through pulverizing, add auxiliary materials and mixing, adorn 1000 capsules, auxiliary material wherein can be that any/multiple mixing in dextrin, starch, the micro mist silicic acid is used.
(2) preparation of Motherwort Herb total alkali sheet: get motherwort total alkaline extraction thing (in stachydrine hydrochloride) 10-60g, the best is 20g, through pulverizing, add auxiliary material, mixing, compressing tablet, packing and make 1000, auxiliary material wherein is that any/multiple mixing in Microcrystalline Cellulose, polyvinylpolypyrrolidone, carboxymethylstach sodium, 30 POVIDONE K 30 BP/USP 30, low-substituted hydroxypropyl cellulose, starch, dextrin, the micropowder silica gel etc. is used, and the film-coat material adopts the gastric soluable film-coat to give the mixture Opadry.
(3) motherwort total alkaline extraction thing (in stachydrine hydrochloride) 5-30g is got in the preparation of Motherwort Herb total alkali injection, and best 15g adds the injection water and dissolves in right amount, regulate pH value, filtration, filtrate adds the injection water to the specified amount embedding, and sterilization gets 1000ml Motherwort Herb total alkali injection liquid.
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| CNB031188281A CN100484915C (en) | 2003-03-21 | 2003-03-21 | Process for extracting leonuridine from fresh motherwort and leonuridine preparation |
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| CNB031188281A CN100484915C (en) | 2003-03-21 | 2003-03-21 | Process for extracting leonuridine from fresh motherwort and leonuridine preparation |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101244121B (en) * | 2007-02-15 | 2010-12-22 | 多菲制药(中国)有限公司 | Leonurus heterophyllus total alkaloid extract and preparation thereof |
| CN105412225A (en) * | 2015-12-11 | 2016-03-23 | 苏州泽达兴邦医药科技有限公司 | Liquid discharging method of round bottom alcohol precipitation tank in motherwort alcohol precipitation process |
| CN107006651A (en) * | 2017-04-15 | 2017-08-04 | 申翰昭 | The preparation method of ball formula eight delicacies with motherwort life-nourishing tea bag and its health preserving tea of preparation |
| CN108567958A (en) * | 2018-07-25 | 2018-09-25 | 杭州光启医疗科技发展有限公司 | A kind of pharmaceutical composition and preparation method thereof for treating gynaecological imflammation |
| CN113490419A (en) * | 2018-12-21 | 2021-10-08 | 利摩日大学 | Bioactive substances, method for producing same, and use thereof as biological tissue protective agents |
-
2003
- 2003-03-21 CN CNB031188281A patent/CN100484915C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101244121B (en) * | 2007-02-15 | 2010-12-22 | 多菲制药(中国)有限公司 | Leonurus heterophyllus total alkaloid extract and preparation thereof |
| CN105412225A (en) * | 2015-12-11 | 2016-03-23 | 苏州泽达兴邦医药科技有限公司 | Liquid discharging method of round bottom alcohol precipitation tank in motherwort alcohol precipitation process |
| CN107006651A (en) * | 2017-04-15 | 2017-08-04 | 申翰昭 | The preparation method of ball formula eight delicacies with motherwort life-nourishing tea bag and its health preserving tea of preparation |
| CN108567958A (en) * | 2018-07-25 | 2018-09-25 | 杭州光启医疗科技发展有限公司 | A kind of pharmaceutical composition and preparation method thereof for treating gynaecological imflammation |
| CN113490419A (en) * | 2018-12-21 | 2021-10-08 | 利摩日大学 | Bioactive substances, method for producing same, and use thereof as biological tissue protective agents |
| CN113490419B (en) * | 2018-12-21 | 2023-06-23 | 利摩日大学 | Bioactive substance, method for producing same, and use of same as biological tissue protective agent |
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| Publication number | Publication date |
|---|---|
| CN100484915C (en) | 2009-05-06 |
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