CN1785308A - Extraction technology of plant total alkaloid extract having anti tumour action and its preparation - Google Patents
Extraction technology of plant total alkaloid extract having anti tumour action and its preparation Download PDFInfo
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- 150000003797 alkaloid derivatives Chemical class 0.000 title claims abstract description 12
- 239000000284 extract Substances 0.000 title claims description 42
- 238000000605 extraction Methods 0.000 title claims description 37
- 238000002360 preparation method Methods 0.000 title claims description 17
- 230000000259 anti-tumor effect Effects 0.000 title claims description 11
- 239000003814 drug Substances 0.000 claims abstract description 12
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- 239000000243 solution Substances 0.000 claims description 101
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 66
- 239000002253 acid Substances 0.000 claims description 55
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- 238000001556 precipitation Methods 0.000 claims description 37
- 239000002244 precipitate Substances 0.000 claims description 30
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 20
- 239000003480 eluent Substances 0.000 claims description 20
- 238000004321 preservation Methods 0.000 claims description 17
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- MBWUSSKCCUMJHO-DVDUUUGDSA-N Solamargine Natural products O([C@@H]1[C@@H](O)[C@@H](O[C@H]2[C@H](O)[C@H](O)[C@@H](O)[C@H](C)O2)[C@H](CO)O[C@@H]1O[C@@H]1CC=2[C@@](C)([C@@H]3[C@H]([C@H]4[C@@](C)([C@H]5[C@@H](C)[C@@]6(O[C@H]5C4)NC[C@H](C)CC6)CC3)CC=2)CC1)[C@H]1[C@H](O)[C@H](O)[C@@H](O)[C@@H](C)O1 MBWUSSKCCUMJHO-DVDUUUGDSA-N 0.000 description 2
- 241000207763 Solanum Species 0.000 description 2
- KNLOWJPFLKGYGQ-UHFFFAOYSA-N Solasodine 3-O-??-L-rhamnopyranosyl (1‘Â∆2)-O-[??-D-glucopyranosyl (1‘Â∆4)]-??-D-glucopyranoside Natural products O1C2(NCC(C)CC2)C(C)C(C2(CCC3C4(C)CC5)C)C1CC2C3CC=C4CC5OC(C(C1O)OC2C(C(O)C(O)C(C)O2)O)OC(CO)C1OC1OC(CO)C(O)C(O)C1O KNLOWJPFLKGYGQ-UHFFFAOYSA-N 0.000 description 2
- QCTMYNGDIBTNSK-QCNFCIKQSA-N Solasonine Natural products O([C@@H]1[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@@H](O)[C@H](C)O2)[C@@H](O[C@@H]2CC=3[C@@](C)([C@@H]4[C@H]([C@H]5[C@@](C)([C@H]6[C@@H](C)[C@@]7(O[C@H]6C5)NC[C@H](C)CC7)CC4)CC=3)CC2)O[C@@H](CO)[C@@H]1O)[C@H]1[C@@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 QCTMYNGDIBTNSK-QCNFCIKQSA-N 0.000 description 2
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- NWMIYTWHUDFRPL-UHFFFAOYSA-N sapogenin Natural products COC(=O)C1(CO)C(O)CCC2(C)C1CCC3(C)C2CC=C4C5C(C)(O)C(C)CCC5(CCC34C)C(=O)O NWMIYTWHUDFRPL-UHFFFAOYSA-N 0.000 description 1
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- KWVISVAMQJWJSZ-UHFFFAOYSA-N solasodine Chemical compound CC1C(C2(CCC3C4(C)CCC(O)CC4=CCC3C2C2)C)C2OC11CCC(C)CN1 KWVISVAMQJWJSZ-UHFFFAOYSA-N 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
Abstract
A common alkaloid extracted from plant and with antineoplastic function, its extracting process and the medicine prepared from it are disclosed.
Description
Technical field
The present invention relates to a kind of method of extracting effective site from herbal raw material, particularly a kind of extraction process with plant total alkaloid extract of antitumor action the invention still further relates to its preparation.
Background technology
Herba Solani Nigri belongs to the Solanaceae Solanum, one to several years this plant of SHENGCAO, cold, bitter in the mouth, little sweet, have mild toxicity, return lung, stomach, urinary bladder channel, the effect of heat-clearing and toxic substances removing, promoting blood circulation to remove blood stasis, inducing diuresis to remove edema, eliminating phlegm and stopping cough is arranged, all there is distribution all parts of the country.In China 5 different shape types are arranged, yellow fruit Herba Solani Nigri, purple stem Herba Solani Nigri, green stem Herba Solani Nigri, green arteries and veins spend Herba Solani Nigri, brown arteries and veins to spend Herba Solani Nigri less less, at present main what study is the wild Herba Solani Nigri of northern China (SolanumnigrumL.), but belongs to purple stem Herba Solani Nigri. the Herba Solani Nigri all herbal medicine.
Herb of Herba Solani Nigri contains the glycoside steroid alkaloid, Herba Solani Nigri polysaccharide, mineral, vitamin, pigment, aminoacid etc., also contain ester, carboxyl compound, sterol, phenoloid (its main component is yellow beta-unsaturated esters) in the extract of Herba Solani Nigri berry, contain saponin and sapogenin in addition, and the chemistry that plays a crucial role is mainly alkaloid, is polysaccharide secondly.Report Herba Solani Nigri total alkaloids such as Liu Ying comprise solasonine, solamargine and B-solamargine, and Li Xiuxia etc. think that containing solamargine, solasonine, solancarpine and eggplant reaches alkali.
Chinese scholars studies confirm that Herba Solani Nigri extract has antitumor action, antibacterial and antivirus action, neuropharmacology effect, cardiovascular pharmacological effect, the effect of digestive system pharmacology, urinary system pharmacological action, genetic toxicity effect, endocrine pharmacological action, the effect of antipyretic-antalgic pharmacology and some other pharmacological action.Its equal plant Australian eggplant (Solanum abiculareparst), Fructus solani xanthocarpi (Solanum xanthocar pum Schrad, et wendl) all contain similar composition, have similar pharmacological action.Now, can remove impurity fully, further promote its pharmacological action, then become the another emphasis of research by which kind of extraction process.
Summary of the invention
Technical problem to be solved by this invention is at the deficiencies in the prior art, provide a kind of make the extract impurity content few, and can promote the extraction process of the plant total alkaloid extract with antitumor action of its pharmacological action.
The present invention also provides said extracted technology extract obtained preparation.
Technical problem to be solved by this invention is to realize by following technical scheme.The present invention is a kind of extraction process with plant total alkaloid extract of antitumor action, is characterized in, its step is as follows,
(1) get herb of Herba Solani Nigri and fruit, perhaps Fructus solani xanthocarpi, perhaps Australian eggplant adds alcoholic solution and extracts, and reclaims ethanol, concentrate, concentrated solution; Concentrated solution transfers pH value to alkalescence with alkaline solution, and cold preservation is left standstill, the centrifuging and taking precipitate; Perhaps add acid solution in the concentrated solution, fully stir, leave standstill, centrifugal, get acid supernatant;
(2) precipitate washing is got precipitation with acid leach solution, gets supernatant, perhaps directly get the acid supernatant of gained in the step (1), transfer pH value to faintly acid with alkaline solution, with low pole or middle polarity resin absorption, water flushing resin column/bed shows colourless to effluent; Closely colourless with alkaline ethanol solution flushing resin column/bed again, perhaps closely colourless with alkaline solution flushing resin column/bed earlier, closely colourless with ethanol liquid flushing resin column/bed again to effluent to effluent to effluent;
(3) discard flushing liquor, carry out eluting with alcoholic solution again, closely colourless to eluent, collect eluent, reclaim ethanol to there not being the alcohol flavor, transfer pH value to alkalescence with alkaline solution, leave standstill, cold preservation, collecting precipitation is washed to white, promptly.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described extraction process is characterized in, when the sedimentary color of step (3) acquisition can not be washed to white, gets this precipitation with acid leach solution, transfers pH value to faintly acid with alkaline solution, and repeating step (2), (3) are white in color until precipitation.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described extraction process is characterized in, its step is as follows,
(1) get herb of Herba Solani Nigri and fruit, perhaps Fructus solani xanthocarpi, perhaps Australian eggplant adds the 50-90% alcoholic solution and extracts 2-4 time, and each 4-8 doubly measures, and reclaims ethanol, is concentrated into every milliliter and contains the concentrated solution that 0.5-4 restrains crude drug; Concentrated solution transfers pH value to 8-10 with the alkaline solution of 0.5-1.5mol/l, and cold preservation is left standstill, the centrifuging and taking precipitate; Perhaps add the 0.05-0.15mol/l acid solution in the concentrated solution, fully stir, leave standstill, centrifugal, get acid supernatant;
(2) the precipitate washing is 2-4 time, get precipitation with the 0.05-0.15mol/l acid leach solution, get supernatant, perhaps directly get the acid supernatant of gained in the step (1), transfer pH value to 2-4 with alkaline solution, with low pole or middle polarity resin absorption, elder generation's water flushing resin column/bed is closely neutral to effluent, not to be higher than alkaline ethanol solution flushing resin column/bed of 20% closely colourless to effluent to contain alcohol amount again, perhaps earlier closely colourless to effluent with 0.05-0.15mol/l alkaline solution flushing resin column/bed, be not higher than 20% ethanol liquid to wash resin column/bed closely colourless to effluent to contain the alcohol amount again;
(3) discard flushing liquor, carry out eluting with 50-80% ethanol again, closely colourless to eluent, collect eluent, reclaim ethanol to there not being the alcohol flavor, transfer pH value to 8-10, leave standstill cold preservation with the alkaline solution of 0.5-1.5mol/l, collecting precipitation is washed 2-4 time, is white in color to precipitating, promptly.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described extraction process, be characterized in, when the sedimentary color of step (3) acquisition can not be washed to white, get this precipitation with the 0.05-0.15mol/l acid leach solution, transfer pH value to faintly acid with the 0.05-0.15mol/l alkaline solution, repeating step (2), (3) 1-2 time are white in color until precipitation.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described extraction process is characterized in, its step is as follows,
(1) get herb of Herba Solani Nigri and fruit, perhaps Fructus solani xanthocarpi, perhaps Australian eggplant adds 80% ethanol extraction 3 times, and each 8 times of amounts reclaim ethanol to there not being the alcohol flavor, are concentrated into every milliliter of concentrated solution that contains 1 gram crude drug; NaOH solution with 1mol/l is transferred pH value to 9, cold preservation, standing over night, centrifuging and taking precipitate; Perhaps add the 0.1mol/l acid solution in the concentrated solution, fully stir, leave standstill, centrifugal, get acid supernatant;
(2) the precipitate washing is 3 times, get precipitation with the 0.1mol/l dissolve with hydrochloric acid solution, get supernatant, perhaps directly get the acid supernatant of gained in the step (1), NaOH solution with 1mol/l is transferred pH value to 3, with low pole or middle polarity resin absorption, elder generation's water flushing resin column/bed is closely neutral to effluent, closely colourless with 0.1mol/l ammonia 20% alcoholic solution flushing resin column/bed again to effluent, perhaps closely colourless with 0.1mol/l ammonia flushing resin column/bed earlier, closely colourless with 20% ethanol liquid flushing resin column/bed again to effluent to effluent;
(3) discard flushing liquor, carry out eluting with 70% ethanol again, show colourless to eluent, collect eluent, reclaim ethanol to nothing alcohol flavor, transfer pH value to 9 with the NaOH solution of 1mol/l, centrifugal, collecting precipitation is washed 3 times, is white in color to precipitating, promptly.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described extraction process is characterized in, when the sedimentary color of step (3) acquisition can not be washed to white, get this precipitation with the 0.1mol/l acid leach solution, transfer pH value to faintly acid with the NaOH solution of 1mol/l, repeating step (2), (3) are white in color to precipitating.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described extraction process is characterized in, described alkaline solution is selected from sodium hydroxide, calcium hydroxide, potassium hydroxide, magnesium hydroxide and ammonia spirit; Described acid solution is selected from acetic acid, hydrochloric acid, sulphuric acid and citric acid solution; Described alkaline ethanol solution is to contain the alkaline ethanol solution that is selected from sodium hydroxide, calcium hydroxide, potassium hydroxide, magnesium hydroxide and ammonia that concentration is 0.05-0.15mol/l.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described extraction process is characterized in, in step (1), other gets centrifugal back liquid, transfers pH value to 10-12, leaves standstill, and the centrifuging and taking precipitate merges precipitate twice.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described extraction process is characterized in, extract obtained dry product contains total alkaloids and is not less than 50% in α-solasonine.
Technical problem to be solved by this invention can also further realize by following technical scheme.The present invention is the extract obtained preparation of the above-described extraction process of a kind of usefulness, is characterized in, gets extract, adds conventional pharmaceutic adjuvant, and technology is made the medicament of any dosage form of clinical acceptable routinely.
Herba Solani Nigri is the plant amedica that contains the number of chemical composition, plant drymeal its pharmacological action of being used as medicine is the result of whole plants chemical constituent comprehensive function, mainly with water soluble compound performance pharmacological action, alcohol extract is brought into play pharmacological action with alkaloid compound to water soluble preparation.Herba Solani Nigri has immunomodulating and cell toxicant dual function, contains several mineral materials and vitamin and aminoacid etc. in addition, so herb is even more ideal through the pharmacological action of pure water mixed extraction composition.
Compared with prior art, technology of the present invention is selected into, and industrial applicibility is strong, and cost is relatively low, and extract obtained impurity is few, the effective component content height, and can further promote its pharmacology curative effect.The extract obtained medicament that can be used for preparing any dosage form of the present invention.
The specific embodiment
Embodiment 1.A kind of extraction process with plant total alkaloid extract of antitumor action, its step is as follows,
(1) get herb of Herba Solani Nigri and fruit, perhaps Fructus solani xanthocarpi, perhaps Australian eggplant adds alcoholic solution and extracts, and reclaims ethanol, concentrate, concentrated solution; Concentrated solution transfers pH value to alkalescence with alkaline solution, and cold preservation is left standstill, the centrifuging and taking precipitate; Perhaps add acid solution in the concentrated solution, fully stir, leave standstill, centrifugal, get acid supernatant;
(2) precipitate washing is got precipitation with acid leach solution, gets supernatant, perhaps directly get the acid supernatant of gained in the step (1), transfer pH value to faintly acid with alkaline solution, with low pole or middle polarity resin absorption, water flushing resin column/bed shows colourless to effluent; Closely colourless with alkaline ethanol solution flushing resin column/bed again, perhaps closely colourless with alkaline solution flushing resin column/bed earlier, closely colourless with ethanol liquid flushing resin column/bed again to effluent to effluent to effluent;
(3) discard flushing liquor, carry out eluting with alcoholic solution again, closely colourless to eluent, collect eluent, reclaim ethanol to there not being the alcohol flavor, transfer pH value to alkalescence with alkaline solution, leave standstill, cold preservation, collecting precipitation is washed to white, promptly.
Embodiment 2.In embodiment 1, when the sedimentary color of step (3) acquisition can not be washed to white, get this precipitation with the acetum dissolving, transfer pH value to faintly acid with sodium hydroxide solution, repeating step (2), (3) are white in color until precipitation.
Embodiment 3.In the step among the embodiment 1 (1), other gets centrifugal back liquid, transfers pH value to 10, leaves standstill, and the centrifuging and taking precipitate merges precipitate twice.
Embodiment 4.A kind of extraction process with plant total alkaloid extract of antitumor action, its step is as follows,
(1) get herb of Herba Solani Nigri and fruit, add 50% alcoholic solution and extract 2 times, each 8 times of amounts reclaim ethanol, are concentrated into every milliliter of concentrated solution that contains 0.5 gram crude drug; Concentrated solution is transferred pH value to 8 with the sodium hydroxide solution of 0.5mol/l, and cold preservation is left standstill, the centrifuging and taking precipitate; Perhaps add the 0.05mol/l hydrochloric acid solution in the concentrated solution, fully stir, leave standstill, centrifugal, get acid supernatant;
(2) the precipitate washing is 2 times, get precipitation with the 0.05mol/l dissolve with hydrochloric acid solution, get supernatant, perhaps directly get the acid supernatant of gained in the step (1), transfer pH value to 2 with sodium hydroxide, with low pole or middle polarity resin absorption, elder generation's water flushing resin column/bed is closely neutral to effluent, be that 20% the concentration that contains is that sodium hydroxide alcoholic solution flushing resin column/bed of 0.05mol/l is closely colourless to effluent to contain alcohol amount again, perhaps closely colourless with 0.05mol/l sodium hydroxide solution flushing resin column/bed earlier to effluent, be that 20% ethanol liquid flushing resin column/bed is closely colourless to effluent to contain the alcohol amount again;
(3) discard flushing liquor, carry out eluting with 50% ethanol again, closely colourless to eluent, collect eluent, reclaim ethanol to nothing alcohol flavor, transfer pH value to 8 with the sodium hydroxide solution of 0.5mol/l, leave standstill, cold preservation, collecting precipitation is washed 2 times, is white in color to precipitating, promptly.
Embodiment 5.In embodiment 4, when the sedimentary color of step (3) acquisition can not be washed to white, get this precipitation with the 0.05mol/l dissolve with hydrochloric acid solution, transfer pH value to faintly acid with the 0.05mol/l aqua calcis, repeating step (2), (3) 1 times are white in color to precipitation.
Embodiment 6.In the step (1) of embodiment 4, other gets centrifugal back liquid, transfers pH value to 12, leaves standstill, and the centrifuging and taking precipitate merges precipitate twice.
Embodiment 7.A kind of extraction process with plant total alkaloid extract of antitumor action, its step is as follows,
(1) get Fructus solani xanthocarpi, add 90% alcoholic solution and extract 4 times, each 4 times of amounts reclaim ethanol, are concentrated into every milliliter of concentrated solution that contains 4 gram crude drugs; Concentrated solution is transferred pH value to 10 with the aqua calcis of 1.5mol/l, and cold preservation is left standstill, the centrifuging and taking precipitate; Perhaps add the 0.15mol/l sulfuric acid solution in the concentrated solution, fully stir, leave standstill, centrifugal, get acid supernatant;
(2) the precipitate washing is 4 times, getting precipitation dissolves with the 0.15mol/l sulfuric acid solution, get supernatant, perhaps directly get the acid supernatant of gained in the step (1), transfer pH value to 4 with aqua calcis, with low pole or middle polarity resin absorption, elder generation's water flushing resin column/bed is closely neutral to effluent, again with contain alcohol amount be 15% to contain 0.15mol/l calcium hydroxide alcoholic solution flushing resin column/bed closely colourless to effluent, perhaps closely colourless with 0.15mol/l aqua calcis flushing resin column/bed earlier to effluent, be that 15% ethanol liquid flushing resin column/bed is closely colourless to effluent to contain the alcohol amount again;
(3) discard flushing liquor, carry out eluting with 80% ethanol again, closely colourless to eluent, collect eluent, reclaim ethanol to nothing alcohol flavor, transfer pH value to 10 with the magnesium hydroxide solution of 1.5mol/l, leave standstill, cold preservation, collecting precipitation is washed 4 times, is white in color to precipitating, promptly; Extract obtained dry product contains total alkaloids and counts 60% with α-solasonine.
Embodiment 8.Embodiment 7 described extraction processes, when the sedimentary color of step (3) acquisition can not be washed to white, get this precipitation with the dissolving of 0.15mol/l citric acid solution, transfer pH value to faintly acid with the 0.15mol/l potassium hydroxide solution, repeating step (2), (3) 2 times are white in color to precipitation.
Embodiment 9.In the step (1) of embodiment 7, other gets centrifugal back liquid, transfers pH value to 11, leaves standstill, and the centrifuging and taking precipitate merges precipitate twice.
Embodiment 10.A kind of extraction process with plant total alkaloid extract of antitumor action, its step is as follows,
(1) get Australian eggplant, add 80% ethanol extraction 3 times, each 8 times of amounts reclaim ethanol to there not being the alcohol flavor, are concentrated into every milliliter of concentrated solution that contains 1 gram crude drug; NaOH solution with 1mol/l is transferred pH value to 9, cold preservation, standing over night, centrifuging and taking precipitate; Perhaps add the 0.1mol/l acid solution in the concentrated solution, fully stir, leave standstill, centrifugal, get acid supernatant;
(2) the precipitate washing is 3 times, get precipitation with the 0.1mol/l dissolve with hydrochloric acid solution, get supernatant, perhaps directly get the acid supernatant of gained in the step (1), NaOH solution with 1mol/l is transferred pH value to 3, with low pole or middle polarity resin absorption, elder generation's water flushing resin column/bed is closely neutral to effluent, closely colourless with 0.1mol/l ammonia 20% alcoholic solution flushing resin column/bed again to effluent, perhaps closely colourless with 0.1mol/l ammonia flushing resin column/bed earlier, closely colourless with 20% ethanol liquid flushing resin column/bed again to effluent to effluent;
(3) discard flushing liquor, carry out eluting with 70% ethanol again, show colourless to eluent, collect eluent, reclaim ethanol to nothing alcohol flavor, transfer pH value to 9 with the NaOH solution of 1mol/l, centrifugal, collecting precipitation is washed 3 times, is white in color to precipitating, promptly; Extract obtained dry product contains total alkaloids and counts 50% with α-solasonine.
Embodiment 11.Embodiment 10 described extraction processes, when the sedimentary color of step (3) acquisition can not be washed to white, get this precipitation with the 0.1mol/l acid leach solution, transfer pH value to faintly acid with the NaOH solution of 1mol/l, repeating step (2), (3) are white in color to precipitating.
Embodiment 12.Press the extract obtained preparation of extraction process of embodiment 1, its preparation method is, gets extract, adds conventional pharmaceutic adjuvant, and technology is made capsule routinely.
Embodiment 13.Press the extract obtained preparation of extraction process of embodiment 3, its preparation method is, gets extract, adds conventional pharmaceutic adjuvant, and technology is made tablet routinely.
Embodiment 14.Press the extract obtained preparation of extraction process of embodiment 5, its preparation method is, gets extract, adds conventional pharmaceutic adjuvant, and technology is made granule routinely.
Embodiment 15.Press the extract obtained preparation of extraction process of embodiment 7, its preparation method is, gets extract, adds conventional pharmaceutic adjuvant, and technology is made injection routinely.
Embodiment 16.Press the extract obtained preparation of extraction process of embodiment 10, its preparation method is, gets extract, adds conventional pharmaceutic adjuvant, and technology is made lyophilized injectable powder routinely.
Claims (10)
1, a kind of extraction process with plant total alkaloid extract of antitumor action is characterized in that, its step is as follows,
(1) get herb of Herba Solani Nigri and fruit, perhaps Fructus solani xanthocarpi, perhaps Australian eggplant adds alcoholic solution and extracts, and reclaims ethanol, concentrate, concentrated solution; Concentrated solution transfers pH value to alkalescence with alkaline solution, and cold preservation is left standstill, the centrifuging and taking precipitate; Perhaps add acid solution in the concentrated solution, fully stir, leave standstill, centrifugal, get acid supernatant;
(2) precipitate washing is got precipitation with acid leach solution, gets supernatant, perhaps directly get the acid supernatant of gained in the step (1), transfer pH value to faintly acid with alkaline solution, with low pole or middle polarity resin absorption, water flushing resin column/bed shows colourless to effluent; Closely colourless with alkaline ethanol solution flushing resin column/bed again, perhaps closely colourless with alkaline solution flushing resin column/bed earlier, closely colourless with ethanol liquid flushing resin column/bed again to effluent to effluent to effluent;
(3) discard flushing liquor, carry out eluting with alcoholic solution again, closely colourless to eluent, collect eluent, reclaim ethanol to there not being the alcohol flavor, transfer pH value to alkalescence with alkaline solution, leave standstill, cold preservation, collecting precipitation is washed to white, promptly.
2, extraction process according to claim 1 is characterized in that, when the sedimentary color of step (3) acquisition can not be washed to white, get this precipitation with acid leach solution, transfer pH value to faintly acid with alkaline solution, repeating step (2), (3) are white in color until precipitation.
3, extraction process according to claim 1 is characterized in that, its step is as follows,
(1) get herb of Herba Solani Nigri and fruit, perhaps Fructus solani xanthocarpi, perhaps Australian eggplant adds the 50-90% alcoholic solution and extracts 2-4 time, and each 4-8 doubly measures, and reclaims ethanol, is concentrated into every milliliter and contains the concentrated solution that 0.5-4 restrains crude drug; Concentrated solution transfers pH value to 8-10 with the alkaline solution of 0.5-1.5mol/l, and cold preservation is left standstill, the centrifuging and taking precipitate; Perhaps add the 0.05-0.15mol/l acid solution in the concentrated solution, fully stir, leave standstill, centrifugal, get acid supernatant;
(2) the precipitate washing is 2-4 time, get precipitation with the 0.05-0.15mol/l acid leach solution, get supernatant, perhaps directly get the acid supernatant of gained in the step (1), transfer pH value to 2-4 with alkaline solution, with low pole or middle polarity resin absorption, elder generation's water flushing resin column/bed is closely neutral to effluent, not to be higher than alkaline ethanol solution flushing resin column/bed of 20% closely colourless to effluent to contain alcohol amount again, perhaps earlier closely colourless to effluent with 0.05-0.15mol/l alkaline solution flushing resin column/bed, be not higher than 20% ethanol liquid to wash resin column/bed closely colourless to effluent to contain the alcohol amount again;
(3) discard flushing liquor, carry out eluting with 50-80% ethanol again, closely colourless to eluent, collect eluent, reclaim ethanol to there not being the alcohol flavor, transfer pH value to 8-10, leave standstill cold preservation with the alkaline solution of 0.5-1.5mol/l, collecting precipitation is washed 2-4 time, is white in color to precipitating, promptly.
4, extraction process according to claim 3, it is characterized in that, when the sedimentary color of step (3) acquisition can not be washed to white, get this precipitation with the 0.05-0.15mol/l acid leach solution, transfer pH value to faintly acid with the 0.05-0.15mol/l alkaline solution, repeating step (2), (3) 1-2 time are white in color until precipitation.
5, extraction process according to claim 3 is characterized in that, its step is as follows,
(1) get herb of Herba Solani Nigri and fruit, perhaps Fructus solani xanthocarpi, perhaps Australian eggplant adds 80% ethanol extraction 3 times, and each 8 times of amounts reclaim ethanol to there not being the alcohol flavor, are concentrated into every milliliter of concentrated solution that contains 1 gram crude drug; NaOH solution with 1mol/l is transferred pH value to 9, cold preservation, standing over night, centrifuging and taking precipitate; Perhaps add the 0.1mol/l acid solution in the concentrated solution, fully stir, leave standstill, centrifugal, get acid supernatant;
(2) the precipitate washing is 3 times, get precipitation with the 0.1mol/l dissolve with hydrochloric acid solution, get supernatant, perhaps directly get the acid supernatant of gained in the step (1), NaOH solution with 1mol/l is transferred pH value to 3, with low pole or middle polarity resin absorption, elder generation's water flushing resin column/bed is closely neutral to effluent, closely colourless with 0.1mol/l ammonia 20% alcoholic solution flushing resin column/bed again to effluent, perhaps closely colourless with 0.1mol/l ammonia flushing resin column/bed earlier, closely colourless with 20% ethanol liquid flushing resin column/bed again to effluent to effluent;
(3) discard flushing liquor, carry out eluting with 70% ethanol again, show colourless to eluent, collect eluent, reclaim ethanol to nothing alcohol flavor, transfer pH value to 9 with the NaOH solution of 1mol/l, centrifugal, collecting precipitation is washed 3 times, is white in color to precipitating, promptly.
6, extraction process according to claim 5, it is characterized in that, when the sedimentary color of step (3) acquisition can not be washed to white, get this precipitation with the 0.1mol/l acid leach solution, transfer pH value to faintly acid with the NaOH solution of 1mol/l, repeating step (2), (3) are white in color to precipitating.
7, according to any one described extraction process among the claim 1-4, it is characterized in that described alkaline solution is selected from sodium hydroxide, calcium hydroxide, potassium hydroxide, magnesium hydroxide and ammonia spirit; Described acid solution is selected from acetic acid, hydrochloric acid, sulphuric acid and citric acid solution; Described alkaline ethanol solution is to contain the alkaline ethanol solution that is selected from sodium hydroxide, calcium hydroxide, potassium hydroxide, magnesium hydroxide and ammonia that concentration is 0.05-0.15mol/l.
According to claim 1 or 3 or 5 described extraction processes, it is characterized in that 8, in step (1), other gets centrifugal back liquid, transfers pH value to 10-12, leaves standstill, the centrifuging and taking precipitate merges precipitate twice.
According to any one described extraction process among the claim 1-8, it is characterized in that 9, extract obtained dry product contains total alkaloids and is not less than 50% in α-solasonine.
10, the extract obtained preparation of any one described extraction process among the claim 1-9 is characterized in that, gets extract, adds conventional pharmaceutic adjuvant, and technology is made the medicament of any dosage form of clinical acceptable routinely.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101246151B (en) * | 2007-02-14 | 2012-02-01 | 刘阳 | Quality control method of nightshade total alkali preparations |
| CN101108872B (en) * | 2006-07-21 | 2012-07-18 | 江苏中康药物科技有限公司 | Plants natural base extract and formulated product and use thereof |
| CN101108224B (en) * | 2006-07-21 | 2012-07-18 | 江苏中康药物科技有限公司 | Plants natural base extractive and formulated product and use thereof |
| CN103099891A (en) * | 2011-11-09 | 2013-05-15 | 安康市天源植物提取有限公司 | Preparation method of belladonna extract |
| CN105267421A (en) * | 2008-02-18 | 2016-01-27 | 徐华民 | Application of solanum nigrum effective ingredients to preparation of drugs treating lithiasis |
| CN106509579A (en) * | 2016-11-24 | 2017-03-22 | 张锦超 | Preparation method for nigrum fruit products |
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2005
- 2005-11-17 CN CNB2005100954557A patent/CN100333753C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101108872B (en) * | 2006-07-21 | 2012-07-18 | 江苏中康药物科技有限公司 | Plants natural base extract and formulated product and use thereof |
| CN101108224B (en) * | 2006-07-21 | 2012-07-18 | 江苏中康药物科技有限公司 | Plants natural base extractive and formulated product and use thereof |
| CN101246151B (en) * | 2007-02-14 | 2012-02-01 | 刘阳 | Quality control method of nightshade total alkali preparations |
| CN105267421A (en) * | 2008-02-18 | 2016-01-27 | 徐华民 | Application of solanum nigrum effective ingredients to preparation of drugs treating lithiasis |
| CN103099891A (en) * | 2011-11-09 | 2013-05-15 | 安康市天源植物提取有限公司 | Preparation method of belladonna extract |
| CN106509579A (en) * | 2016-11-24 | 2017-03-22 | 张锦超 | Preparation method for nigrum fruit products |
| CN106509579B (en) * | 2016-11-24 | 2017-06-30 | 张锦超 | A kind of preparation method of black nightshade fruit product |
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