DE909936C - Process for the extraction of active ingredients from flowers of Arnica montana - Google Patents
Process for the extraction of active ingredients from flowers of Arnica montanaInfo
- Publication number
- DE909936C DE909936C DEK3104D DEK0003104D DE909936C DE 909936 C DE909936 C DE 909936C DE K3104 D DEK3104 D DE K3104D DE K0003104 D DEK0003104 D DE K0003104D DE 909936 C DE909936 C DE 909936C
- Authority
- DE
- Germany
- Prior art keywords
- active ingredients
- flowers
- iodine
- arnica montana
- extraction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- 239000004480 active ingredient Substances 0.000 title claims description 7
- 241000086254 Arnica montana Species 0.000 title claims description 4
- 238000000034 method Methods 0.000 title claims description 4
- 238000000605 extraction Methods 0.000 title description 2
- 238000001556 precipitation Methods 0.000 claims description 5
- 229930013930 alkaloid Natural products 0.000 claims description 4
- 150000003797 alkaloid derivatives Chemical class 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 230000001376 precipitating effect Effects 0.000 claims description 4
- 239000006286 aqueous extract Substances 0.000 claims description 3
- RCTYPNKXASFOBE-UHFFFAOYSA-M chloromercury Chemical compound [Hg]Cl RCTYPNKXASFOBE-UHFFFAOYSA-M 0.000 claims description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 2
- SWJBITNFDYHWBU-UHFFFAOYSA-N [I].[I] Chemical compound [I].[I] SWJBITNFDYHWBU-UHFFFAOYSA-N 0.000 claims description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 2
- 229910052740 iodine Inorganic materials 0.000 claims description 2
- 239000011630 iodine Substances 0.000 claims description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims 1
- 230000004048 modification Effects 0.000 claims 1
- 238000012986 modification Methods 0.000 claims 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000002244 precipitate Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 241000208983 Arnica Species 0.000 description 4
- 239000006188 syrup Substances 0.000 description 4
- 235000020357 syrup Nutrition 0.000 description 4
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 description 3
- 229960001231 choline Drugs 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 2
- LWJROJCJINYWOX-UHFFFAOYSA-L mercury dichloride Chemical compound Cl[Hg]Cl LWJROJCJINYWOX-UHFFFAOYSA-L 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- LWQAYTWMEQUUFP-UHFFFAOYSA-K [K].I[Bi](I)I Chemical compound [K].I[Bi](I)I LWQAYTWMEQUUFP-UHFFFAOYSA-K 0.000 description 1
- ZVAKTWSQIIRIIH-UHFFFAOYSA-N [K].[I] Chemical compound [K].[I] ZVAKTWSQIIRIIH-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- IYDGMDWEHDFVQI-UHFFFAOYSA-N phosphoric acid;trioxotungsten Chemical compound O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.OP(O)(O)=O IYDGMDWEHDFVQI-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- YPNVIBVEFVRZPJ-UHFFFAOYSA-L silver sulfate Chemical compound [Ag+].[Ag+].[O-]S([O-])(=O)=O YPNVIBVEFVRZPJ-UHFFFAOYSA-L 0.000 description 1
- 229910000367 silver sulfate Inorganic materials 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G5/00—Alkaloids
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Description
Verfahren zur Gewinnung von Wirkstoffen aus Blüten von Arnica montana Im Patent 744 283 ist ein Verfahren zur Gewinnung von Wirkstoffen aus Blüten von Arnica montana beschrieben, welches darin besteht, daß der vorgereinigte wäßrige Extrakt aus Arnicablüten durch Extraktion mit Äther von toxischen Bestandteilen befreit und mit einem der üblichen Alkaloidfällungsmittel, wie Kieselwolframsäure, Phosphorwolframsäure, Kaliumwismutjodid, Jodjodkalium, gefällt wird. Darauf wird die Fällung zerlegt und die die gereinigten Wirkstoffe enthaltende Lösung bis zur Kristallisation eingeengt.Method for obtaining active ingredients from flowers of Arnica montana In patent 744 283 a method for obtaining active ingredients from flowers of Arnica montana is described, which consists in that the pre-purified aqueous extract from arnica flowers is freed of toxic components by extraction with ether and with a the usual alkaloid precipitating agents, such as silicatungstic acid, phosphotungstic acid, potassium bismuth iodide, iodine iodide, is precipitated. The precipitate is then broken down and the solution containing the purified active ingredients is concentrated until it crystallizes.
Es wurde nun weiterhin gefunden, daß man als Alkaloidfällungsmittel vorteilhaft auch Quecksilberchlorid anwenden kann; hierbei besteht die Fällung in der Hauptsache aus dem Doppelsalz Cholinchlorid-Quecksilberchlorid, während im Filtrat die übrigen therapeutisch wertvollen, blutdrucksteigernden Wirkstoffe der Arnica vorhanden sind. Diese Wirkstoffe werden durch Fällung mit Jodjodkalium abgetrennt und aus dem erhaltenen Niederschlag nach Entfernung des Jods gewonnen. Beispiel i kg Arnicablüten werden mit Petroläther erschöpfend extrahiert und dann mit Wasser ausgezogen. Der wäßrige Extrakt wird im Vakuum zu einem dicken Sirup eingedampft, mit Alkohol gefällt, das Filtrat nach dem Abtrennen des Niederschlags abermals zum Sirup eingedampft und der verbleibende Rückstand von etwa 2o bis 30 g reit der doppelten bis dreifachen Menge Wasser aufgenommen. Die so erhaltene wäßrige Lösung wird erschöpfend mit Äther extrahiert, zum Sirup eingedampft, mit Alkohol wieder aufgenommen und so lange mit alkoholischer Quecksilberchloridlösung versetzt, bis kein Niederschlag mehr ausfällt. Die Lösung wird dann von dem ausgeschiedenen Niederschlag, der in der Hauptsache aus dem Doppelsalz Cholinchlorid-Quecksilberchlorid besteht, abgetrennt, mit Schwefelwasserstoff vom überschüssigen Quecksilber befreit und zur Entfernung des Alkohols eingedampft. Es verbleibt ein dünner rotbrauner Sirup, der die therapeutisch wertvollen, blutdrucksteigernden Bestandteile der Arnica frei von dem entgegengesetzt wirkenden und an sich therapeutisch wertlosen Cholin enthält. Er wird mit Jodjodkalium versetzt. Der sich abscheidende schwarze schmierige Niederschlag wird nach 24stündigem Stehen in der Kälte abgetrennt, in Alkohol gelöst, bis zum Verschwinden der Jod-Stärke-Reaktion mit schwefliger Säure und dann mit überschüssigem Silbersulfat versetzt und filtriert. Das Filtrat wird mit Natriumchloridlösung vom Überschuß des Silbers befreit, nochmals filtriert, mit Natriumcarbonat neutralisiert und im Vakuum zur Trockne verdampft. Die Lösung des Eindampfrückstandes in absolutem Alkohol wird filtriert und wiederum im Vakuum stark eingeengt. Beim weiteren Verdunsten des Lösungsmittels hinterbleibt ein amorpher Rückstand. Ausbeute etwa o,og g je r kg Blüten.It has now also been found that mercury chloride can also advantageously be used as the alkaloid precipitating agent; Here the precipitation consists mainly of the double salt choline chloride-mercury chloride, while the other therapeutically valuable, blood pressure-increasing active substances of arnica are present in the filtrate. These active ingredients are separated off by precipitation with iodine iodine and obtained from the resulting precipitate after the iodine has been removed. Example 1 kg of arnica flowers are exhaustively extracted with petroleum ether and then extracted with water. The aqueous extract is evaporated to a thick syrup in vacuo, precipitated with alcohol, the filtrate is again evaporated to a syrup after the precipitate has been separated off and the remaining residue of about 20 to 30 g is taken up with twice to three times the amount of water. The aqueous solution obtained in this way is extracted exhaustively with ether, evaporated to a syrup, taken up again with alcohol and mixed with alcoholic mercury chloride solution until no more precipitate separates out. The solution is then separated from the precipitate, which consists mainly of the double salt choline chloride-mercury chloride, freed from excess mercury with hydrogen sulfide and evaporated to remove the alcohol. What remains is a thin red-brown syrup that contains the therapeutically valuable, blood pressure-increasing components of arnica, free of the opposing and therapeutically worthless choline. Iodine potassium is added to it. The black, greasy precipitate which separates out is separated after standing in the cold for 24 hours, dissolved in alcohol, treated with sulphurous acid and then with excess silver sulfate until the iodine-starch reaction disappears and then filtered. The filtrate is freed from excess silver with sodium chloride solution, filtered again, neutralized with sodium carbonate and evaporated to dryness in vacuo. The solution of the evaporation residue in absolute alcohol is filtered and again strongly concentrated in vacuo. When the solvent evaporates further, an amorphous residue remains. Yield about o, og g per kg of flowers.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEK3104D DE909936C (en) | 1942-11-03 | 1942-11-03 | Process for the extraction of active ingredients from flowers of Arnica montana |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEK3104D DE909936C (en) | 1942-11-03 | 1942-11-03 | Process for the extraction of active ingredients from flowers of Arnica montana |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE909936C true DE909936C (en) | 1954-04-26 |
Family
ID=7209724
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DEK3104D Expired DE909936C (en) | 1942-11-03 | 1942-11-03 | Process for the extraction of active ingredients from flowers of Arnica montana |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE909936C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6742512B1 (en) | 2003-06-23 | 2004-06-01 | Avalon Manufactoring Co. | Paintball guns having hopper, adapter and/or feed tube aiming/pointing device mounting assemblies |
-
1942
- 1942-11-03 DE DEK3104D patent/DE909936C/en not_active Expired
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6742512B1 (en) | 2003-06-23 | 2004-06-01 | Avalon Manufactoring Co. | Paintball guns having hopper, adapter and/or feed tube aiming/pointing device mounting assemblies |
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