DE1911862C3 - Process for obtaining a standardized, spasmolytically effective Petasites extract with a content of 50 to 55% of genuine Petasin - Google Patents

Description

Until a few days ago, there was still rulership among experts the popular belief that over 40% petasin-containing petasites extracts are effective and petasin content are unstable over a long period of time.

The method according to the invention is described below using an exemplary embodiment:

Embodiment

100 kg of Radix petasües pul vis were macerated for ten days with 200 liters of 96 percent by volume ethyl alcohol, the maceration temperature being 22 ° C. Subsequently was the whole thing coated with linen, the extraction material pressed in a press and the colatur united with the press fluid. This total macerate solution was then filtered through quick paper filters filtered. The clear, brown filtrate was gently under reduced pressure below 50 ° C to honey-like consistency of the base extract.

The distillate was collected and used for the next extractions of new drugs. The base extract yield was 4.2%. The petasin content of this base extract was 23.5%.

2.5 kg of this base extract became at 62 ° C with stirring with 2.7 liters of 96 percent by volume Ethyl alcohol slurried and in a separator with 2.5 liters of a 2% aqueous Tartaric acid solution added. After vigorous mixing, the mixture became 4.4 liters of chloroform added and the whole batch again vigorously stirred for 5 minutes. For a good separation of the layers, the mixture was then left to rest for two hours.

During this time the pctasin-containing, very dark brown chloroform layer collected at the bottom of the vessel. The watery top layer appeared light brown and cloudy. Between the two Phases, a whitish intermediate layer formed, which consisted of a fine, insoluble crystal brci. It is part of the so-called upper phase and was treated as such in the shaking process and not worked up separately.

The chloroform phase was separated off after the prescribed time and collected in another separating container. The remaining upper phase was extracted again with 1 liter of chloroform. After being sharply separated, this became Combined chloroform phase of the first extraction. The upper phase was discarded. The United Chloroform phases were washed once with a mixture of ISO ml of ethyl alcohol and 950 ml of water. As soon as both layers are sharp had separated, the chloroform phase was transferred to a distillation apparatus and the solvent under reduced pressure and at about 40 distilled off up to 45 ° C. The distillation residue

S was a dark brown, medium-viscosity, strongly bitter-tasting oil with a petasin content of 58.4%. The yield, based on the initial amount of base extract used, was 40.2% petasin-rich faction.

ίο To standardize the petasin content to one With a petasin content of 50 to 55%, the extract, which is richer in petasin, is made in a blender with as much des Basic extract added so that an end product with a content of 50 to 55% Petasin is created

The purpose was to use 1000 grams of the higher petasin fraction intensively mixed with 230 grams of base extract.

If necessary, the whole thing can be done before mixing

be heated to about 40 ° C.

Extended durability tests due to

a »of UV-spectroscopic determinations of the petasin content and of measurements of the spasmolytic Potency in comparison with papaverine hydrochloride have shown that of the present 50 to 55% petasitesex produced by the

»5 trakt does not suffer any loss of quality even after long periods of storage. Of particular importance in This method is the distribution of the ethanol base extract between a 1 to 3% / own aqueous tartaric acid solution in the ethyl alcohol suspension

mung and the chloroform. On the one hand, the good dissolving power of chloroform plays a role for everyone homoeopolar organic substances play a decisive role, as well as the hydrophilic on the other hand Character of ethanol. The dosage of the wine acid is chosen so that indifferent ballast Substances are largely separated without changing the active ingredients. Only the mixture of the petasin-containing phase with the base extract guarantees this Version of a galenically highly effective end product

* ° dukts.

If the concentration of tartaric acid is increased, the final content of petasin deteriorates. It has also been shown that the tartaric acid cannot be replaced by another acid without

To accept losses to Petasin.

Is z. B. used in place of ethyl alcohol, methyl alcohol as a solvent, so isomerized the petasin. The determination of the petasin content is based on

others on the one determined by Aebi / Waalcr molar extinction coefficient based on the absorption maximum at 230 nm in ethyl alcohol, including petasin and petasin-like substances.

Claims (1)

Patent; iisprudi: Process for obtaining a standardized, spasmolytically effective Petasites extract with a content of 50 to 55% of genuine Petasin, characterized in that by ten days of maceration of finely ground Petasites rhizomes with 96 percent by volume ethyl alcohol, the maceration temperature being at least 20 ° C and Should not exceed 30 ° C, first a base extract with an approximate petasin content of 25% is obtained by colourizing the extraction material and then squeezing it in a press, that the colature is combined with the pressing liquid that is then filtered, after which the clear, brown filtrate under reduced pressure and below 50 ^c C gently until the honey-like consistency is concentrated, that then the basic extract obtained in this way at 60 to 65 ° C while stirring with ethyl aufschwemmt and in a waste "cheideapparatur with as many liters 1 to 3% aqueous tartaric acid solution added, such as the e The basic extract obtained weighs in at kilograms, so that after vigorous mixing, at least as many liters of chloroform are added to this mixture as the ethyl alcohol required to suspend it, the total salt being stirred vigorously for a few minutes, so that the whole thing is then left to stand until the layers are separated have separated, whereby the petasin-containing, very dark brown chloroformschidite collects at the bottom of the vessel, that this chloroform layer is then separated off and collected in a separate separating container, that the upper layer is again stirred with chloroform and the combined chloroform extracts with a mixture consisting of 1, 5 volumes of ethyl alcohol and 9.5 volumes of water, washed once, that the solvent is distilled off under reduced pressure at 40 to 45 ° C, and that finally the distillation residue, a dark brown, medium-viscosity, strongly bitter-tasting oil with a petasin content of 65 to 70%, for standardization ng to an i'etasin content of 50 to 55% with so much of the base extract with about 25% petasin content added that the end product has a content of 50 to 55% petasin. The invention relates to a method for obtaining a standardized, spasmolytically effective Petasites extract with a content of 50 to 55% of genuine petasin, which is characterized by it is that through ten days of maceration of finely ground Petasites rhizomes with Ethyl alcohol by volume with a maceration temperature of at least 20 ° C and Should not exceed 30 ° C, initially a basic extract with a petasin content of approximately 25% is obtained in that the extraction material is koliert and then pressed in a press that the colatur is combined with the press liquid, that is then filtered, after which the clear, brown filtrate under reduced pressure and below 50 ° C gently to a honey-like consistency restricts that then the base extract obtained in this way at 60 to 65 ° C with stirring floated with ethyl alcohol and in a separator with as many liters of a 1- to ίο 3% aqueous tartaric acid solution added, such as the basic extract obtained weighs in kilograms that after vigorous mixing! this mixture add at least as many liters of chloroform as the ethyl alcohol required to float, the whole batch being stirred vigorously for a few minutes so that the whole thing is then Let rest until the layers have separated, whereby the petasin-containing, strongly dark brown Chloroform layer accumulates at the bottom of the vessel, so that this chloroformschidit then separates and collects in a separate separator that you can again with the top layer Stirring out chloroform and the combined chloroform extracts mic a mixture consisting of »5 1.5 volumes of ethyl alcohol and 9.5 volumes of water, washed once that the solvent is distilled off under reduced pressure at 40 to 45 ° C, and that you finally get the distillation residue, a dark brown, medium viscosity, strongly bitter Tasting oil with a petasin content of 65 to 70%, for standardization on a petasin content from 50 to 55% with so much of the base extract with about 25% petasin content added that the end product has a content of 50 to 55% petasin. So far it has not been possible to produce standardized petasites extracts with a petasin content of 50 to 55%.
One of the difficulties was that particular care had to be taken that petasin and S-petasin isomerize in the presence of mineral acids or aluminum oxides to iso-petasin and S-iso-petasin, respectively. In an alkaline environment, the petasin also splits into iso-petasol, angelicic acid and partially into a-methyl- / 3-hydroxybutyric acid. If only because of the impossibility of producing crystallized, stable Petasin of constant potency, such as. B. spasmolytic efficacy, to iso-Heren in a rational yield, urged - by bypassing crystallizations and adsorption chromatography with regard to undesired isomerization - shaking operations with selective solvents in a two-phase system with the aim of eluting highly concentrated petasin fractions. Among all the constituents of the Petasites Rhizome is due mainly to spasmolytic The effects of substances investigated, the petasin - in addition to some other spasmolytics that tasin are more or less chemically related - the attributed the greatest effectiveness. Some of these ingredients include: Petasin, iso-Petasin, iso-PetasoI, S-Petasin and iso-S-Petasin. These active ingredients are largely Angehca-Tiglin or methyl mercaptoacrylic acid compounds, which are esterified with a Cu alcohol.