HU209998B - Process for producing plant extract against catarrh - Google Patents

Abstract

The present invention relates to a method for producing a herbal extract against colds, comprising 20-30% thyme, 30-40% of soap cake, 5-15% linden blossom, 15-25% marshmallow, 5-15% sweet fennel. containing a known excipient (s), (a) extracted by cooking recovery, or (b) soaked in water at 40 to 70 ° C for 1 to 4 hours, pressurized and / or centrifuged from the paste. , if desired, the residue is again soaked in water and reprocessed and / or centrifuged, and the resulting liquor is then concentrated, optionally adding an adsorbent to the effluent and vapor, which is washed with a solvent at the end of the concentration, and the resulting solution is combined after the dewatering of the concentrate. the remaining part of. EN 209 998 A Scope of the description: 6 pages

Description

FIELD OF THE INVENTION The present invention relates to a novel process for the preparation of herbal extracts for colds, containing 2030% by weight of thyme, 30-40% by weight of soap root, 5-15% by weight of linden blossom, 15-25% by weight of mallow leaves, 5-15% by weight of fennel. starting from a herbal blend containing known excipient (s).

Herbs containing medicinal and aromatic substances have been playing an increasingly important role in medicine in recent decades.

There are many arguments for the medicinal use of herbs. It is a very important fact that herbs that are known and used today (hundreds of herbs) have been in use for centuries, * and it has been clarified, besides curative effects, that they have no harmful effects and / or side effects on the human body.

Recently, the so-called aromatherapy, which focuses on the use of aromatic and essential oil constituents of various herbs (G. Rácz, A. Laza, E. Coiciu: Medicinal and essential oil plants, Ceres Publishing House, Bucharest, 1972) has recently come to the fore.

There is currently a wide variety of herbal remedies available from various herbs, and of course, the literature also suggests a variety of mixtures for the treatment of various diseases.

It is still a much debated question which of the herbal blends used to cure various diseases or even to maintain health is the most suitable to achieve the desired effect. In the current state of science, this debate cannot be resolved because, while some plants can identify the molecule responsible for the effect (eg, Digital, Claviceps, Papaver, Catharantus, Vinca), many plants have been isolated and their structure has not been determined. it was possible to find the molecule that is clearly responsible for the effect, so the theory is likely that the effect may be due to the combined effect of potentially complex organic molecules (sometimes very complex) (alkaloids, glycosides, terpenes, flavonides, anthraquinone derivatives, etc.). synergist) (H. Wagner, Drogen und Ihre Inhalttsstoffe, Pharmazeutische Biologie, 1979, G. Fischer Verlag, Stuttgart, New York; F. Deutschmann et al., Droganalyse I: Morphologie and Anatomie Pharmazeutische Biologie, 1979, G. Fischer). Verlag, Stuttgart, New York).

The synergistic effect or effects of a system of molecules made up of many herbs that are theoretically capable of exerting many effects, and this depends on the proportion of the ingredients, is generally inconceivable based on our present knowledge.

The various formulations used in a particular field of action are said to have a common principal effect, but differ in their degree of effect and in other, generally advantageous, side effects, and each generally has some positive effect over the others.

However, it seems clear that herbal-based medicinal products will have the greatest effect if the highest proportion of the original active ingredients of the herb are contained in the formulation or application form to be used.

There are several works that describe the blend of colds for tea.

The following compositions are mentioned in the book Rápóti-Romváry Healing Plants:

I. Marshmallow root (20 units of mass (hereinafter: you.)), Liquorice root (15 teas.), Hyssop (10 teas.), Yarrow (10 teas.), Sage leaves (10 teas.), Mallow flowers (5 teas.), Elderflower (5 teas.), Peppermint leaves (3 teas.), Linden flowers (5 teas.), Camomile flowers (5 teas.), Willow bark (5 teas.), Sickle (5 teas.).

II. Nettle leaves (40 teas), thyme (40 teas), narrow-leaved plantain (30 teas), linden flowers (20 teas), marshmallow root (20 teas), licorice (15 teas), hyssop (10 teas) , Jerusalem artichoke (10 tsp.), sage leaves (10 tsp.), mallow flowers (5 tsp.).

There are two other recipes in the book that use different types of herbs in a variety similar to the above.

It is clear from the above that there are indeed many herbal remedies for different herbal remedies with different compositions, and it is likely that each of them has some positive additional effects over the others (while, of course, they have other, also called positive) effects.

Specifically, each of the works mentioned in the above sources considers it necessary to boil the drug mixture for a period of time (usually at least 20 minutes).

A common feature of herbal, volatile and aromatic herbs is that they are generally heat-, light- and oxygen-sensitive and hydrolyze when heated in aqueous solution. For centuries, it has been observed that boiling or boiling the plants can produce aqueous solutions which are curative. Only one or two of the very decomposing plants, such as rose hips, are subjected to a gentler heat treatment, however, as shown above, in the field of tea mixtures for colds, boiling recovery is used. One reason for this is that, by boiling, the more soluble components can be dissolved, and on the other hand, the solution is sterilized. Significant loss of active ingredient was previously unimportant given the low availability of starting materials.

Currently, commercially available herb-based products are manufactured on an industrial scale, reaching the required production capacity by simple enlargement and enlargement of traditional methods. Due to the size increase, the large amount of starting material will remain relatively longer in the active ingredient under non-mild conditions.

HU 209 998 A

We have investigated the question of the proportion of useful materials in the final product which is present in the manufacturing processes used.

At the generally used extraction at 100 ° C (for 15-20 minutes, with about 25-27% dry solids recovery), the alkaloids are ca. 50% by weight of glycosides. 55% by weight of flavonoids. 60%, anthraquinones ca. 65% of the terpene, ca. 50% by volume can be analyzed in the aqueous solution and only 10-15% of the aromatics are found.

For commercial formulations, it is essential to concentrate the resulting solution, usually by vacuum evaporation (atmospheric evaporation is even more disadvantageous). According to our measurements, the amount of organic matter belonging to the group listed above is further reduced by 10-30%, while the aroma substances are completely eliminated.

It is an object of the present invention to provide an herbal extract which contains a proportion of components which, in addition to its action against colds, has beneficial physiological effects, requires a large amount of available starting materials, and on the other hand, provides significantly better yields of active ingredients and flavorings.

The initial herbal composition of the present invention required lengthy experimentation to find a mixture that is commercially available in large quantities, relatively inexpensively, and that the brew or mixture of derivatives prepared from the mixture has an effective action against colds, while having an effect on the body. which helps to withstand the increased workload and to overcome the accompanying weakness and fatigue.

Another very important element of the process according to the invention lies in the new method of preparing the herbal extract.

A method has been developed during lengthy laboratory and field experiments that avoids boiling that is commonly used in the preparation of such herbal extracts, and provides significantly better yields (100-300% increase in yields) of the active, volatile and aromatic substances compared to prior art processes. .

A reference example to illustrate the advantages of the process of the invention is also provided herein (see Example 3).

Among the analytical results supporting the increase in yield, the following are highlighted:

Yield: 60-65 ° C 60-65 ° C 80-100 ° C Adsorbent: Yes no no Example number: 1. Second Third Essential oil (mg / ml): 9.2 8.6 1.6 Flavones (mg / ml): 0.15 0.15 0:08.

The present invention relates to a process for the preparation of a herbal extract for the treatment of colds comprising 20-30% by weight of thyme, 30-40% by weight of soap root, 5-15% by weight of linden blossom, 15-25% by weight of mallow leaves, 5-15% of fennel. dried powder, if appropriate, containing known excipients,

(a) extracted by cooking in a manner known per se, or

b) Soak for 1-4 hours in water at 40-70 ° C, squeeze and / or centrifuge the resulting slurry, optionally soak again in water and re-squeeze and / or centrifuge, then concentrate the resulting press juice, optionally placing an adsorbent in the path of the exhaust gases and vapors, which is flushed with solvent at the end of concentration, and the resulting solution is combined with the remainder of the concentrate after solvent removal.

In carrying out the methods of the present invention, the herbs to be used are dried, comminuted and, if sterility problems are encountered in the manufacturing process, preferably the initial mixture is sterilized by radiation treatment. Alternatively, the finished products may be sterilized, preferably by radiation sterilization. If radiation sterilization is not used, the water-soaked mixture may be boiled or pasteurized for desiccation if desired.

In the process (a) of the present invention, the novel starting mixture is worked up in a manner known per se, for example as described in U.S. Patent No. 189,162. The concentrate thus obtained has a novel, very advantageous spectrum of action resulting from the new starting composition. This process, of course, yields a lower yield and less aroma and essential oil content than process b), but is significantly more advantageous than those known in the art.

In carrying out the process according to the invention, which is much more preferred, b) the starting mixture is swollen in 2 to 5 times its weight, preferably 3 times its weight, for 1 to 4 hours, preferably 2 to 2.5 hours. The water used in the swelling (digestion) is preferably acidic pH = 1.0-4.0). The acidification is carried out using a pharmacologically acceptable acid such as citric acid. If radiation sterilization is not used, the mixture may be boiled or pasteurized for desiccation if desired.

The temperature used during digging is a very important factor. Although yields of up to 40 ° C can be achieved which are not much worse than conventional processes, yields of 60-65 ° C yield extremely high active ingredient, volatile and aroma yields. At temperatures higher than 70 ° C, many valuable components are decomposed (these components are lost to a much greater extent in conventional processes).

After digestion, the resulting pulp is separated from the solid residues by filtration or centrifugation, and the residue is squeezed and / or subjected to vigorous centrifugation. If centrifugation is used,

It is advisable to use a speed of at least 10000 rpm. The preferred solution is pressing, in which case it is advisable to use a screw press or press extractor in this step. It is desirable to rinse the press residue (centrifugation residue) several times, preferably twice, with slightly acidic water. The resulting mixture was cooled (20-30 ° C) and filtered.

The filtrate is concentrated by vacuum evaporation to a volume of 0.1 to 0.2 volumes. In this case, too, gentle conditions are used (pressure is 6-8x10 ^{1 * 3} Pa, preferably 7x10 ^{3 *} Pa, and the temperature is 30- 10 ° C, preferably 35 ° C).

In a preferred embodiment of the present invention, an adsorbent, preferably granular activated carbon, is added in front of the cooling unit (condenser) to bind the flavoring and volatile substances. Of course, other materials suitable for solvent and temperature conditions, such as silica gel, Al ₂ O ₃ , synthetic adsorbents, and the like, may also be used as adsorbents. At the end of the distillation, the adsorbent is washed with a non-toxic organic solvent, preferably ethyl acetate. The resulting flavoring solution is also degassed under gentle conditions. The resulting aroma concentrate is blended with the main weight of the product at any stage of the refining process, preferably in the final step.

Flavorings may also be recovered by extracting flavorings from a condensed aqueous solution in the receiver.

The resulting concentrate can be converted into a formulation conventional in pharmaceutical products using methods and additives known per se. It is preferred that the resulting concentrate be lyophilized and spray dried, in which case the aroma extract may be added to the product after lyophilization.

The process of the invention will be described in more detail below.

EXAMPLE 1 g Garden thyme (Tymi vulgaris herba), g Soap root (Saponariae radix) g Lime blossom (Tiliae flos), g Marshmallow leaf (Altheae folium), G fennel (Foeniculi fructus) (the plants are used in dried form, gamma sugi) the plants are ground to a maximum particle size of 6 mm. The flour is swelled in 300 g of 0.25% strength citric acid in water at 65 ° C for a minimum of 2 hours and a maximum of 3 hours. The drug pulp is then passed through a screw press (pressurized 6.07.0 x ^{10 6} Pa). The press juice is collected (200-220 ml) and the drug is washed with 200 g, also 0.25% citric acid water, to give 140-150. The resulting extract (340-370 ml) was cooled to ambient temperature (20-25 ° C) and filtered on a Hyfo supercell filter bed (20 g) to dryness (crude and solid free). After washing with water, the wash solution is added to the filtrate (360-390 mL of solution is obtained).

A laboratory vacuum evaporator is assembled by inserting a G3 glass-bottomed tube section with a suitable abrasive (sealed) connection between the evaporator flask and the cooling condenser into which 20 g of granulated activated carbon is inserted and the vapor is passed through.

The above approx. The extract (360-390 ml) was concentrated to a volume of 65 ml on the above vacuum evaporator.

After disassembly of the vacuum evaporator, the adsorbent was washed with 50 ml of ethyl acetate at 20-25 ° C. The solution was collected in a 100 ml round-bottomed flask and the solvent removed on a Rotavapor vacuum evaporator by evaporation of the ethyl acetate. The remaining approx. Check the absence of ethyl acetate in 0.5 ml of oil by gas chromatography. If the oil is ethyl acetate free, it is added to the concentrate with stirring.

The analytical results of the 65 ml concentrate obtained above are described below.

(a) Solids content: 0,34 g / ml (calculated as 100 g of starting mixture: 22,1 g).

b) Essential oil content: 9.2 mg / ml (based on 100 g of starting mixture: 598 mg).

From the oil the following components can be detected by gas chromatography: thymol (about 3 mg / ml), carvacrol, bomeol, anethole, fenchone.

(c) Flavonide content: content of quercetin and isoquercetin, expressed in rutoside: 0,15 mg / ml (calculated on the basis of 100 g of the starting mixture: 9,75 mg).

Example 2

Starting from the composition of Example 1, and

As described in Example 1, 360-390 ml of herb-filtered herbal extract is obtained.

Concentration of the extract is carried out with the exception that no carbon adsorbent is used. Concentration is also performed by vacuum distillation (65 ml final volume). After the distillation is complete, the condensed water (ca. 300 mL) from the collecting flask is transferred to a shaking funnel and extracted with 3 x 50 mL ethyl acetate. The combined solutions were de-solvented as described in Example 1. 0.28 g of an oil is obtained which is combined with the concentrate with stirring.

The analytical results of the 65 ml concentrate obtained above are described below.

(a) Solids content: 0,34 g / ml (calculated on 100 premixes: 22,1 g).

(b) Essential oil content: 8.6 mg / ml (calculated as 100 g of starting mixture: 559 mg).

From the oil by gas chromatography azl. The components given in Example 1A can be detected.

(c) Flavonide content: content of quercetin and isoquercetin, expressed in rutoside: 0,15 mg / ml (calculated on a 100 g feed mixture: 9,75 mg).

Example 3

We start from the herb mixture of Example 1. The flour is swelled with 300 g of water for 2.5 hours and then the thick, non-agitated pulp is stirred by addition of 700 g of water. The operation is carried out in a 3 L round bottom flask, after dilution, the flask is refluxed

EN 209 998 A and heat on a flask crater. Continue heating to reflux and reflux for 15 minutes. The mixture was then cooled to 20-30 ° C and the solid was collected by filtration. The filtered material was rinsed with 200 g of water and the washing solution was combined with the filtrate. The resulting approx. Filter 980 ml of extract sharply on a 20 g Hyflo supercell filter bed. The filter bed is washed with 20 ml of water and the washing liquid is added to the extract. The resulting approx. 1000 ml of herbal extract are then concentrated on a vacuum evaporator (without adsorbent) to a volume of 65 ml.

The analytical results of the concentrate obtained as described above are described below.

(a) Solids content: 0,32 g / ml (calculated on 100 g of starting mixture: 20,8 g).

b) Essential oil content: 1.6 mg / ml (based on 100 g of the starting mixture: 104 mg).

From the oil by gas chromatography, only thymol can be detected from the components of Example 1.

(c) Flavonide content: quercetin and isoquercetin rutoside: 0,08 mg / ml (calculated as 100 g of the starting mixture: 5,2 mg).

Example 4

The preparation of Example 1 is carried out except that the initial herb mixture is not soaked but first soaked in water at room temperature, then boiled abruptly, then cooled to 60-65 ° C with cold water and the active ingredient is recovered. continued at this temperature as described in Example 1, with the additional difference that the drug pulp was separated from the solution by accelerated filtration.

Claims (5)

PATIENT INDIVIDUAL POINTS 1. A method for producing a herbal extract against colds, comprising 20-30% thyme, 30-40% saponification, 5-15% lime, 15-25% marshmallow, 5-15% by weight of dried ground meal, which may contain known excipient (s), (a) extracted by cooking, or b) soaking in water at 40-70 ° C for 1 to 4 hours, squeezing the liquid from the resulting pulp and / or centrifuging, if desired, re-soaking the residue in water and re-centrifuging and / or centrifuging and compressing the resulting slurry, if necessary. an adsorbent is introduced into the path of the exhaust gases and vapors, which is washed with a solvent at the end of the condensation, and the solution thus obtained is combined with the remainder of the thickening after solvent removal. Process according to claim 1, characterized in that an acidic, pharmacologically acceptable aqueous solution is used for soaking. 3. Process according to any one of claims 1 to 5, characterized in that in the course of soaking, water is used in an amount of 2-5 times that of the dried mill. 4. Referring to 1-3. Process according to any one of claims 1 to 5, characterized in that carbon is used as the adsorbent. 5. Process according to any one of claims 1 to 5, characterized in that ethyl acetate is used to rinse the adsorbent.