HU193247B - Method for producing chamomille extracts and/or ethereal oil from tetraploide chamomille sorts - Google Patents

Abstract

Alcoholic camomile extract, prepd. from the dried flowers of the tetraploid variety described in DE3423207, contains at least 5 mg% chamazulene (I); at least 15 mg% (-)-alpha-bisabolol (II) and less than 8 mg% other bisaboloids (III). Also new are ethereal oils from the same source contg. at least 5% (I), at least 15% (II) and less than 10% (III). - Dried flowers of the camomile variety 'Manzana' are extracted with an alcohol conventionally, pref. at 10-50 deg.C, using 2-20 (esp. 3-10) pts. solvent per pt. plant material. The extract pref. contains about 5.6 mg% (I) and at least 15.5 mg% (II). The ethereal oil is obtd. by boiling the dried flowers with water (pref. in presence of ascorbic acid) at pH 4-6 (pref. 5-5.5) for 2-8 hrs., using 10-50 pts. water and 0.1-1 pt. ascorbic acid per wt.pt. plant material. The aq. distillate formed is repeatedly extracted with a lower aliphatic hydrocarbon solvent, then the dried organic phase evapd.

Description

The present invention relates to a process for the preparation of chamomile extracts and / or essential oil from tetraploid chamomile varieties, which can be used to produce high levels of kamazulene and (-) - bisabolol, but also low extract bisaboloids and essential oils.

Tetraploid chamomile species with high content of both camazulene and (-) - bisabolol are known. The dried flowers of these chamomile varieties at 40 ° C shall have a dry matter content of at least 150 mg% kamazulene, at least 300 mg ° / o (-) - << - bisabolol and less than 50 mg% bisaboloid.

Experimental and industrial experience shows that extracts and essential oils of such chamomile varieties also have high content of chamazulene and (-) - K-bisabolol. Of course, the amount of these materials also depends to a large extent on the process by which the extract and essential oil are produced.

Various procedures have already been tried to perform the extraction. Of these, for example, the methods described in German Patent Nos. 2,227,292 and 2,606,961 are frequently used. The essence of these procedures is to treat the starting material, the dried flower heads, with a solvent (polar solvent, alcohol, ketone, ester) for a period of 15 minutes to 3 hours and to pH 2-6.

The common mistake of these methods, as well as of all other known methods, is that the chamomile extracts and / or ether oil obtained by their use do not contain as much carriaseulene and (-) -? 6-bisabolol as the starting material, kamazulene, and (-) -? based on the content of bisabolol. Another mistake is that the composition of the result obtained, the extract obtained and / or the essential oil is not always the same even if the same starting material is used, the result cannot be reproduced with certainty.

SUMMARY OF THE INVENTION It is an object of the present invention to provide a process for the preparation of chamomile extracts and / or ether oil from tetraploid chamomile varieties which provides at least 150 mg% kamazulene, at least 300 mg% (-) -? - bisabolol and less than 50 mg% bisaboloid Extracts and / or essential oils containing amounts of kamazulene and (-) -? - Z-bisabolol can be extracted which are not obtainable by any of the methods known hitherto, and at the same time the bisaboloid content of the extract and / or essential oil is unusually low.

SUMMARY OF THE INVENTION The present invention solves the object of the present invention by providing a process using a dried chamomile flower or a medicinal raw material derived therefrom, treating the starting material with a solvent at pH 2-6 for 15 minutes to 3 hours, and process 2 yields at least 5 mg% of kamazulene, at least 15 mg ° / o (-) - o-bisabolol and a product containing less than 8 mg% and 10 mg% of bisaboloid, characterized in that chamomile extracts for obtaining the starting material is mixed with the solvents or mixing of aqueous solvents mixture of the apparatus, the treated material in the mixing device ¹⁰ temperature is maintained with stirring at 10-15 ° C in an ether to obtain and dried camomile flowers such as salt, in particular in sodium salt in the presence of ascorbic acid, between 4 and 6, preferably between 5 and 5.5 heated to boiling with water at pH álla15 pre pot boiled for 2-8 hours, the aqueous distillate is obtained in a low aliphatic liquid hydrocarbon (for example petroleum ether, pentane, dimethyl ilbenzollal, decalin) repeatedly purged ²⁰ Juk, the organic phase is dried for example by means of sodium sulfate and the organic solvent is gently evaporated, for example in a rotary evaporator or at a temperature of 40-70 ° C, preferably 50-60 ° C.

When extracting the chamomile extract, the mixture of starting material and solvent is preferably treated in a turtle mixer, sometimes in a percolator, during extraction.

The peripheral speed of any peripheral point of the mixing device of the starting material and solvent is maintained at 1.7-2.7 m / sec during the process.

Feature of the invention ³⁵ is that each one is part of at least 2, preferably 2 to 20 parts of solvent is added gyógyáru raw material.

An ether recovery of the dried camomile vi chew _40, water and a mixture of ascorbic acid, pH is adjusted with acid, preferably hydrochloric acid.

Further, preferably, 10 to 50 parts water and optionally 0.1 to 1 part ascorbic acid are added to 1 part dried chamomile flower.

The process of the invention will now be described in detail.

Mixing devices such as turtle mixers, percolators ₅₀ and other suitable extraction devices may be used for extraction. During extraction, for example, the temperature may be between 10 ° C and 50 ° C. No cooling required.

If the extraction is carried out by means of a stirrer, the stirrer must be set so that the circumferential speed of any point on the circumference of the rotating part is between 1.7 and 2.7 m / sec, in which case the extraction time is preferably between 15 minutes and 3 hours. per person, may be between 30 and 120 minutes.

A keverömünél whose radius cm, for example a favorable application of the 50- minute -250 rpm, in which case the duration of the extraction is between 15 minutes and 3 hours, and such a size of the mixer for ⁶⁵ Gasim speed is preferably from 50 to 250 revolutions 2,193,247 lat per minute. For the latter rotation speed, a subtraction time of 15 minutes to 120 minutes may be sufficient.

Suitable solvents are straight or branched aliphatic, mono- or polyhydric alcohols having from 1 to 6 carbon atoms and a sol ketal (2-dimethyl-4-oxymethyl-1,3-dioxolane) such as methyl alcohol, ethanol, propanol (2), butyl alcohol, glycerol. and the like, and mixtures of these solvents with water.

Mixtures of these solvents may also be used. The minimum amount of solvents added to 1 ton of pharmaceutical raw material is 2 ton. Generally, 2 to 20 parts by volume of solvent, mainly 3 to 10 parts by weight, are used for 11 rosewood raw materials.

The resulting essential oil contains at least 5 mg% of kamazulene and at least 15 mg% of (-) - d - bisabolol and the bisaboloid content is less than 10 mg%.

Essentially, the essential oil is prepared by heating the dried chamomile flowers to a boiling point with, for example, ascorbic acid in the form of a salt, especially a sodium salt, at a pH of 4 to 6, preferably of 5 to 5.5. The pH is adjusted with an acid such as hydrochloric acid.

For example, 10 to 50 parts by weight of water and optionally 0.1 to 1 part by weight of ascorbic acid are used for t parts of dried chamomile flowers.

The heating is usually carried out for 2 to 8 hours.

The resultant aqueous distillation product is rinsed several times with a low aliphatic hydrocarbon (e.g. , preferably by distillation at 50-60 ° C). At higher temperatures in hot solvents, the evaporator is operated under vacuum.

Example:

200 g of camomile flowers dried at 50 ° C and sunlight were mixed with 3.6 L of water and 2 g of sodium ascorbate in a 5 L round bottom flask and adjusted to pH 5.0 with 1N HCl. After the addition of boiler stone it was heated to boiling. Within about 3 hours, about 1.2 liters of distillation product was collected.

After distillation was complete, the distillate was rinsed three times with 100-100 ml of light petroleum and dried over anhydrous sodium sulfate. The dried solution was filtered and the solvent was distilled off in a rotary evaporator. The result was 1.44 g of essential oil.

It is an advantageous feature of the process according to the invention that when starting materials of the same composition are used, the composition and content of the obtained substances are always the same, the obtained extract and / or ethereal oil have a very high content of camiazulene and (-) - Λ-bisabolol and a low bisaboloid content. moreover, the process is very economical compared to the result obtained.

Claims (6)

PATENT CLAIMS A process for the preparation of chamomile extracts and / or essential oil from tetraploid chamomile varieties using a dried chamomile flower or a medicinal raw material derived therefrom, which process comprises treating the starting raw material with a pH of 2-6 for 15 minutes to 3 hours. and yielding at least 5 mg% of kamazulene, at least 15 mg% of (-) - oC-bisabolol, and a product containing less than 8 mg% or 10 mg / o of o-bisabolol, assuming that chamomile extracts to obtain the starting material by mixing the solvents or an aqueous mixture of solvents in a mixing apparatus while maintaining the temperature of the treated material in the mixing apparatus at 10 to 50 ° C, and to obtain the ethereal oil the dried chamomile flowers in salt, mainly ascorbic acid between 6 and 6, preferably between 5 and 5, The resulting aqueous distillation product is rinsed several times with a low aliphatic liquid hydrocarbon (e.g. petroleum ether, pentane, dimethylbenzene, decane), the organic phase is dried over sodium sulfate, the organic solvent is gently evaporated, for example by rotary evaporation or by distillation at 40-70 ° C, preferably 50-60 ° C. Process according to Claim 1, characterized in that, in the extraction of chamomile extract, the mixture of starting material and solvent is preferably treated during the extraction in a turtle mixer, sometimes in a percolator. The process according to claim 1 or 2, wherein the peripheral speed of a peripheral point of the mixing device of the starting material and the solvent is maintained at 1.7-2.7 m / sec during the process. 4. Process according to any one of claims 1 to 3, characterized in that at least 2 parts by weight of solvent, preferably 2 to 20 parts by weight, are added to each 1 part by weight of the pharmaceutical raw material. Process according to Claim 1, characterized in that the pH of the mixture of dried chamomile flowers, water and ascorbic acid is adjusted with an acid, preferably hydrochloric acid, to obtain the essential oil. The method of claim 1 or 5 3.193,247, characterized in that preferably 10 to 50 parts by weight of water and optionally 0.1 to 1 part by weight of ascorbic acid are added to 1 part by weight of dried chamomile flower.