CS268538B2 - Method of fat extraction from serenoa repens fruits - Google Patents

Abstract

The extraction of drugs from oily fruits is effected using carbon dioxide in a hypercritical condition as solvent. The fruits are pref. of Serenoa repens, a small palm tree growing in the United States, N. Africa, and Spain. - The extraction is at 30-50 deg. C and 100-350 bar, the CO2 is then evaporated at 20-30 deg. C and 50-70 bar. The extract can be dehydrated e.g. by drying under vacuum at 35-85 deg. C or by using a dehydrating agent such as Na2SO4. The process is carried out in a continuous cycle.

Description

The invention also relates to a method for extracting fat from Serenoa repens.

Seronoa Beet Fruits, a small palm, growing in the United States, North Africa, have been used for a long time to produce extracts in alcohol, alcohol and water and oil, and these extracts are then used to treat pathological conditions associated with adenonene The use of Serenoa repens for this purpose has been worded for a long time and has been described, for example, in the Diepeneatory of the Unit of America *, 1988. Also known is the extraction of the drug with polar solvents and partly the qualitative and quantitative storage of the oil. gain·

More recently, French Patent Specification No. 2,480,754 has described a process for producing Serenoa repens extracts using apolar solvents, petroleum ether or halogenated hydrocarbons in the presence of an antioxidant and an inert gas atmosphere. use of inert gas in the production of the resulting product essential to prevent oxidation of aliphatic kyaalins and unsaturated alcohols whose extract contains a high percentage · The obtained extract must then be treated with activated carbon to remove undesirable components and finally dried.

It has now surprisingly been found that the oily substances of Serenoa repens are readily obtainable on an industrial scale by extracting the material with carbon dioxide from the liquid and tp conditions in a selective manner without the need for natural or eynthetic additives with stabilizing effect, the solvent itself prevents oxidation because it deprives the environment perfectly of the presence of the air · In addition, the extract obtained in this way does not need to discolour

In comparison with previously known methods, the process according to the invention has the substantial advantage of allowing complete extraction of unchanged lipid material, so that after complete evaporation of the solvent and filtration using a dshydrating agent, an extract is obtained which is free of solvent residues or non-volatile contaminants. they are usually used with solvents commonly used in industry. In addition, the extract obtained can be used directly for the manufacture of conventional pharmaceutical compositions without further purification. The products obtained can optionally be dried under vacuum at temperatures ranging from 35 to 80 ° C.

SUMMARY OF THE INVENTION The present invention provides a process for extracting fat from Serenoa repens fruits by using carbon dioxide as the extraction solvent under hypercritical conditions and extraction at a temperature of 30 to 50 ° C and a pressure of 10 to 35 MPa.

Under these operating conditions, after drying the resulting product, a yellow-orange dehydrated oil is obtained without any odor, the most volatile of which has been removed during the process according to the invention.

The resulting product thus obtained has the following physico-chemical properties:

- density 0,9,

- refractive index of approximately 1,45 at 20 ° C,

- non-aponifiable substances content of approximately 3% ·

Non-saponifiable substances consist mainly of a mixture of phytostroles, the most important of which is [J-eitosterol, and of mixtures of saturated alcohols of 20 to 30 carbon atoms in the molecule, the most important of which is octacosanol ·

Under normal conditions and e content of beta-eitosterol is in the range of 0.2 to 0.35%, the amount of n-octacosanol is in the range of 0.1 to 0.2% ·

In the oil, these alcohols and sterols are present in the form of esters with negligible amounts in the free form.

Quantitative determination of the abovementioned alcohols and sterols The gas chromatography after methanolysis and eilylalc in a capillary column is readily accomplished as described in the literature, for example by Martinelli et al, Sixth International

CS 268 538 82

Symposium on Cepillery Chromatography, Riva dal Garda, May 14 (1985) ·

In the biochemical and pharmacological tests, the oil obtained in this way has a remarkable androgenic and anti-oedemotic effect together with a hormone-regulating effect, which is convenient and indicated in the literature for similar products prepared by previously known methods.

The following examples illustrate the invention.

Example 1

In a 5 L ae extraction apparatus, extracting 1.2 kg of Serenoa repene fruit after milling at -20 ° C under heating and pressure control ·

Extraction ae is carried out for 2 hours using 10 liters of continuously circulating carbon dioxide at a temperature of 35 ° C and a pressure of 25 MPa · After evaporation of the solvent, the extracted oil is isolated and au 24 hours at 0.014 MPa and 45 ° C.

In this way 0.138 g of a clear yellow-orange oil is obtained with the following characteristics:

- density 0,096

- refractive index: 1.46.

- amount of non-aponifiable substances 2,52%

- eaponflection index 230

Free Aliphatic Acid Content 86% ·

Example 2

In a 5 L extraction apparatus, 1.2 kg of Serenoa repens fruits are extracted under heating and pressure control at -20 ° C.

The material was then extracted for 2 hours using 10 liters of continuously circulating carbon dioxide at a pressure of 22 MPa and a temperature of 45 ° C, maintaining a pressure of 5 MPa and a temperature of 25 ° C in a condensation screen.

After extraction and complete evaporation of the carbon dioxide from the condenser, the extracted oil saturated with water is isolated and filtered to 12 g of anhydrous sodium sulphate.

In this way, 145 g of a yellow-orange oil are obtained, which are dried under vacuum at 50 psi (50 psi) to completely remove water. The oil has the same properties as the oil of Example 1.

Claims (4)

Process for the extraction of fat from Serenoa repene fruit, characterized in that the extraction solvent is carbon dioxide under herercritical conditions and the extraction is carried out at a temperature between 30 and 50 ° C and at a pressure of between 10 and 35 MPa. ·. 2. A process according to claim 1, characterized in that after the extraction step the carbon dioxide is evaporated at a temperature in the range from 20 to 30 [deg.] C. and at a pressure ranging from 5 to 7 MPa. Process according to either of Claims 1 and 2, characterized in that the extract obtained can further be subjected to dehydration. 4. A method according to any one of claims 1 to 3, characterized in that the process is carried out continuously.