FR2578744A1 - New process for preparing a concentrated Hamamelis virginiana extract and its pharmaceutical and cosmetic use - Google Patents

New process for preparing a concentrated Hamamelis virginiana extract and its pharmaceutical and cosmetic use Download PDF

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Publication number
FR2578744A1
FR2578744A1 FR8503667A FR8503667A FR2578744A1 FR 2578744 A1 FR2578744 A1 FR 2578744A1 FR 8503667 A FR8503667 A FR 8503667A FR 8503667 A FR8503667 A FR 8503667A FR 2578744 A1 FR2578744 A1 FR 2578744A1
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Prior art keywords
extract
solvent
concentrated
aqueous phase
pharmaceutical
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FR8503667A
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FR2578744B1 (en
Inventor
Daniele Chausse
Daniel Jean
Jean Thebault
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VAILLANT DEFRESNE LABORATOIRE
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VAILLANT DEFRESNE LABORATOIRE
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783—Angiosperms [Magnoliophyta]
    • A61K8/9789—Magnoliopsida [dicotyledons]

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  • Life Sciences & Earth Sciences (AREA)
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  • Biotechnology (AREA)
  • Botany (AREA)
  • Engineering & Computer Science (AREA)
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  • Natural Medicines & Medicinal Plants (AREA)
  • Dermatology (AREA)
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  • Chemical & Material Sciences (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Medical Informatics (AREA)
  • Medicinal Chemistry (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Cosmetics (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The present invention relates to a process for preparing a concentrated Hamamelis virginiana extract. The process is characterised in that the ground plant is treated with about 30 times its weight of a dilute alcoholic solvent, in that all the alcohol is removed by evaporation under vacuum, in that the rich aqueous phase obtained is supplemented with 8 to 10 times its volume of an aqueous saturated saline solution, in that the precipitate formed is removed, in that this aqueous phase is extracted with a chlorine-containing solvent and in that the solvent is removed by distillation under vacuum until a dry powder is obtained. Pharmaceutical and cosmetic use.

Description

La présente invention est relative a un nouveau procédé de préparation d'un extrait concentré d'Hamamélis virginiana et a l'utilisation de cet extrait en pharmacie et en cosmétologie. The present invention relates to a new process for the preparation of a concentrated extract of witch hazel virginiana and to the use of this extract in pharmacy and in cosmetology.

L'Hamamélis est un remède populaire et est considéré comme spécifique des maladies du système veineux. Witch hazel is a popular remedy and is considered to be specific to diseases of the venous system.

On lui reconnait généralement une action décongestive, sédative et vaso-constrictive, favorisant surtout la circulation en retour. 11 est également utilisé en cosmétologie grace à son pouvoir astringent.It is generally recognized as a decongestant, sedative and vaso-constrictive action, especially promoting return circulation. It is also used in cosmetology thanks to its astringent power.

Toutefois, les effets benefiques veinotoniques de cette plante ne sont pas aussi largement utilisés comme ils le mériteraient, et ceci par suite de la faible concentration en principe actif des extraits commerciaux actuellement disponibles. Ceci est particulierement vrai en cosmétologie : il faut ajouter actuellement dans une crème de beauté par exemple, au moins 50 % de l'extrait fluide disponible pour que l'effet soit optimal, mais alors l'aspect esthétique de ces crèmes laisse à desirer et rend oes dernières invendables. D'ot la tendance de diminuer la quantité d'extrait ajoutée, au détriment, bien entendu, de l'effet thérapeutique et/ou cosmétique. However, the beneficial venotonic effects of this plant are not as widely used as they deserve, and this is due to the low concentration of active ingredient in the commercial extracts currently available. This is particularly true in cosmetology: it is currently necessary to add in a beauty cream for example, at least 50% of the fluid extract available for the effect to be optimal, but then the aesthetic appearance of these creams leaves something to be desired and makes these last unsaleable. Hence the tendency to decrease the amount of extract added, to the detriment, of course, of the therapeutic and / or cosmetic effect.

La présente invention s'est par conséquent, donné pour but de pourvoir à un procédé de préparation d'un extrait d'Hamamélis qui réponde mieux aux nécessités de la pratique, que les procédés antérieurement connus, notamment en ce qu'il permet l'obtention d'un extrait 20, 50, voire 100 fois plus concentré pour permettre de joindre à l'aspect esthétique parfait, une activité thérapeutique et cosmétologique optimale. The present invention has therefore given itself the aim of providing a process for the preparation of a witch hazel extract which better meets the needs of the practice than the previously known processes, in particular in that it allows the obtaining an extract 20, 50, or even 100 times more concentrated to allow to join to the perfect aesthetic appearance, an optimal therapeutic and cosmetological activity.

La présente invention a pour objet, un procédé de préparation d'un extrait concentré d'Hamamélis virginiana caractérisé en ce que l'on traite la plante broyée par environ 30 fois son poids d'un solvant hydro-alcoolique, en ce que l'on élimine la totalité de l'alcool par évaporation
sous vide, en ce que l'on ajoute à la phase aqueuse riche
obtenue 8 a 10 fois son volume d'une solution aqueuse
saline saturée, en ce que l'on élimine le précipité formé,
en ce que l'on extrait cette phase aqueuse par un solvant
chloré et en ce que l'on élimine le solvant par distilla
tion sous vide jusqu'à obtention d'une poudre sèche.The subject of the present invention is a process for the preparation of a concentrated extract of witch hazel virginiana, characterized in that the ground plant is treated with approximately 30 times its weight of a hydro-alcoholic solvent, in that the all alcohol is removed by evaporation
under vacuum, by adding to the rich aqueous phase
obtained 8 to 10 times its volume of an aqueous solution
saturated saline, in that the precipitate formed is removed,
in that this aqueous phase is extracted with a solvent
chlorinated and the solvent is distilled off
vacuum until a dry powder is obtained.

Cette dernière poudre obtenue permet d'avoir
des extraits aussi riches que possible et constitue la
matiere première pour toutes les préparations pharmaceu
tiques et cosmétologiques.This last powder obtained makes it possible to have
extracts as rich as possible and constitutes the
raw material for all pharmaceu preparations
ticks and cosmetology.

Selon un mode de réalisation avantageux du pro
cédé objet de la présente invention I'extractjcal se fait par percolation et l'extrait hydro-alcoolique titre envi
ron 350 en alcool.According to an advantageous embodiment of the pro
assigned object of the present invention I'extractjcal is done by percolation and hydro-alcoholic extract title envi
ron 350 in alcohol.

Conformément à l'invention, le traitement par
une solution aqueuse saline saturée s'effectue à une tem
pérature comprise entre 45 et 650 C.According to the invention, treatment with
a saturated aqueous saline solution is carried out at a time
temperature between 45 and 650 C.

Selon un autre mode de réalisation avantageux du
procédé objet de la présente invention, le solvant chloré
est constitué par du chloroforme.According to another advantageous embodiment of the
process object of the present invention, the chlorinated solvent
consists of chloroform.

L'invention sera mieux comprise à l'aide du com
plément de description qui va suivre, qui se réfère à un
exemple de préparation d'un extrait d'Hamamélis virginiana.The invention will be better understood using the com
additional description which follows, which refers to a
example of preparation of an extract of witch hazel virginiana.

I1 doit etre bien entendu toutefois, que cet exemple est donné uniquement à titre d'illustration de l'objet de l'invention, dont il ne constitue en aucune manière une limitation. It should be understood, however, that this example is given only by way of illustration of the subject of the invention, of which it in no way constitutes a limitation.

EXEMPLE DE PREPARATIQN :
Un kg de feuilles d'Hamamélis virginiana est extrait par 30 kg d'un mélange hydro-alcoolique titrant 350 alcoolique. Au bout de 2 heures de lixiviation , on filtre et on élimine l'alcool par évaporation sous vide (30 - 350 C. > . On obtient 15 litres d'une phase aqueuse à laquelle on ajoute 135 litres d'une solution aqueuse saturée de chlorure de sodium portée à 60 C. Il y a formation d'un abondant précipité que l'on élimine par filtration ou par centrifugation. On recueille la phase aqueuse limpide.EXAMPLE OF PREPARATION:
One kg of witch hazel virginiana leaves is extracted with 30 kg of a hydro-alcoholic mixture grading 350 alcoholic. After 2 hours of leaching, the mixture is filtered and the alcohol is removed by evaporation under vacuum (30 - 350 ° C.). 15 liters of an aqueous phase are obtained to which 135 liters of a saturated aqueous solution of sodium chloride brought to 60 C. An abundant precipitate is formed which is eliminated by filtration or by centrifugation, the clear aqueous phase is collected.

Apres avoir vérifié sur un échantillon de filtrat l'absence de précipitation apres addition de la solution de chlorure de sodium, on entrait en continu la phase aqueuse par du chloroforwe (3 à 4 fois le volume de la phase aqueuse). After having checked the absence of precipitation on a filtrate sample after adding the sodium chloride solution, the aqueous phase was continuously entered with chloroforwe (3 to 4 times the volume of the aqueous phase).

Les phases chloroformiques réunies sont sechées par distillation sous vide. On obtient environ 10 g. (soit 1 % par rapport au poids de la plante) d'extrait sec. The combined chloroform phases are dried by vacuum distillation. We obtain about 10 g. (i.e. 1% relative to the weight of the plant) of dry extract.

La quantité de cet extrait concentré utilisée pour la préparation de crèmes, gélules, dragées, sirops, lotions, pommades, compresses et autres formes galéniques ou cosmétiques, est de l'ordre de 0,1 % à 1 t. La dose unitaire est comprise entre 10 et 50 mg environ (forme orale) ou entre 5 et 25 mg environ (forme rectale). The quantity of this concentrated extract used for the preparation of creams, capsules, dragees, syrups, lotions, ointments, compresses and other galenical or cosmetic forms, is of the order of 0.1% to 1 t. The unit dose is between 10 and 50 mg approximately (oral form) or between 5 and 25 mg approximately (rectal form).

La poudre obtenue est de couleur brune et son identification -est réalisée à l'aide de la chromatographie sur oouche mince sur support de gel de silice HF 254 de 0,25 mm d'épaisseur. La phase mobile est constituée par de l'hexane 10 p, eau 15 p, acide acétique glacial 35 p, et pentanol 35 p. The powder obtained is brown in color and its identification is carried out using thin layer chromatography on a 0.25 mm thick HF 254 silica gel support. The mobile phase consists of hexane 10 p, water 15 p, glacial acetic acid 35 p, and pentanol 35 p.

On opère de la manière suivante
Solution essai : on dissout 0,1 g de poudre dans
10 ml d'éthanol à 950. We operate as follows
Test solution: 0.1 g of powder is dissolved in
10 ml of 950 ethanol.

Solution témoin : est constituée par du gallate d'éthyle 0,1 % dans du méthanol. Control solution: consists of 0.1% ethyl gallate in methanol.

On dépose 20 p1 de chacune de ces solutions et on révèle à l'aide d'uns solution de chlorure ferrique à 2 % dans 1'méthanol.  20 µl of each of these solutions is deposited and revealed using a 2% ferric chloride solution in methanol.

L'extrait sec d'Hamamélis présente à 254 nm une tache principale de Rf = 0,8 correspondant au gallate d'éthyle qui se colore en violet après révélation. The dry extract of Witch Hazel has at 254 nm a main spot of Rf = 0.8 corresponding to ethyl gallate which turns purple after revelation.

Sous U.V. à 360 nm, l'extrait présente une tache jaune de Rf supérieur.  Under U.V. at 360 nm, the extract has a yellow spot of higher Rf.

Ainsi que cela ressort de'ce qui précede, l'invention ne se limite nullement à ceux de ses modes de mise en oeuvre de réalisation et d'application qui viennent d'être décrits de façon plus explicite ; elle embrasse au contraire toutes les variantes qui peuvent venir à l'esprit du technicien en la matière, sans s'écarter du cadre, ni de la portée, de la présente invention.  As is apparent from the foregoing, the invention is in no way limited to those of its embodiments of implementation and application which have just been described more explicitly; on the contrary, it embraces all the variants which may come to the mind of the technician in the matter, without departing from the framework, or the scope, of the present invention.

Claims (6)

REVENDICATIONS 1. - Procédé de préparation d'un extrait concentré d'Hamamélis virginiana caractérisé en ce que l'on traite la plante broyée par environ 30 fois son poids d'un solvant hydro-alcoolique, en ce que l'on élimine la totalité de l'alcool par évaporation sous vide, en ce que l'on ajoute à la phase aqueuse riche obtenue 8 à 10 fois son volume d'une solution aqueuse saline saturée, en ce que l'on élimine le précipité formé, en ce que l'on extrait cette phase aqueuse par un solvant chloré et en ce que l'on élimine le solvant par distillation sous vide jusqu'à obtention d'une poudre sèche. 1. - Process for the preparation of a concentrated extract of Hamamelis virginiana, characterized in that the ground plant is treated with approximately 30 times its weight of a hydro-alcoholic solvent, in that all of the alcohol by evaporation under vacuum, in that one adds to the rich aqueous phase obtained 8 to 10 times its volume of a saturated aqueous saline solution, in that one eliminates the precipitate formed, in that the 'This aqueous phase is extracted with a chlorinated solvent and in that the solvent is removed by vacuum distillation until a dry powder is obtained. 2. - Procédé selon la revendication 1 caractérisé en ce que l'extraction se fait par percolation et l'extrait hydro-alcoolique titre environ 35Q en alcool. 2. - Method according to claim 1 characterized in that the extraction is done by percolation and the hydro-alcoholic extract titer about 35Q in alcohol. 3. - Procédé selon l'une quelconque des revendications 1 et 2, caractérisé en ce que le traitement par une solution aqueuse saline saturée s'effectue à une température comprise entre 45 et 650 C. 3. - Method according to any one of claims 1 and 2, characterized in that the treatment with a saturated aqueous saline solution is carried out at a temperature between 45 and 650 C. 4. - Procédé selon la revendication 1 caractérise en ce que le solvant chloré est constitué par du chloroforme. 4. - Method according to claim 1 characterized in that the chlorinated solvent consists of chloroform. 5. - Médicament contenant ou constitué par l'extrait d'Hamamélis préparé selon l'une quelconque des revendications 1 à 4. 5. - Medicament containing or consisting of the extract of Witch Hazel prepared according to any one of claims 1 to 4. 6. - Préparations cosmétiques contenant ou constituées par l'extrait d'Hamamélis préparé selon l'une quelconque des revendications 1 à 4.  6. - Cosmetic preparations containing or consisting of the witch hazel extract prepared according to any one of claims 1 to 4.
FR8503667A 1985-03-13 1985-03-13 NOVEL PROCESS FOR THE PREPARATION OF A CONCENTRATED EXTRACT OF WAMAMELIS VIRGINIANA AND USE IN PHARMACY AND COSMETOLOGY Expired FR2578744B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
FR8503667A FR2578744B1 (en) 1985-03-13 1985-03-13 NOVEL PROCESS FOR THE PREPARATION OF A CONCENTRATED EXTRACT OF WAMAMELIS VIRGINIANA AND USE IN PHARMACY AND COSMETOLOGY

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FR8503667A FR2578744B1 (en) 1985-03-13 1985-03-13 NOVEL PROCESS FOR THE PREPARATION OF A CONCENTRATED EXTRACT OF WAMAMELIS VIRGINIANA AND USE IN PHARMACY AND COSMETOLOGY

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FR2578744A1 true FR2578744A1 (en) 1986-09-19
FR2578744B1 FR2578744B1 (en) 1988-02-19

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0576936A1 (en) * 1992-07-01 1994-01-05 Dr. Willmar Schwabe GmbH & Co. Hamamelis dry extract, process for its preparation and its use as a medicine
EP0582147A2 (en) * 1992-08-03 1994-02-09 Societe Des Produits Nestle S.A. Anti-urease cosmetic or dermatologic composition
FR2849777A1 (en) * 2003-01-10 2004-07-16 Pf Medicament Stable Hamamelis extracts, obtained by extraction with hot water and concentration, useful as pharmaceutical or cosmetic agents, having e.g. antiinflammatory, wound healing and hemostatic action

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1165037A (en) * 1955-10-28 1958-10-16 Humphreys Medicine Company Method of extracting and reconstituting tincture of witch hazel
DE1149856B (en) * 1961-08-25 1963-06-06 E Holdermann Soehne Ri Method for the production of Hamamelitannin
FR2128251A1 (en) * 1971-03-05 1972-10-20 Balansard Pierre Hamamelis extract compsns - for treating cardiovascular disorders

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1165037A (en) * 1955-10-28 1958-10-16 Humphreys Medicine Company Method of extracting and reconstituting tincture of witch hazel
DE1149856B (en) * 1961-08-25 1963-06-06 E Holdermann Soehne Ri Method for the production of Hamamelitannin
FR2128251A1 (en) * 1971-03-05 1972-10-20 Balansard Pierre Hamamelis extract compsns - for treating cardiovascular disorders

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0576936A1 (en) * 1992-07-01 1994-01-05 Dr. Willmar Schwabe GmbH & Co. Hamamelis dry extract, process for its preparation and its use as a medicine
EP0582147A2 (en) * 1992-08-03 1994-02-09 Societe Des Produits Nestle S.A. Anti-urease cosmetic or dermatologic composition
EP0582147A3 (en) * 1992-08-03 1994-08-24 Nestle Sa Anti-urease cosmetic or dermatologic composition
FR2849777A1 (en) * 2003-01-10 2004-07-16 Pf Medicament Stable Hamamelis extracts, obtained by extraction with hot water and concentration, useful as pharmaceutical or cosmetic agents, having e.g. antiinflammatory, wound healing and hemostatic action

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Publication number Publication date
FR2578744B1 (en) 1988-02-19

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