WO2013183065A2 - Extraction de produits phytochimiques à partir de matière végétale - Google Patents

Extraction de produits phytochimiques à partir de matière végétale Download PDF

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Publication number
WO2013183065A2
WO2013183065A2 PCT/IN2013/000351 IN2013000351W WO2013183065A2 WO 2013183065 A2 WO2013183065 A2 WO 2013183065A2 IN 2013000351 W IN2013000351 W IN 2013000351W WO 2013183065 A2 WO2013183065 A2 WO 2013183065A2
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Prior art keywords
plant matter
extraction
matter
nutrient
plant
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WO2013183065A3 (fr
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Ramaswamy Rajendran
Kamala Rajendran
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    • 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
    • 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)
    • A61K36/24—Apocynaceae (Dogbane family), e.g. plumeria or periwinkle
    • 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)
    • A61K36/47—Euphorbiaceae (Spurge family), e.g. Ricinus (castorbean)
    • 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)
    • A61K36/61—Myrtaceae (Myrtle family), e.g. teatree or eucalyptus
    • 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)
    • A61K36/75—Rutaceae (Rue family)
    • A61K36/752—Citrus, e.g. lime, orange or lemon
    • 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)
    • A61K36/82—Theaceae (Tea family), e.g. camellia
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30—Extraction of the material
    • A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps

Definitions

  • This invention relates to a method/process of extraction of vitamins, minerals and other phytochemicals from plant matter and more particularly to the extraction of vitamins, minerals and other phytochemicals from a first plant matter(s) by employing an alcoholic solvent, or solvent mixture, and comprising the application of one or more reacting compound(s) thereto such as to at least convert one or more of the alcoholic-solvent-insoluble nutrients(vitamins, minerals and other phytochemical constituents) therein into form(s) soluble in the alcoholic solvent, said reacting compound(s) being preferably applied in the form of acid(s)/acidic- constituent(s)-containing second plant matter(s).
  • the highlight of this invention is that by a suitable choice of the nature and concentration of the alcoholic solvent and the said acid(s)/acidic-component(s) containing second plant matter(s), an extract solution can be obtained containing all, or substantially all of the desired phytochemical constituents in a single extraction operation.
  • one of the purposes of the application of said acid acidic compound containing second plant matter(s) is to convert the one or more phytochemical constituents of interest that are insoluble in the said alcoholic solvent, or solvent mixtures, into form(s), that is into compounds, that are soluble therein thus making it possible to get substantially the entire set of desired said constituents extracted out into a single solution through a single primary extraction operation
  • the invention provides for regulating the proportions of the said constituents that are extracted out and obtained in the extract solution. This is particularly advantageous when the extraction of nutrients such as vitamins and minerals is being considered.
  • the plant species constituting said first and second plant matter(s) and the quantities thereof and the nature and concentration of the alcoholic primary extraction solvent are selected such as to get the desired set of vitamins and minerals in the desired proportions in the resulting extract.
  • One set of methods known in the prior art for the extraction and/or isolation of the said nutrients are the extraction processes that involve contacting the plant matter with solvents.
  • the solvent extracts out said nutrients by dissolution.
  • the solution(extract) containing the solvent and the dissolved nutrients therein is separated from the spent plant matter.
  • the solvent is separated from the extract solution by evaporation or other methods and the dissolved said nutrients recovered in a solid or semi-solid form. Alternatively, the nutrients are recovered in the form of a concentrated solution.
  • the said extract solution usually comprises a plurality of the plant constituents, it is referred to as a primary extract solution, or primary extract and the operation as a primary extraction.
  • the material obtained after said solvent removal whether in the form of a dilute extract, solid, semisolid or a concentrated solution is also referred to as the primary extract, extract solution or as just extract.
  • the solvent used is referred to as the primary solvent.
  • Primary extractions, extracts and solvents are also referred to as crude extractions, crude extracts and crude solvents respectively in the art.
  • Said nutrients(phytochemicals in general) in a plant matter are rarely all soluble in a single solvent.
  • Said nutrients broadly fall into groups of nutrients that can be extracted by single solvents.
  • one extraction may be carried out using water as the primary solvent to extract out the water-soluble nutrients while another may be carried out with a solvent that extracts out the fat-soluble components(nutrients) therein such as, for example, the vitamins A, D, E and .
  • a solvent that extracts out the fat-soluble components(nutrients) therein such as, for example, the vitamins A, D, E and .
  • Numerous other combinations of primary solvents are known in the art to extract out different groups of said nutrients.
  • the plant matter(s) to be extracted is treated with a suitable reacting agent(s) that is preferably in the form of acid or acidic-component-containing plant matter(s).
  • a suitable reacting agent(s) that is preferably in the form of acid or acidic-component-containing plant matter(s).
  • This treatment is carried out either prior to, or during the contacting of the plant matter to be extracted with the adopted solvent.
  • Said two plant matters are referred to as the first and second plant matter(s) respectively herein.
  • This invention provides for an alcohol solvent or an aqueous alcohol solvent.
  • alcohols have certain advantages over water.
  • the preferred solvent is aq. ethanol, the choice of which offers a combination of advantages associated with water and ethanol as solvents.
  • Said second plant matter, in the present invention may be a single plant species or a plurality thereof.
  • This invention offers the scope for developing different said combinations to serve one or more objectives such as, for example, faster extraction, more comprehensive extraction of the desired nutrient(s), reduced requirement and handling of materials such as the plant matter(s) and solvents), less processing steps, simpler flow sheet and others.
  • one or more of the solvent-soluble nutrients of the said first and second plant matter(s) are converted into forms that are more soluble in alcoholic solvents.
  • the invention offers the scope of obtaining such said converted form(s) that offer a wide range of such processing advantages, improved product properties and features and cost benefits.
  • conversion such as to make the insoluble plant nutrient(s) soluble and/or to enhance the solubilities thereof is an object of this invention.
  • conversion such as to make the inactive plant constituents) biologically or metabolically active, or to enhance said activities and efficacies is another object of the invention.
  • the features, advantages and objects of the cited invention mentioned hereinabove are also features of this invention.
  • references in the cited invention are to water-insoluble and water soluble forms whereas in the present invention the references are to forms that are soluble/insoluble in water and/or alcohols depending on whether the solvent selected is an alcohol or an aqueous alcohol.
  • Such extracts are directly administrable to subjects. They can be easily converted into different dosage forms and/or divided into suitable dosage quantities for administration to subjects. It will be observed that obtaining substantially all the targeted nutrients in the extract in substantially the targeted proportions considerably reduces subsequent processing operations required in converting the extract into the final pharmaceutical, food or nutraceutical composition formulation product.
  • a said primary extract of the invention containing the set of desired nutrients in the desired proportions is suitable for direct administration to human and animal subjects without the necessity of further processing. Conversion of the primary extract into different dosage forms suitable for different administration routes is feasible and is within the scope of the invention. Division of the primary extract into different dosage units based on RDA(Recommended Daily Allowance) quantities or other requirements and standards may be carried out within the scope of the invention.
  • first and second plant matter(s) in the present invention are not necessarily mutually exclusive.
  • Each may contain nutrient(s) of interest and the set of nutrients of interest that are extracted may come fronrone or both the sources.
  • Each said plant matter, first and second may comprise a mixture of plant matters of different species and may comprise any plant part such as leaves, fruits, roots, stems, bark, flowers, rhizomes or others, or mixtures thereof within the scope of the present invention.
  • Said acidic reagents for the acidic treatment of the plant matter may come from said first plant matter(s), in addition to said second plant matter(s) within the scope of the invention.
  • This invention provides for selection of said first and second plant matter(s) such that all, or most of the nutrients of interest are preferably obtained in the extract following a single primary extraction operation.
  • the invention further preferably provide that the extraction and yield of the nutrients of interest is enhanced/maximised, the biological and metabolic activities of the nutrients of interest are also enhanced maximised, processing times are reduced/minimised and that the nutrients of interest in the final extract are preferably in the desired proportions that are required in the projected pharmaceutical, nutrition and dietary formulations, or are close thereto such as to eliminate/minimise subsequent treatment operations such as topping-up of constituents, or addition of absent constituents, and others.
  • Alcohols are very convenient and widely used solvents for plant extractions. Ethanol is particularly versatile and widely used solvent.
  • Aqueous ethanol as also non-aq. ethanol, is a particularly convenient solvent that also happens to be a good pharmaceutically acceptable carrier.
  • Ethanol is generally edible and non-toxic, easy to handle and easy to remove from solutions where required. They are better and faster solvents for plant nutrients and dissolve a wider range of said nutrient solutes.
  • aqueous alcohols as said single primary solvents, and particularly aqueous ethanol coupled with said acid treatment of the plant matters by the present invention is novel and offers several technical advantages and cost benefits. It combines the advantages associated with both water and ethanol solvents.
  • alcoholic solvent(s) provides for the adoption of alcoholic solvent(s).
  • the term 'alcoholic solvent' is understood to be quite general as far as this specification is concerned, and includes within the scope thereof any alcohol or a solution thereof, aqueous solution or others.
  • the alcohol may be any of the aliphatic alcohols or mixtures thereof. It is further intended to include within the scope thereof, any solution of an alcohol, or of an alcohol mixture in a suitable solvent such as for example, water.
  • aqueous alcohols of all strengths are included in the scope of the term 'alcoholic solvents' of this invention.
  • the alcohol(s) in an alcohol solution of this invention may be one that is a liquid at ambient temperatures or that is solid.
  • Aqueous ethanol is the preferred solvent of the present invention.
  • the object of this invention to devise a process for the extraction of a first plant matter(s) by an alcoholic solvent and employing a second plant matter(s) that comprises reactive component(s)(compound(s)) that convert one or more of the alcoholic-solvent-insoluble nutrient(s) therein into soluble forms such that a greater range(number) of the desired plant nutrients can be extracted out through a single primary extraction operation.
  • a further object is to enhance the yield of the nutrients of interest.
  • a still further object is to provide that said soluble forms are those possessing a greater degree of biological and metabolic
  • a still further object is to convert one or more of the soluble nutrient(s) in the original plant matter into forms that are more soluble in the adopted alcoholic solvents and/or possessing a greater degree of said activity/availability.
  • a still further object of the invention is to obtain an extract that conforms to, or is close, to a desired nutrient composition/formulation as regards the components therein and the proportions thereof. Examples of such desired formulation are supplements based on RDA(Recommended Daily Allowance) values, or other medical, nutritional or dietary standards/requirements.
  • a said extraction operation may comprise a single stage or a plurality thereof.
  • extract of any concentration generated from any of said stages in the process of the invention is considered to be a product of the invention. All such extract solutions are referred to herein as primary extracts or dilute extracts. A concentrated solution obtained by the removal of solvent from such a dilute extract is also a product of this invention.
  • extracts, dilute or otherwise, solid or liquid may be further subjected to physical and/or chemical treatments) towards the production of said compositions/formulations. Products resulting from such treatments are also considered to be products of the present invention. This is elaborated further hereinbelow.
  • Examples of such further treatment of the said primary extract of the invention within the scope of the invention are: conversion of the constituents) of the solution into the form of any of the known pharmaceutical salts, conversion into forms that have enhanced metabolic and biological , efficacy and activity, conversion into different dosage forms, conversions for obtaining specific form and appearance, consistency, particle size, colour, taste, flavour, bulk, texture and other properties, addition of other nutrient(s), topping-up of nutrient(s), adaption to any of the known pharmaceutically acceptable carriers, incorporation of other food and nutrition factors such as to obtain food, dietary and nutrition supplements, pharmaceutical compositions or nutraceutical formulations, and the like.
  • said second plant matter(s) comprises acidic components(free acids and/or acidic compounds) based on one or more of the plant organic acids such as citric, tartaric, oxalic and others.
  • the treatment of said first plant matter(s) with the acidic-component containing second plant matter(s) may be carried out before the said extraction operation of the first plant matter(s) with the alcoholic solvent, or during said extraction operation, or partly in one and partly in the other.
  • contacting the two plant matter(s), said first and second, and of contacting the plant matter(s) and the solvent or solvent mixtures are within the scope of the invention.
  • said contacting may be carried out in solid or liquid phase or alternatively in a slurry phase using any of the contacting methods known in the art.
  • the process of the invention offers the scope for adjusting the parameters such as the nature and amount of said first and second plant matters and the extraction parameters to obtain an extract product containing substantially all the desired nutrient constituents in substantially the desired proportions such as, for example, the RDA figures.
  • Such an extract product can be made by the invention to be substantially close to the desired formulation such that it is suitable for administration directly to subjects. It is also easily and simply convertible into any of the known dosage forms and is a suitable intermediate therefor and for other subsequent conversion operations leading to the production of pharmaceutical, food and nutraceutical formulations/ compositions/supplements. Said adjusting can also be carried out to obtain other advantageous features/properties in the extract.
  • the process of the invention offers substantially a ready-mixed, formulation upon the removal of the solvent from the extract solution product of the invention.
  • Such nutrient mixtures are very suitable and convenient intermediates and starting points for the making of dosage form nutrient supplements. They are also suitable for easy conversion into nutraceutical formulations and food and dietary preparations and supplements.
  • the process of the invention may comprise optional additional steps such as topping-up of any nutrient that is deficient in the extract of the invention and/or addition of a nutrient that is absent in the extract but required in the formulation.
  • additives may be added to the extract of the invention for colour, appearance, flavour, taste, texture, bulk, odour or others.
  • additional optional treatment steps are within the scope of the invention to convert one or more of the nutrient constituents that are not biologically active into active forms and/or for converting one or more said nutrients that are less metabolically and biologically active into forms having greater said activity.
  • Optional steps for converting the extract into specific dosage forms are also within the scope of the invention.
  • Similar optional steps for conversion of the extract into different food and/or nutraceutical formulations are also within the scope of the invention.
  • the process of the invention makes the conventional practice of the isolation of the plant-based nutrients followed by subsequent admixing of the separated nutrients for the making of formulations, wasteful and redundant.
  • the advantages of the process of the invention for extracting nutrients from plant matters are:
  • said alcohol(s) may be any of the aliphatic alcohols which may be liquid or solid at ambient temperatures.
  • the acidic matter(s) selected for reacting with said nutrients may be in any of the following forms or combinations thereof:
  • extraction' is used herein to refer to both the overall process of extraction such as of plant matter comprising a series of steps including the actual extraction step(unit operation) involving the contact of the plant matter with the solvent or solvent mixture.
  • Said extraction step may comprise leaching, soxhlet extraction or other known means of carrying out the extraction operation. Such extractions may be carried out at room temperatures or at elevated temperatures.
  • An extraction operation may comprise a single extraction stage or a plurality thereof within the scope of the invention. The meaning appropriate to the context and offering the widest scope may be taken. It is intended herein that the scope of the term 'solvent' also covers the adoption of a solvent mixture unless otherwise specified.
  • the scope of the term includes all phytochemicals contained in the plant matter being extracted and extends to all constituents in the plant matter relevant to food, dietary, nutrition, medicinal and therapeutical considerations. Specifically, it includes vitamins and minerals, anti-oxidants, carbohydrates, proteins and fats, medicinal principles and other compounds. It also extends to factors in the plant matter such as for odour, taste, colour and others.
  • the term 'nutrients' also covers the precursors thereof, if any, present in the two plant matters.
  • the terms 'acidic components', acidic reagents' and 'acidic compounds' are intended to be interchangeable and are intended to refer to either a free acid(s) or an acidic substance(s) or both.
  • Said acidic reagents may be inorganic or organic. Use of mixtures of organic and inorganic origin acidic components is also within the scope of the invention.
  • the acidic components are in the form of plant matter.
  • the term 'reagent' is intended to mean a reactive compound herein.
  • a said extraction operation may comprise a single stage or a plurality thereof. Different flow arrangements of the various process streams such as of the incoming plant matters, the solvent, the partly and fully spent plant matters and the different streams of the extract solutions of different concentrations are feasible in multi-stage extraction operations and the same are within the scope of the invention.
  • a nutrient(sXvitamins and minerals and other phytochemicals) contained in a first plant matter(s) and a second plant matter(s), by means of an alcoholic solvent comprising providing said first and second plant matter(s), contacting the two said plant matter(s) with the said solvent or solvent mixture, separating the extract solution from the spent plant matter to yield an extract solution comprising phytochemical constituent(s) in the form(s) originally present in the said first and second plant matter(s) and/or in form(s) derived therefrom through reaction(s) with the acid(s)/acidic components) contained in the said first and/or second plant matter(s), said reaction(s) being such as to at least convert an insoluble said constituents) into a soluble form(s) and further to optionally convert a soluble said constituent(s) into a form(s) that possess greater solubility and/or convert an inactive said constituents) into a form(s) having biological and metabolic efficacy and activity and/or convert a said constituents) into
  • the extract solution obtained by the process of the invention may be subjected to solvent removal by any of the known processes such as evaporation thereof to yield a solid extract, or a semi-solid extract or a concentrated solution extract.
  • the extract product in any of the abovementioned forms may be subjected to any known complementary or supplementary treatment such as, for example, to enhance the efficacy, activity, effectiveness, biological/metabolical availability, form, colour, taste, flavour, bulk, appearance and other factors.
  • said reacting compound(s) may be acidic, alkaline or others.
  • Said compounds are preferably acidic and may be actual acids or acidic compounds. They may be any of the mineral acids(inorganic acids) or organic acids within the scope of the invention.
  • they are plant-based organic acids which may be applied to the first plant matter to be extracted either as free acids and/or in the form of plant matter or other forms.
  • the said reacting compound(s) are in the form of free plant-based organic acid(s) and/or acidic compound(s) contained in a plant matter(s) which is referred to herein as the acidic plant matter(s) or second plant matter(s).
  • the term 'acidic component' is intended to refer to both free acid(s) and/or acidic compound(s) and the meaning offering the wider scope may be taken to be applicable.
  • Said treatment with organic acids makes the one or more said alcoholic-solvent-insoluble nutrients soluble in the solvent.
  • Suitable choice of the plant-based organic acid constituents is provided such that the alcoholic-solvent solubility of one or more of the soluble nutrients is preferably enhanced through said conversion.
  • said organic acids can be partly or fully in the form of reagents.
  • suitable selection of the acidic components) containing plant matter(s) can give better yields of said nutrient components and also provide other cost benefits.
  • Suitable choice of said acid components can give said converted forms of the nutrients that are more metabolically active and absorbable.
  • Use of plant matter(s) as a source of the required acidic matter in the process of the invention in contrast to other sources is more eco-friendly.
  • this invention preferably provides for the use of plant matter(s) as the source of said acidic components). They may be complemented and/or supplemented by non-plant based acidic component(s), whether inorganic or organic or both, within the scope of the invention.
  • Said reacting compounds adopted for treatment of said first plant matters may comprise free acid(s) or acidic reagents in addition to the said acidic component(s) containing second plant matter(s) within the scope of the invention. Addition of free acids/acidic components may be carried out to complement, or supplement the action of the adopted said second plant matter(s). Said addition may be carried out before the extraction or at other points in the process of the invention.
  • the process of the invention involves applying said reacting compounds to the said first plant matter(s) that contains the nutrient(s) to be extracted.
  • the application may be in the solid state wherein the two plant matters are brought into intimate contact. Suitable size reduction and other operations on the plant matter may be carried out for better contact. Other suitable preparatory operations may be carried out on the said first and second plant matters such as cutting, chopping, dicing, crushing, grinding, cleaning, washing, drying, blanching and others, optionally as required.
  • the two plant matters may be contacted in a liquid phase comprising a suitable liquid wherein the two plant matters are dispersed.
  • Contacting may be enhanced by stirring/agitation or by fluidisation means.
  • said contacting may be at ambient temperatures and pressures or under elevated temperatures and/or pressures.
  • Hydrothermal cooking may also be adopted in the interests of better yields and faster processing and for other cost benefits.
  • Said liquid contacting phase may be any suitable liquid wherein the plant matter mixture is slurried.
  • the adopted extraction solvent may be utilised as the liquid wherein said two plant matters are brought into contact by slurrying them in the solvent.
  • said two plant matters in suitable sizes are intimately mixed and allowed time for the reaction between said acids/acidic components and the plant matter constituents.
  • a sigma blade mixer or other suitable equipment may be employed for the mixing operation. The mixing operation results in a pulpy mass. Water or other liquid may be optionally added to enhance contact of the two plant matters. After standing for some time the pulpy mixture is contacted with the alcoholic solvent. Cooking of said mass by heating with steam, or hydrothermal cooking thereof are within the scope of the invention.
  • the two plant matters may be dispersed in the alcoholic solvent, such that said conversion(s) and extraction by dissolution in the solvent proceed side-by-side.
  • the two plant matters are firstly mixed together in powder forms and then slurried in the solvent.
  • said first and second plant matters may be added to the alcoholic solvent separately in that order but addition of the two matters the other way round is also within the scope of the invention.
  • the extraction of the alcoholic-solvent-soluble components of the said first plant matter may be carried out separately prior to carrying out said reaction(s) for the conversion of the alcoholic- solvent-insoluble components, within the scope of the invention. It would be necessary then to have a second extraction operation for the extraction of the said converted nutrient(s).
  • each said first and second plant matter(s) may be a mixture of two or more species of plants.
  • Nutrient(s) in the extract may also come from the said acidic components) containing second plant matter(s) within the scope of the invention. That is, within the scope of the invention, the nutrient components from both said first and second plant matters may be extracted. Similarly, a part of the acidic component for said conversion may come from the said first plant matter(s) which may comprise some acidic components, within the scope of the invention.
  • Suitable physical treatment such as, for example, cleaning, drying, cutting, washing, pulping, crushing, grinding, powdering or other may be carried out on the said first plant matter(s) in preparation for contacting the same with the said acidic component containing second plant matter(s). If the said contacting is projected to be done in the solid phase, preferably both the said plant matters are converted into pulp form for more effective contact. Alternatively, if contacting in liquid phase is adopted, the same may be carried out by bringing together the two plant matter(s) in the powder form or juice form or in the form of a water extract or other.
  • a preferred second plant matter comprises amla fruits(Emblica officinalis)or other similar species. These are preferably pulped and the first plant matter(s) intimately mixed with the pulped amla fruit matter.
  • Other preferred acidic plant matters are anatto seed matter, tamarind fruit concentrate, and Jujube(Ziziphus jujube) fruits. Extracting the juice of the second plant matter(s) is also within the scope of the invention. Applying a fruit juice concentrate is another option provided by the invention.
  • This invention finds that amla fruits is a very versatile and advantageous source of said acidic components. Amla fruit matter offers better extraction of the nutrients with less requirement of the acidic fruit matter.
  • the panel of desired nutrients is obtained in the extract solution by means of a single extraction operation.
  • said panel may comprise all the nutrients present in the two plant matters in which case the resulting extract constitutes an essence of the two plant matters.
  • plant matter of two or more species may be combined to constitute the said first plant matter(s) and similarly the said second plant matters).
  • the solid, semisolid or concentrated extract solution product of the invention comprises the required combination of said nutrients in the required proportions and concentrations.
  • Said required combination and the amounts of the constituents may be in accordance with any of the medicinal, nutritional and other standards and specifications.
  • two or more plant species may form said second plant matter.
  • the species for the two said plant matters may be selected such that together they give the desired combinations of the said acidic reacting compounds as also of the nutrients.
  • Said first and second plant matters may comprise the roots, leaves, fruits, flowers, stems, branches, rhizomes or other plant parts or any mixture thereof within the scope of the invention.
  • a said plant matter(first or second) may provide the said nutrient(s) or said organic acid reacting components) or both.
  • the process of the invention eliminates a number of primary extraction and fractional extraction steps as also the said step of admixing the isolated nutrients for the purpose of making a formulation and simplifies the process of making nutrient mixtures.
  • the extract product of the invention is a ready intermediate for preparing the formulations and processing them into various dosage forms.
  • the only processing required as far as their nutrient content is concerned is the said topping step and the addition of missing nutrients if any.
  • the process of the invention can be easily adapted to bring out substantially the full spectrum of nutrients originally present in the plant matter extracted if desired.
  • Some of the mineral acids tried and found suitable by this invention for said conversion are: hydrochloric, sulphuric, phosphoric, nitric and perchloric acids.
  • Some of the organic acids similarly tried and found suitable for said conversion by this invention are succinic, citric, tartaric, acetic and ascorbic acids.
  • Said treatment with acidic components converts the said nutrients into salts, esters, alcohols and other compounds that are soluble in alcoholic solvents.
  • the action of the reacting compound(s) of the said second plant matter(s) may be supplemented by addition of free acids or acidic compounds at one or more stages in the process.
  • said organic acids may be added to said first plant matter(s) in reagent forms or in the form of said second plant matter(s) or both.
  • the acidic components may also come from the said first plant matter(s).
  • the process of the invention will also extract nutrients from the said second plant matters) that contains the desired organic acid components) required for said conversions. From the range of plant matter available for use as said acidic second plant matter(s), an optimum selection of one or more thereof may be made that optimally extracts the desired vitamins and minerals of said first plant matters).
  • the process of the invention offers great flexibility in selecting the plant species for the said first and second plant matters such as to maximise yields, obtain specific combinations of said nutrients, reduce processing times and material requirements and achieve other cost and material benefits.
  • the said acidic second plant matter(s) may be such that the resulting converted nutrient(s) are soluble in the adopted solvent but one or more thereof are not biologically(metabolically) active.
  • the process of the invention provides for the incorporation of a further step(s) after the extraction step wherein either the extract solution or the solid or semisolid extract is treated with a suitable reagent(s) to convert the said biologically inactive components into active forms.
  • the processing steps in the process of the invention described above are amenable to being arranged hi different combinations. It is also feasible to combine some steps. The order of the said processing steps may also be varied within the scope of the invention. Several variants of the process of the invention can be visualised by persons in the art. Such variants, orders and arrangements are within the scope of the invention.
  • the preferred solvent is aqueous ethanol which may be of any strength from about 10% v/v to about 95% v/v. More preferred is the strength range: from about 40% v/v to about 60% v/v.
  • the aq. ethanol solvent strength adopted in many of the embodiments described in detail hereinbelow is about 50% v/v.
  • This invention finds that the yield comes down as the aq. ethanol strength is reduced from the level of about 50% v/v. On the other hand, increasing the strength does not appear to have much effect on the yield which remains substantially unchanged as the aq. ethanol concentration is raised from the most preferred level of about 50% v/v.
  • said acidification of the first plant matter can be optimised with regard to yield and other considerations by a suitable choice of one or more of the abovementioned acidic- compound-containing second plant matters.
  • said first plant matter that can be extracted by the process of the invention to yield an extract containing a mixture of substantially all the vitamins and minerals therein through a single extraction with alcoholic solvents are:
  • an extract containing all the desired constituents of a formulation is a major techno-commercial advantage as several extraction steps, solvent recovery and handling steps, fractionation and partitioning steps and admixing steps of prior art processes are eliminated. These advantages can be further increased and enlarged by suitable choice of said plant matters and the acid components thereof.
  • a said plant matter labelled a first plant matter implies that its function as a nutrient source is primary while its role as a source for said acidic constituents for reacting with the said nutrient compounds is secondary.
  • a said plant matter labelled a second plant matter implies that its function as a provider of said acidic reactants is primary while its role as a nutrient source is secondary. It will be observed that said labels, primary and secondary are a formality and both roles of a plant matter may be of equal importance within the scope of the invention.
  • compositions of the extracts are in weight %(w/w) and that of the alcohol solvent in v/v aq. ethanol, unless otherwise specified.
  • four extraction procedures were followed:
  • This embodiment is a process of extraction of Trichilia connaroides with about 50% v/v aq.ethanol. Amla fruits have been adopted as the said second plant matter. The steps in the process are:
  • Blend entire batch quantity (Stainless Steel Double Cone Blender / Ribbon Blender / Octagonal Blender)
  • the extract is named Alcohol synergy extract(TASE, for short).
  • TASE Alcohol synergy extract
  • the adoption of the said second plant matter in the form of amla fruit matter produces a synergy effect leading to higher overall yield and higher yields of the nutrient components and reduced processing times.
  • TC(Trichilia connaroides) plant matter was extracted with about 50% v/v aq. ethanol but without employing said second plant matter, namely, amla fruits.
  • the steps in the procedure adopted were as above except that the amla fruit matter was not used.
  • TC matter was also extracted by water using amla fruit matter as the said second plant matter.
  • the process involved extraction of Trichilia connaroides aerial parts along with synergistic quantity of Amla fruits with water to yield an extract.
  • the process adopted for the extraction of T. connaroides with water using amla fruits as second plant matter comprised the steps of:
  • Blend entire batch quantity (Stainless Steel Double Cone Blender / Ribbon Blender / Octagonal Blender)
  • TWSE Trichilia connaroides - Water extract
  • the overall yield of the TC principles in water extraction coupled with the adoption of the acidic second plant matter, namely amla fruits was about 12% by wt.
  • the yield of the saponins and terpenes was about 12.3% by wt and about 3.9% by wt. respectively.
  • the respective figures for water extraction without the adoption of the second plant matter were: about 10%, about 8.2% and about 1.1 % by wt. respectively.
  • the extraction of Trichilia connaroides aerial parts along with synergistic quantity of Amla fruits was carried out with about 50% v/v aqueous ethanol as solvent.
  • the overall yield of the TC principles in the aq. ethanol extract together with the adoption of the acidic second plant matter, amla fruits was about 14% by wt.
  • the yield of the saponins and terpenes was about 15.6% by wt and about 5.5% by wt. respectively.
  • the respective figures for aq. ethanol extraction without the adoption of the amla second plant matter were found to be: about 8%, about 11.1% and about 4.1 % by wt. respectively.
  • the yield of saponins and terpenes in the extracts of the invention compared to said
  • amla fruit matter and Trichilia plant matter(Dried aerial parts) are found to be from about 3 kg. to about 7 kg. of amla fruit matter for about 100 kg. of Trichilia plant matter.
  • the more preferred figure is about 5 kg. of amla fruit matter for about 100 kg. of Trichilia plant matter.
  • Increasing the amla quantity beyond the upper figure of about 7 kg. does not appear to influence the nutrient yield. However, at still greater amla quantity levels, there is a fall in the nutrient yield.
  • This embodiment provides for extraction of Moringa oleifera leaves with about 50% v/v aq. ethanol.
  • the said second plant matter comprises amla fruit matter.
  • the process steps which given below are generally along the lines of corresponding processes i Example 1.
  • Blend entire batch quantity (Stainless Steel Double Cone Blender / Ribbon Blender / Octagonal Blender)
  • Moringa oleifera leaves were extracted with about 50% v/v aq. ethanol but without adopting the said second plant matter, that is, without using amla fruit matter.
  • the steps adopted are given below and are similar to the steps above for the aq. ethanol plus amla process except for the absence of amla in the latter.
  • Blend entire batch quantity (Stainless Steel Double Cone Blender / Ribbon Blender / Octagonal Blender)
  • Moringa oleifera leaves were extracted with water as the solvent and amla fruit matter as the said second plant matter by the process of the invention.
  • the process steps adopted are similar to the extraction of Moringa oleifera with aq. ethanol plus amla fruit matter except that water is substituted for aq. ethanol as the solvent.
  • Blend entire batch quantity (Stainless Steel Double Cone Blender / Ribbon Blender / Octagonal Blender)
  • Blend entire batch quantity (Stainless Steel Double Cone Blender / Ribbon Blender / Octagonal Blender)
  • Moringa oleifera extract The following table presents a comparison of the yields and the extract composition obtained with the different processes mentioned hereinabove.
  • This embodiment is a process for the extraction of green tea leaves with about 50% v/v aq. ethanol.
  • the second plant matter adopted is amla fruit matter.
  • the four process variants namely, extraction of green tea leaves with water; with water and amla fruits; with 50% v/v aq. ethanol and with 50% v/v aq. ethanol and amla system were adopted, the procedures involving water and amla fruit matter and 50% v/v aq. ethanol and amla fruit matter being the processes of the invention.
  • the processing procedure in the four systems was similar to that outlined in the corresponding procedures of Examples 1 and 2.
  • the yield was about 24% for the extract made by the process of the invention using 50% v/v aq. ethanol solvent and amla fruit matter.
  • the extract contained about 30% total polyphenols and about 18% Epigallo catechin gallate.
  • green tea leaves were extracted with the same solvent as above but without employing the second plant matter, namely, amla fruits.
  • the yield was about 18%.
  • the extract contained about 18% total polyphenols and about 6% Epigallo catechin gallate.
  • Green Tea leaves were also extracted with water and amla fruits process of the invention.
  • the yield was about 18 %.
  • the extract contained about 12% total polyphenols and about 4% Epigallo catechin gallate.
  • the extract contained about 10% total polyphenols and 3% Epigallo catechin gallate.
  • Vasaka leaves were extracted using about 50% v/v aq. ethanol as solvent and amla fruits as the said second plant matter in accordance with the invention.
  • the yield was about about 14%.
  • the total alkaloid content of the extract was found to be about 5%.
  • the productivity gain is apparent from the fact that extraction of about 1000 kgs Vasaka leaves in the aq.ethanol-amla system of the invention yielded about 140 kgs of extract as against about 80 kgs obtained with the water-amla system of the invention. In terms of saponins, the yield was observed to be about three times in the aq. ethanol-amla system of the invention.
  • Example 3 Said four process variants mentioned in Example 3 were adopted in this example. As mentioned, the processing steps are similar to those in the corresponding procedures elaborated in and referred to in Examples 1 and 2.
  • the flow sheets for the aq. ethanol-amla and the water-amla processes for the examples 3 and 4 are similar except for the difference of solvent. Processes where amla has not bee adopted are similar to their with-amla counterparts except that amla is not in the picture in the former.
  • This example covers the extraction of citrus peels by the processes, of the invention and by two processes of the prior art for comparison.
  • the four process variants as outlined in the abovementioned examples were adopted.
  • the variants are: extraction with water, extraction with water and amla plant matter(fruits), extraction with about 50% v/v aq. ethanol and with about 50% v/v aq. ethanol and amla fruit matter.
  • the procedures involving extraction with about 50% v/v aq. ethanol and amla fruit matter and with water and amla fruit matter are processes of the invention.
  • the prior art procedures were adopted to provide comparison of yields. The comparison is presented in Table ⁇ hereinbelow.
  • Table III Extraction of Folates as Folic acid from Citrus peels by the processes of the invention - Comparison of the overall yield of the phytochemicals and of folates as folic acid and of the bioflavonoids
  • Extraction Extract yield Amount of Amount of process % by wt Folates as Bioflavonoids
  • This example is of the extraction of a set of B group of vitamins.
  • the set comprises:
  • the said first plant matter comprises two plant species: Guava fruits and Holy basil leaves.
  • the second plant matter is lemon fruit peels. It may be noted that as mentioned before, the roles of the said first and second plant matters are not mutually exclusive.
  • the first batch was extracted according to the process of the invention.
  • the first plant matter was admixed with about 4 kg. lemon fruit peels which constituted said second plant matter.
  • the mixture was extracted with about 50% v/v aq. ethanol.
  • the processing steps were corresponding to the processing steps in the process of the invention adopted in the examples described hereinabove.
  • the second batch was also extracted with about 50% v/v aq. ethanol but without the use of lemon fruit peels. It will be noted that this extraction is without the adoption of said second plant matter.
  • This procedure was conducted to provide a comparison of the yields and the nutrient proportions in the extract. The processing steps in this procedure were generally similar to the steps in the corresponding procedures in the abovementioned examples.
  • the third batch was extracted with water. Lemon fruit peels were used as the said acidic second plant matter.
  • the processing steps in this procedure were generally similar to the steps in the corresponding procedures in the abovementioned examples.
  • the fourth batch was also extracted with water but without the use of said lemon fruit peels. As would be observed, second plant matter was not adopted in this extraction. The processing steps in this procedure were generally similar to the steps in the corresponding procedures in the abovementioned examples. . This extraction was also carried out to provide said comparison of yields and proportions.
  • B3 (Niacin) 39 mg/g
  • B3 (Niacin) NLT 34 mg/g
  • the extract is directly administrable to subjects. It can be easily converted into dosage units for such administration.
  • the extract is also a suitable intermediate for conversion into other dosage forms; into any of the known pharmaceutically accepted salts or coupled with any

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Abstract

Procédé/processus d'extraction par traitement d'une ou de plusieurs premières matières végétales avec un solvant alcoolique, au cours duquel lesdites premières matières végétales sont traitées avec une ou plusieurs secondes matières végétales contenant un ou plusieurs composants acides qui convertissent un ou plusieurs des constituants insolubles des premières matières végétales en formes solubles, permettant ainsi l'extraction d'une plus large gamme de constituants. Des espèces végétales contenant les substances nutritives souhaitées et les composants acides appropriés sont soumises à une réaction et à une extraction pour l'obtention d'une composition contenant les vitamines et les minéraux désirés (et/ou d'autres substances nutritives), sensiblement dans les proportions désirées, par l'intermédiaire d'une seule opération d'extraction avec un seul solvant, ce qui permet d'éliminer plusieurs étapes de traitement intervenant dans des procédés classiques. Les matières végétales acides appropriées comprennent les fruits d'amla, les zestes de citron, etc. Le solvant préféré est l'éthanol aqueux Ledit traitement acide peut être effectué avant ou pendant l'opération d'extraction. La conversion en formes présentant une solubilité améliorée et/ou une activité/efficacité biologique et métabolique accrue est également possible.
PCT/IN2013/000351 2012-06-06 2013-06-03 Extraction de produits phytochimiques à partir de matière végétale Ceased WO2013183065A2 (fr)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015187120A1 (fr) * 2014-06-02 2015-12-10 Thomas Thomas Nadackal Eau améliorée phytochimique
WO2017073473A1 (fr) * 2015-10-28 2017-05-04 太陽化学株式会社 Extrait de moringa

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7381434B2 (en) * 2003-04-08 2008-06-03 Herbalscience Llc Methods and compositions of Areca catechu
US8613910B2 (en) * 2005-07-27 2013-12-24 Merck Patent Gmbh Flavonoids as synergists for enhancing the action of self-tanning substances

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015187120A1 (fr) * 2014-06-02 2015-12-10 Thomas Thomas Nadackal Eau améliorée phytochimique
WO2017073473A1 (fr) * 2015-10-28 2017-05-04 太陽化学株式会社 Extrait de moringa
JP6200122B1 (ja) * 2015-10-28 2017-09-20 太陽化学株式会社 モリンガエキス
US10441618B2 (en) 2015-10-28 2019-10-15 Taiyo Kagaku Co., Ltd. Moringa extract

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