CA2008135A1 - Process for the complex extraction of plant materials and use of the extracts and residues obtained - Google Patents
Process for the complex extraction of plant materials and use of the extracts and residues obtainedInfo
- Publication number
- CA2008135A1 CA2008135A1 CA002008135A CA2008135A CA2008135A1 CA 2008135 A1 CA2008135 A1 CA 2008135A1 CA 002008135 A CA002008135 A CA 002008135A CA 2008135 A CA2008135 A CA 2008135A CA 2008135 A1 CA2008135 A1 CA 2008135A1
- Authority
- CA
- Canada
- Prior art keywords
- extraction
- extracting
- extracted
- optionally
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Abandoned
Links
Landscapes
- Medicines Containing Plant Substances (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
PROCESS FOR THE COMPLEX EXTRACTION OF PLANT MATERIALS AND USE OF THE EXTRACTS AND RESIDUES OBTAINED A b s t r a c t The invention relates to a process for the complex extraction of the useful ingredients of fresh, frozen or dried plant materials by extraction, which comprises optionally pretreating the fresh, frozen or dried plant materials or their mixtures after a suitable purification and crushing, then extracting once or several times with an extracting agent taken in a 1 to 40-fold, particularly 1 to 20-fold weight ratio, optionally by using additives and before at least one extraction stage, digesting the plant material to be extracted by streaming steam, vapour of aqueous acid or solvent vapour through the plant material or by boiling it with water, aqueous acid or a solvent in a microwave oven and when a dried plant material is used wetting the material with the agent to be employed for digestion before the digestion, and immediately separating the extract from the plant material extracted after each stage of the extraction, optionally adjusting the pH of the mixture to be extracted to the desired value in the separate stages of extraction and/or optionally adding a reducing agent to the mixture and/or optionally using deionized or distilled water in all operations and using the same or different extracting solvent(s) in the succesive stages of the extraction. The extracts, concentrates or other preparations thus obtained are utilized as: active ingredients in human and veterinary pharmaceutical compositions; flavouring and/or colouring agents in food products or fodders; active ingredients and/or colouring agents in cosmetic compositions; or for the preparation of compositions of the paint industry.
Description
Z008~S
PROCESS FOR THE COMPLEX EXTRACTION OF PLANT MATERIALS
AND USE OF THE EXTRACTS AND RESIDUES O~TAINED
" '.~ ' ', . ':
This invention relates to a process for the complex extraction of useful ingredients of fresh, frozen or dried plant materials or of their mixtures and to the use of the extracts and residues obtained. -More particularly, the invention concerns the successive or simultaneous extraction of biologically active substances such as vitamin C, therapeutically active ingredients, amino acids, colouring and flavouring agents and carbohydrates being present in the plant as well as to the use of the extracts and residues obtained as ~ -ingredients in the food and paint industries, therapeutics cosmetics or fodders.
The extraction of the above plant materials is known;
such processes have been described in many literary references.
It has been reported in several cases of the known processes that a great part of vitamin C and flavours are lost in the course of washing, soaking and preheating;
and 8 to 50% thereof get lost even at room temperature ~
tK. Kubst et al.: Konzerv-Paprikaipar 5, 121 (1976); A. Jin ~ ~ -et al.: Skipin Kexue (Beijing) 43, 20 (1983)/.
The adjustment of the pH value of 4.3 to 4.5 is suggested in the Hungarian patent specification No. 182,514 for preserving the colour and vitamin content of vegetables.
A cell burst by gas diffusion under a high pressure in the presence of carbon dioxide and nitrogen oxide is suggested for the preparation of apple and hip juices in the Hungarian patent specification No. 186,512. The fruit is premoistened or presoaked.
According to a process described in the Hungarian ~ x~
patent specification No. 186,495 the fruit juices are obtained by using an extracting agent of pH 3.26 value to 67618-10257 G~
~ r~
d s: ' ' ' " " ' : ' ' ' , , , . . ~ . ' . ., ~
" .
gether with enzymes promoting the decomposition.
If using the known processes decompositions occur in the material to be extracted or a part of the useful substances cannot be extracted.
Thus, the object of the present invention is to ~ -avoid these drawbacks and to provide a more efficient fùrther developed complex process for extracting the useful ingredients of plant materials than the known ones.
The invention is based on the recognition that several biologically active ingredients, plant constituents which are believed to be decomposed by heat treatment such as vitamin C or several essential amino acids, flavours and colouring agents, are not decomposed even on higher temperatures within a short time period; indeed, it is necessary to carry out one or more heat-treatment of a short period in combination with known extraction processes -~
for recovering these substances with a suitable efficiency.
At least one of the heat-treatments should be carried out in such a way that the material to be extracted is penetrat- ~-ed by steam or vapours of an aqueous acidic solution, e.g.
by vapour of formic or hydrochloric acid solution used also for the extraction, or by vapour of a solvent. This can be accomplished by streaming the vapour of the above -~
solutions or solvents through the plant material, however, it has been found that an equivalent result can be achieved if the plant material is mixed with the above extracting agents and is boiled in a microwave oven for 10 to 20 minutes. ir.i~.
The invention is further based on the recognition that the extractSare to be separated from the plant residue extracted immediately after the extraction, since otherwise the ingredients di-ssolved are adsorbed on the solid material whereby the efficiency of the extraction is decreased.
The invention is based on the further recognition that the recovery of colouring agents can be improved by carrying out an additional extraction with an apolar ;
organic solvent following the recovery with common aqueous or alcoholic extractions. -The invention is further based on the recognition that the efficiency of extraction of the active ingredients, ;
particularly of vitamin C and of colouring agents can be -improved by reducing the additives used in the process before their use and/or employing reagents of analytical grade as well as using deionized or distilled water as extracting agent.
The invention is based further on the recognition that by extracting vitamin C-containing plant materials together with flavonoid- and/or hydroquinone-containing plant materials the extract obtained has a higher vitamin C
content than the total vitamin C content of the extracts obtained by separate extractions of the components; and the stability of vitamin C in these solutions is higher ;-~
in comparison to that of vitamin C in a solution containing no flavonoid and/or hydroquinone.
The invention is further based on the recognition ~ ~ -that essential amino acids such as lysine, methionine and cysteine being present in the plant material but being otherwise partially decomposed during extraction, are stable if the plant material is treated by formic acid vapours preceding the extraction, like this after oxida~
tion with hydrogen peroxide the plant material can be extracted without decomposition.
The process according to the invention comprises ~ ;
30 optionally pretreating the fresh, frozen or dried plant -materials or their mixtures after a suitable purification and crushing, then extracting once or several times with an extracting agent taken in a 1 to 40-fold, particularly -1 to 20-fold weight ratio, optionally by using additives 35 and before at least one extraction stage, digesting the ~
, ;' plant material to be extracted by streaming steam, vapour of aqueous acid or solvent vapour through the plant material or by boiling it with water, aqueous acid or a solvent in a microwave oven and when a dried plant material is used wetting the material with the agent to be employed for digestion before the digestion, and immediately separating the extract from the plant material extracted after each stage of the extraction, optionally adjusting the pH of the mixture to be extracted to the desired value 10 in the separate stages of extraction and/or optionally -adding a reducing agent to the mixture and/or optionally ~ -using deionized or distilled water in all operations and using the same or different extracting solvent(s) in the -successive stages of the extraction.
"Pretreatment" as used herein means first of all the activation of one or more own enzyme(s) of the plant .
which enzyme(s) can influence the extraction of the active ingredients and constituents. The pretreatment is carried out by ensuring the suitable temperature and pH value during the time required.
Fermentation may also be used as a pretreatment; ;~
after a fermentation of 5 to 14 days some of the active r~
ingredients become easier to be extracted.
"Extraction" as used herein means extraction in its 25 widest meaning such as soaking, stirring or treating in a -blender with an extracting agent or using countercurrent extraction with solvent, percolation, Soxhlet extraction, boiling or steaming in a Papin's pot or treating in micro-wave oven and the like. In opposition to the usual practice, ~ the first extraction in the percolation and Soxhlet extrac-tion is carried out for at least 15 to 20 minutes, then the extracting agent is separated whereby due to the separation of enzymes decomposing the active ingredient the recovery of the active ingredient is increased.
As extracting agents the ~ollowing are used: water, : ' '.':
. . ~ , .. ,~ , .
,,", ~,.,"~, ,,, ," ,-,,, ,,,,,,,sj.,.,,,,.,,, , . " ". " ,;," " , ., ", , , . ., , : , , : , ~ , : ` . ,. : .
2008~35 preferably deionized water, optionally salt, acid or base solutions or buffer solutions and/or organic solvents, e.g.: petroleum ether; chlorinated hydrocarbons; ethers;
ketones such as acetone; esters such as ethyl acetate;
5 or aliphatic alcohols. --~
Suitable salts are e.g. sodium hydrogen carbonate, sodium chloride, potassium chloride, calcium chloride or magnesium chloride. These salts are components of buffer solutions and, on the other hand, they stabilize the colouring agents. Sodium metabisulfite, potassium metabi~
sulfite or sodium thiosulfate can be employed as antioxi-. .~.
dants.
As additives added to the extracting agent, prefer-ably analytical-grade or reduced sugars, sugar solutions (e.g. glucose, lactose, saccharose, maltose, ribose, invert sugar or honey) are employed. Glycerol, propylene glycol and aliphatic alcohols, preferably ethanol or ethanol~
-containing foodstuffs such as wine may also be considered as additives.
The object of the use of the additives listed above is to break up (loosen) the plant cells and to promote thereby the dissolution of the useful ingredients.
Suitable reducing or pH-adjusting agents are vitamin C, lemon juice, acids of the citrate cycle, fumaric, tartaric, --25 malic, lactic, succinic, glucuronic, sulfurous, formic, -acetic, propionic and phosphoric acid or hydrogen chloride.
The extracts obtained may be: preserved by steriliza- ~ ~;
tion or by adding reducing agents and/or preservatives or antioxidants; flavoured by adding flavouring agents; mixed 30 with each other to achieve a desired combination of effects; ---adsorbed on a solid carrier or mixed therewith after evaporation. ~-Suitable preservatives and antioxidants are e.g.
potassium sorbate, sorbic acid, benzoic acid, sodium benzoate,-propylene glycol, polysorbate 80, propyl gallate, "~ , ' ', :' ' ' -' '.
. ' ' ..
fatty acids, L-epicatechin as well as propolis and extracts of poplar bud and of berry of Hippophae rhamnoides L.
The extracts may be directly employed or converted -to jellies or pulverized products.
The extracts obtained can be utilized in the food and paint industries, or as ingredients of therapeutics, -cosmetics and fodder materials.
The main advantage of the process according to the invention consists in that the constituents of the plant ~ -, lû material are extracted with a higher efficiency than that achieved by using known processes. -~
The invention is illustrated in detail by the follow~
ing non limiting Examples. ;
Example 1 Preparation of iuices rich in vitamin C
lûûû g of mixed fresh fruits (hip, raspberry, straw-berry, apple, mango and the like) is treated with steam of lûû C for 5 minutes, then crushed, mixed with 500 9 20 of deionized water of 100 C for 15 minutes and filtered.
The residue is repeatedly stirred for 15 minutes at 100 C
with 500 9 of water containing 30% of glucose and 10% of glycerol, filtered and the residue is again steamed at 100 C for 2 minutes, stirred with deionized water for 5 ~ ~;
minutes and again filtered. The combined extract is adjusted to a pH value between 4 and 4.5 by adding lemon juice and citric acid. After adding 0.5 kg/10 litres of honey and settling for 8 hours, it is filtered on a drum filter under reduced pressure and sterilized at 95 to 105 ~
for 20 minutes.
The juice obtained can be used as a soft drink or concentrated (thickened) to a jam or lyophilized and employed in a pulverized form for flavouring sweets or as an ingredient in cosmetics or medicaments.
-2008~35 ~ ~
Example 2 Recovery of anthocYans. flavonoids and carotenoids 200 9 of raspberries, 200 9 of bilberries, 200 9 of pritamin paprikas, 200 9 of carrots, 200 9 of black currants, 200 9 of red beets, 200 9 of hips, 200 9 of apple skins, 50 9 of peonypbetals and 50 9 of red rose petals are washed with water containing carbon dioxide, then homogenized and blended in an electric blender for 15 minutes with 12 litres of ethanol containing 30 9 of concentrated hydrochloric acid. The extraction is repeated with ethanol containing 30 9 of hydrochloric acid, the mixture is filtered, the filtrate is evaporated under reduced pressure and the plant residue is extracted with the steam of 1000 9 of water at 100 C, stirred with 8 volumes of water at 100 C for 15 minutes, then filtered and pressed. The residue is boiled with 4 volumes of water in a Papin's pot for 3 hours, filtered as hot and pressed.
The residue is extracted with 5 volumes of petroleum ether to obtain the colouring agents in a known manner. The -~
aqueous filtrates are combined and after evaporation water is added to the residue until complete dissolution. Then, the proteins and polysaccharides are precipitated from the solution by adding 10 volumes of ethanol, the ethanolic part is distilled and the destillate is added to the above 25 ethanolic hydrochloric acidic extract, the combined solvent ~;~
phase is evaporated under reduced pressure and the residue containing anthocyans is recrystallized from alcohol.
The mixture of anthocyans is capable to regenerate the rhodopsin, relieves the haemorrhage of eyes, inhibits the thrombogenesis, protects against coronary constriction induced by vasopressin and improves the cardiac function;
in addition, it exerts a favourable wound-healing effect.
The mixture of polysaccharides and the anthocyans isolated from the extract are useful either separately or together for diminishing inflammations and enhancing -` Z008~35 the resistance of capillaries.
The above active ingredients are also suggested for healing and preventing the crepuscular blindness of diabetic patients, for healing ulcers as well as for the :~
treatment of vascular diseases, arterioschlerosis and veinous vasculitis; they have been suggested for the prevention of gastric ulcer, too. ~ ~
The above extract is a face skin-regenating, vitamin- ~ --rich flavouring agent thus, it may be used in cosmetic preparations, too.
To the precipitate containing the mixture of poly-saccharides and proteins, 30-fold amount by weight of an 8 : 1 by volume mixture of 80% formic acid and 30% hydrogen ~ -peroxide is added, the mixture is heated to the boiling ~ -point in a microwave oven, and boiled to dry; then due to its high protein content the dry residue is used as an additive in foodstuffs, e.g. in roborating mixtures or in fodders. -Example 3 Preparation of an extract with a high vitamin and protein (cysteine~ methionine and lYsine) content A mixture of plant materials rich in vitamin-C, i.e. 200 9 each of poplar buds, pollens, lemon juices, hips, paprikas, tomatoes, carrots, cabbages, red beets, Hippophae rhamnoides L., elderblossoms, and garlics is crashed, stirred with 2400 9 of 80% formic acid up to homogeneous distribution, steamed under a pressure of .
PROCESS FOR THE COMPLEX EXTRACTION OF PLANT MATERIALS
AND USE OF THE EXTRACTS AND RESIDUES O~TAINED
" '.~ ' ', . ':
This invention relates to a process for the complex extraction of useful ingredients of fresh, frozen or dried plant materials or of their mixtures and to the use of the extracts and residues obtained. -More particularly, the invention concerns the successive or simultaneous extraction of biologically active substances such as vitamin C, therapeutically active ingredients, amino acids, colouring and flavouring agents and carbohydrates being present in the plant as well as to the use of the extracts and residues obtained as ~ -ingredients in the food and paint industries, therapeutics cosmetics or fodders.
The extraction of the above plant materials is known;
such processes have been described in many literary references.
It has been reported in several cases of the known processes that a great part of vitamin C and flavours are lost in the course of washing, soaking and preheating;
and 8 to 50% thereof get lost even at room temperature ~
tK. Kubst et al.: Konzerv-Paprikaipar 5, 121 (1976); A. Jin ~ ~ -et al.: Skipin Kexue (Beijing) 43, 20 (1983)/.
The adjustment of the pH value of 4.3 to 4.5 is suggested in the Hungarian patent specification No. 182,514 for preserving the colour and vitamin content of vegetables.
A cell burst by gas diffusion under a high pressure in the presence of carbon dioxide and nitrogen oxide is suggested for the preparation of apple and hip juices in the Hungarian patent specification No. 186,512. The fruit is premoistened or presoaked.
According to a process described in the Hungarian ~ x~
patent specification No. 186,495 the fruit juices are obtained by using an extracting agent of pH 3.26 value to 67618-10257 G~
~ r~
d s: ' ' ' " " ' : ' ' ' , , , . . ~ . ' . ., ~
" .
gether with enzymes promoting the decomposition.
If using the known processes decompositions occur in the material to be extracted or a part of the useful substances cannot be extracted.
Thus, the object of the present invention is to ~ -avoid these drawbacks and to provide a more efficient fùrther developed complex process for extracting the useful ingredients of plant materials than the known ones.
The invention is based on the recognition that several biologically active ingredients, plant constituents which are believed to be decomposed by heat treatment such as vitamin C or several essential amino acids, flavours and colouring agents, are not decomposed even on higher temperatures within a short time period; indeed, it is necessary to carry out one or more heat-treatment of a short period in combination with known extraction processes -~
for recovering these substances with a suitable efficiency.
At least one of the heat-treatments should be carried out in such a way that the material to be extracted is penetrat- ~-ed by steam or vapours of an aqueous acidic solution, e.g.
by vapour of formic or hydrochloric acid solution used also for the extraction, or by vapour of a solvent. This can be accomplished by streaming the vapour of the above -~
solutions or solvents through the plant material, however, it has been found that an equivalent result can be achieved if the plant material is mixed with the above extracting agents and is boiled in a microwave oven for 10 to 20 minutes. ir.i~.
The invention is further based on the recognition that the extractSare to be separated from the plant residue extracted immediately after the extraction, since otherwise the ingredients di-ssolved are adsorbed on the solid material whereby the efficiency of the extraction is decreased.
The invention is based on the further recognition that the recovery of colouring agents can be improved by carrying out an additional extraction with an apolar ;
organic solvent following the recovery with common aqueous or alcoholic extractions. -The invention is further based on the recognition that the efficiency of extraction of the active ingredients, ;
particularly of vitamin C and of colouring agents can be -improved by reducing the additives used in the process before their use and/or employing reagents of analytical grade as well as using deionized or distilled water as extracting agent.
The invention is based further on the recognition that by extracting vitamin C-containing plant materials together with flavonoid- and/or hydroquinone-containing plant materials the extract obtained has a higher vitamin C
content than the total vitamin C content of the extracts obtained by separate extractions of the components; and the stability of vitamin C in these solutions is higher ;-~
in comparison to that of vitamin C in a solution containing no flavonoid and/or hydroquinone.
The invention is further based on the recognition ~ ~ -that essential amino acids such as lysine, methionine and cysteine being present in the plant material but being otherwise partially decomposed during extraction, are stable if the plant material is treated by formic acid vapours preceding the extraction, like this after oxida~
tion with hydrogen peroxide the plant material can be extracted without decomposition.
The process according to the invention comprises ~ ;
30 optionally pretreating the fresh, frozen or dried plant -materials or their mixtures after a suitable purification and crushing, then extracting once or several times with an extracting agent taken in a 1 to 40-fold, particularly -1 to 20-fold weight ratio, optionally by using additives 35 and before at least one extraction stage, digesting the ~
, ;' plant material to be extracted by streaming steam, vapour of aqueous acid or solvent vapour through the plant material or by boiling it with water, aqueous acid or a solvent in a microwave oven and when a dried plant material is used wetting the material with the agent to be employed for digestion before the digestion, and immediately separating the extract from the plant material extracted after each stage of the extraction, optionally adjusting the pH of the mixture to be extracted to the desired value 10 in the separate stages of extraction and/or optionally -adding a reducing agent to the mixture and/or optionally ~ -using deionized or distilled water in all operations and using the same or different extracting solvent(s) in the -successive stages of the extraction.
"Pretreatment" as used herein means first of all the activation of one or more own enzyme(s) of the plant .
which enzyme(s) can influence the extraction of the active ingredients and constituents. The pretreatment is carried out by ensuring the suitable temperature and pH value during the time required.
Fermentation may also be used as a pretreatment; ;~
after a fermentation of 5 to 14 days some of the active r~
ingredients become easier to be extracted.
"Extraction" as used herein means extraction in its 25 widest meaning such as soaking, stirring or treating in a -blender with an extracting agent or using countercurrent extraction with solvent, percolation, Soxhlet extraction, boiling or steaming in a Papin's pot or treating in micro-wave oven and the like. In opposition to the usual practice, ~ the first extraction in the percolation and Soxhlet extrac-tion is carried out for at least 15 to 20 minutes, then the extracting agent is separated whereby due to the separation of enzymes decomposing the active ingredient the recovery of the active ingredient is increased.
As extracting agents the ~ollowing are used: water, : ' '.':
. . ~ , .. ,~ , .
,,", ~,.,"~, ,,, ," ,-,,, ,,,,,,,sj.,.,,,,.,,, , . " ". " ,;," " , ., ", , , . ., , : , , : , ~ , : ` . ,. : .
2008~35 preferably deionized water, optionally salt, acid or base solutions or buffer solutions and/or organic solvents, e.g.: petroleum ether; chlorinated hydrocarbons; ethers;
ketones such as acetone; esters such as ethyl acetate;
5 or aliphatic alcohols. --~
Suitable salts are e.g. sodium hydrogen carbonate, sodium chloride, potassium chloride, calcium chloride or magnesium chloride. These salts are components of buffer solutions and, on the other hand, they stabilize the colouring agents. Sodium metabisulfite, potassium metabi~
sulfite or sodium thiosulfate can be employed as antioxi-. .~.
dants.
As additives added to the extracting agent, prefer-ably analytical-grade or reduced sugars, sugar solutions (e.g. glucose, lactose, saccharose, maltose, ribose, invert sugar or honey) are employed. Glycerol, propylene glycol and aliphatic alcohols, preferably ethanol or ethanol~
-containing foodstuffs such as wine may also be considered as additives.
The object of the use of the additives listed above is to break up (loosen) the plant cells and to promote thereby the dissolution of the useful ingredients.
Suitable reducing or pH-adjusting agents are vitamin C, lemon juice, acids of the citrate cycle, fumaric, tartaric, --25 malic, lactic, succinic, glucuronic, sulfurous, formic, -acetic, propionic and phosphoric acid or hydrogen chloride.
The extracts obtained may be: preserved by steriliza- ~ ~;
tion or by adding reducing agents and/or preservatives or antioxidants; flavoured by adding flavouring agents; mixed 30 with each other to achieve a desired combination of effects; ---adsorbed on a solid carrier or mixed therewith after evaporation. ~-Suitable preservatives and antioxidants are e.g.
potassium sorbate, sorbic acid, benzoic acid, sodium benzoate,-propylene glycol, polysorbate 80, propyl gallate, "~ , ' ', :' ' ' -' '.
. ' ' ..
fatty acids, L-epicatechin as well as propolis and extracts of poplar bud and of berry of Hippophae rhamnoides L.
The extracts may be directly employed or converted -to jellies or pulverized products.
The extracts obtained can be utilized in the food and paint industries, or as ingredients of therapeutics, -cosmetics and fodder materials.
The main advantage of the process according to the invention consists in that the constituents of the plant ~ -, lû material are extracted with a higher efficiency than that achieved by using known processes. -~
The invention is illustrated in detail by the follow~
ing non limiting Examples. ;
Example 1 Preparation of iuices rich in vitamin C
lûûû g of mixed fresh fruits (hip, raspberry, straw-berry, apple, mango and the like) is treated with steam of lûû C for 5 minutes, then crushed, mixed with 500 9 20 of deionized water of 100 C for 15 minutes and filtered.
The residue is repeatedly stirred for 15 minutes at 100 C
with 500 9 of water containing 30% of glucose and 10% of glycerol, filtered and the residue is again steamed at 100 C for 2 minutes, stirred with deionized water for 5 ~ ~;
minutes and again filtered. The combined extract is adjusted to a pH value between 4 and 4.5 by adding lemon juice and citric acid. After adding 0.5 kg/10 litres of honey and settling for 8 hours, it is filtered on a drum filter under reduced pressure and sterilized at 95 to 105 ~
for 20 minutes.
The juice obtained can be used as a soft drink or concentrated (thickened) to a jam or lyophilized and employed in a pulverized form for flavouring sweets or as an ingredient in cosmetics or medicaments.
-2008~35 ~ ~
Example 2 Recovery of anthocYans. flavonoids and carotenoids 200 9 of raspberries, 200 9 of bilberries, 200 9 of pritamin paprikas, 200 9 of carrots, 200 9 of black currants, 200 9 of red beets, 200 9 of hips, 200 9 of apple skins, 50 9 of peonypbetals and 50 9 of red rose petals are washed with water containing carbon dioxide, then homogenized and blended in an electric blender for 15 minutes with 12 litres of ethanol containing 30 9 of concentrated hydrochloric acid. The extraction is repeated with ethanol containing 30 9 of hydrochloric acid, the mixture is filtered, the filtrate is evaporated under reduced pressure and the plant residue is extracted with the steam of 1000 9 of water at 100 C, stirred with 8 volumes of water at 100 C for 15 minutes, then filtered and pressed. The residue is boiled with 4 volumes of water in a Papin's pot for 3 hours, filtered as hot and pressed.
The residue is extracted with 5 volumes of petroleum ether to obtain the colouring agents in a known manner. The -~
aqueous filtrates are combined and after evaporation water is added to the residue until complete dissolution. Then, the proteins and polysaccharides are precipitated from the solution by adding 10 volumes of ethanol, the ethanolic part is distilled and the destillate is added to the above 25 ethanolic hydrochloric acidic extract, the combined solvent ~;~
phase is evaporated under reduced pressure and the residue containing anthocyans is recrystallized from alcohol.
The mixture of anthocyans is capable to regenerate the rhodopsin, relieves the haemorrhage of eyes, inhibits the thrombogenesis, protects against coronary constriction induced by vasopressin and improves the cardiac function;
in addition, it exerts a favourable wound-healing effect.
The mixture of polysaccharides and the anthocyans isolated from the extract are useful either separately or together for diminishing inflammations and enhancing -` Z008~35 the resistance of capillaries.
The above active ingredients are also suggested for healing and preventing the crepuscular blindness of diabetic patients, for healing ulcers as well as for the :~
treatment of vascular diseases, arterioschlerosis and veinous vasculitis; they have been suggested for the prevention of gastric ulcer, too. ~ ~
The above extract is a face skin-regenating, vitamin- ~ --rich flavouring agent thus, it may be used in cosmetic preparations, too.
To the precipitate containing the mixture of poly-saccharides and proteins, 30-fold amount by weight of an 8 : 1 by volume mixture of 80% formic acid and 30% hydrogen ~ -peroxide is added, the mixture is heated to the boiling ~ -point in a microwave oven, and boiled to dry; then due to its high protein content the dry residue is used as an additive in foodstuffs, e.g. in roborating mixtures or in fodders. -Example 3 Preparation of an extract with a high vitamin and protein (cysteine~ methionine and lYsine) content A mixture of plant materials rich in vitamin-C, i.e. 200 9 each of poplar buds, pollens, lemon juices, hips, paprikas, tomatoes, carrots, cabbages, red beets, Hippophae rhamnoides L., elderblossoms, and garlics is crashed, stirred with 2400 9 of 80% formic acid up to homogeneous distribution, steamed under a pressure of .
2 atmospheres for 10 minutes, then stirred with 8 volumes of water at 100 C in a boiling water bath for 15 minutes, filtered, the solid residue is heated to the boiling point with 4 volumes of water in a microwave oven, boiled for 20 minutes, then filtered, mixed again with 4 volumes of ;,~
,. ., ~. :
water and then the boiling in the microwave oven is repeated for 20 minutes. The combined aqueous extracts ::: . : ~: .:
:; '''' ~ ~' ~
.. . .. .... .. . ..
2008~35 ::
_ 9 _ are concentrated to 500 ml, treated with 500 ml of 30%
H202, evaporated again and the residue is mixed in se or together with the solid plant residues with starch, cellulose, zeolite or with a salt mixture; or after partial evaporation the combined extracts are adsorbed on starch, cellulose or zeolite and the product is used as a fodder mixture. --~
Example 4 -Preparation of lemon juice from the flesh and peel of lemon -1000 9 of whole lemons in 200 ml of water is boiled in a microwave oven for 10 minutes, then peeled, the inner juice-rich part made free from the white part is pressed, 15 the juice is separated, the fibrous residue is heated ;
to ~the boiling point with 8 volumes of water, then filtered -~
and pressed. The crushed lemon peel is added to the solid residue and the operation is repeated, except that the -heating in this step is by all means carried out in a 20 microwave oven for 10 minutes. After filtering as hot and ;
pressing, the native lemon juice and lemon extract are combined and sterilized. As preservative 0.1 9 of potassium sorbate is used for 1000 ml of product.
, ExamPle 5 Recovery of lanatoside AOC from Digitalis lanata folia~e 10 9 of dried and ground plant material is steamed with water at 100 C, then cooled to 80 C and stirred 30 with 80 9 of methanol for 20 minutes. The solvent is sucked -~
off and the extraction is repeated with stirring for 20 minutes with 40 9 of methanol. The extract is filtered, the residue is pressed and the solid material is subjected to a repeated extraction. The extracts are evaporated, the 35 residue is dissolved in 30 9 of a phosphate buffer (pH 7.4) ~ ,--, ~ ,:
and extracted 3 times with a 3:1 mixture of chlorform/methanol at the boiling point of the solvent mixture. The extracts are combined, evaporated and the lanatoside ABC residue is ~
recrystallized from methanol.
Example 6 Recoverv of di~oxin from Digitalis lanata foliage 100 9 of dried and, ground plant material is sieved through a sieve with diameter of openings of 0.8 to 1.2 mm -and is soaked in 800 ml of water at a pH value of 5.5 to -6 at 45 C for 72 hours, then the extract is filtered, the ;
residual plant material is pressed, the solid residus is vigorously stirred with an isotonic phosphate buffer solu~
tion of pH 7.4 for 25 minutes, then is filtered and pressed.
The residue is steamed with the vapours of 100 ml of water for 10 minutes, then warmed to 100 C with 4 volumes of a buffer solution of pH 7.4 and kept on this temperature -for 15 minutes, then it is filtered and pressed. The separate -extracts are evaporated, the residues are shaken with a H~
,. ., ~. :
water and then the boiling in the microwave oven is repeated for 20 minutes. The combined aqueous extracts ::: . : ~: .:
:; '''' ~ ~' ~
.. . .. .... .. . ..
2008~35 ::
_ 9 _ are concentrated to 500 ml, treated with 500 ml of 30%
H202, evaporated again and the residue is mixed in se or together with the solid plant residues with starch, cellulose, zeolite or with a salt mixture; or after partial evaporation the combined extracts are adsorbed on starch, cellulose or zeolite and the product is used as a fodder mixture. --~
Example 4 -Preparation of lemon juice from the flesh and peel of lemon -1000 9 of whole lemons in 200 ml of water is boiled in a microwave oven for 10 minutes, then peeled, the inner juice-rich part made free from the white part is pressed, 15 the juice is separated, the fibrous residue is heated ;
to ~the boiling point with 8 volumes of water, then filtered -~
and pressed. The crushed lemon peel is added to the solid residue and the operation is repeated, except that the -heating in this step is by all means carried out in a 20 microwave oven for 10 minutes. After filtering as hot and ;
pressing, the native lemon juice and lemon extract are combined and sterilized. As preservative 0.1 9 of potassium sorbate is used for 1000 ml of product.
, ExamPle 5 Recovery of lanatoside AOC from Digitalis lanata folia~e 10 9 of dried and ground plant material is steamed with water at 100 C, then cooled to 80 C and stirred 30 with 80 9 of methanol for 20 minutes. The solvent is sucked -~
off and the extraction is repeated with stirring for 20 minutes with 40 9 of methanol. The extract is filtered, the residue is pressed and the solid material is subjected to a repeated extraction. The extracts are evaporated, the 35 residue is dissolved in 30 9 of a phosphate buffer (pH 7.4) ~ ,--, ~ ,:
and extracted 3 times with a 3:1 mixture of chlorform/methanol at the boiling point of the solvent mixture. The extracts are combined, evaporated and the lanatoside ABC residue is ~
recrystallized from methanol.
Example 6 Recoverv of di~oxin from Digitalis lanata foliage 100 9 of dried and, ground plant material is sieved through a sieve with diameter of openings of 0.8 to 1.2 mm -and is soaked in 800 ml of water at a pH value of 5.5 to -6 at 45 C for 72 hours, then the extract is filtered, the ;
residual plant material is pressed, the solid residus is vigorously stirred with an isotonic phosphate buffer solu~
tion of pH 7.4 for 25 minutes, then is filtered and pressed.
The residue is steamed with the vapours of 100 ml of water for 10 minutes, then warmed to 100 C with 4 volumes of a buffer solution of pH 7.4 and kept on this temperature -for 15 minutes, then it is filtered and pressed. The separate -extracts are evaporated, the residues are shaken with a H~
3:1 mixture of chloroform/methanol and the digoxin is re-crystallized from methanol. ;~
The lanatoside ABC and digoxin content were determinedby using the method described in: Europaisches Arzneibuch I, page 274; or: Deutsches Arzneibuch, Amtliche Ausgabe 25 Deutscher Apotheker Verlag, Stuttgart, Gori Verlag GmbH, ;
Frankfurt 1986, Ed. 9, page 730.
Exame~ 7 , ~ : `
Recoverv of the total alkaloids from Chinae cortex -~
100 9 of dried and ground plant material falling-~
through on a sieve with diameter of openings of 0.8 to 1.2 mm is heated together with 250 9 of water and 100 ml of a 50%
methanolic trichloroacetic acid solution twice to boiling in a microwave oven. The mixture is allowed to cool, then is mixed with 300 ml of concentrated ammonia .-, , ~, : ", 20()8135 solution and extracted with benzene in a Lorincz-Szasz ~ .
type alkaloid-extracting equipment. The extract is extracted twice each with 100 ml of û.2 mol/litre sulfuric acid solution then is alkalinized up to pH 9-10 by adding ;
6 mol/litre ammonia solution, is extracted 3 times each with 100 ml of chloroform, then evaporated. The residue is recrystallized from ethanol.
Example B -Recovery of k-strophanthoside from Strophanthi semen 100 9 of ground plant material falling through on a sieve with diameter of openings of 0.8 to 1.2 mm is steamed ;
at 100 C for 10 minutes, then extracted 3 times each with 400 ml of ethanol, filtered and pressed. The ethanolic parts are combined, evaporated and after adding 100 ml of water the residue is extracted 3 times with a 3:1 mixture of chloroform/methanol. After evaporation of the combined chloroform/methanol extracts the solution is evaporated and the residue is recrystallized from ethanol to obtain k-strophanthoside.
Example 9 Recoverv of solasodine from Solanum laciniatum ~ 8 5.00 9 of powdered Solanum laciniatum plant material falling through on a sieve with diameter of openings of 0.8 to 1.2 mm is steamed at 100 C for 10 minutes, then extracted with 100 ml of 80% aqueous methanol under stirring for 15 minutes and pressed. The solid residue is extracted 30 with 300 ml of 80% aqueous methanol in a Soxhlet equipment for 3 hours and the combined extracts are evaporated. 200 ml of 5N hydrochloric acid is added to the residue and the mixture is hydrolyzed on a water bath for 3 hours. After adjusting the pH value of the hydrolysate to 9 to 10 with ~ ~
35 5N sodium hydroxide solution, the mixture is extracted with ; ~ ~-~: . .
n-heptane, the solvent phase is evaporated and the residue :
is recrystallized from n-hexane. ~:
, .
Table 1 ; :
Recovery of vitamin C from hips by using various ~ ~ -extracting agents and processes .
Vitamin C content was determined according to the 10 method described in: Pharmacopoea Hungarica VII., Medicina ~ :: -Konyvkiado, Vol. III, page 1603 (1986).
The highest recovery of vitamin C (table 1, process 5) is considered to be lûû%; the other results are related to this value.
Extracting solvent, Recovery Total recovery :~
temperature (duration % of vitamin C ,i, of the extraction) %
._ ._ .. . .. _ . .. ' ,"',.' i ,' 2û 1. Deionized water, 25 C 13.52 Deionized water, 25 C 11.03 89.6]. -,~
(20 min) Deionized water, 100 C 65.06 -.. -,.-^,- -(20 min) ,-~. ,:.:-. .-25 2. Deionizgd water, standing 20.21 at 100 C (2û min) Deioniz&d water, standing 13.01 95.6 ..
at 100 C (20 min) Deionized water, 100 C 62.74 in microwave oven (10 min) 3. Deionized water, 100 C 52.74 (20 min) . ,~
Deionized water, boiled on 26.50 ~4.24 a water bath (20 min) Deionized water, boiled on 15.0 . .:--a water bath (20 min) .- ~ -. .. : . : ~:
": ':" :' ~ """ '" ~', i''' " , ' ' ' ~"' ' ' ' ,'','''"'.'' "' '' '.'' ' Extracting solvent, Recovery Total recovery of .
temperature (duration % vitamin C :.
of the extraction) % .
.. ._ .,,:
5 4. Deionized water, boiled 52.59 - , .-. .--over a gas flame at 100 C
(20 min) Deionized water, boiled 25.56 92.95 over a gas flame at 100 C
(20 min) Deionized water, boiled 14.8 : -over a gas flame at 100 C
(20 min) :
5. PretOeatment with steam of 100 C for 5 minutes Deiogized water, boiled at 57.06 100 C (15 min) DeioOized water, boiled at 33.B0 100.00 100 C (20 min) :~
Deiogized water, boiled at 9.14 100 C (20 min) 6. Deionized water, boiled in a 20.21 .
microwave oven (3 min) Deionized water, boiled in a 13.01 97.96 microwave oven (3 min) Deionized water, boiled in a 64.74 microwave oven (10 min) 7. 10% glucose solution 12.48 :~
conOaining 0.9% of NaCl, 25 C (20 min) ::~
10% glucose solution 12.40 77.37 conOaining 0.9% of NaCl, .
25 C (20 min) 10% glucose solution 52.49 containOng 0.9% of NaCl, at 100 C in a microwave oven (10 min) . .
~ .
.. .: ~
.,",, ,,. ,; .,, ~,, .:; ., ",,, ,"~ ,, ",, , .,~ "", ,,., ", ..... ...
, " "," "",~ , ", ~ :- , , ,, , , " ~,"" " , ~ -. :
Extracting solvent, Recovery Total recovery of temperature (duration % vitamin C
of the extraction) %
. . . _ _ _ . . . _ _ .
8. 5% citric acid solution 10.38 containing 0.9% of NaCl saturated by C0~ (C0 is generated by adding ~aHC03 to Ohe acidic solution) C (20 min) 5% citric acid solution8.62 71.73 containing 0.9% of NaCl ~ --saturated by C0 (C0 is generated by ad~ing ~aHC03 -- ~
to ~he acidic solution) : ~ -25 UC (20 min) -~
5% citric acid solution52.73 -~
containing 0.9% of NaCl saturated by C0 (C0 is .~: -generated by ad~ing ~aHC03 to thOe acidic solution) --100 C in a microwave oven (10 min) 9. 3% Ocetic acid solution,9.48 25 C (20 min) 3%.Ocetic acid solution,8.21 53.19 25 C (20 min) 3% agetic acid solution,35.5 ~~;
100 C in a microwave ~ -`
oven (10 min) . ~ -It is obvious from the data of the above Table 1 that the treatment by steam or treatment in a microwave oven, respectively, as well as the use of deionized water ~.;
as extracting solvent are favourable. ~ ; -: :
,~ "' ' ' ". " ' ~ ' ' . ,' ' ' ,. ' ' ~ ' . .
Table 2 ~, , Percentage increase in the recovery of active ingredient by using steaming or treatment in a -microwave oven according to the invention, consider- -ing the active ingredient extracted frnm the un-treated plant material as 100% (except of the above ~:
treatment the extraction of each sample is carried out in a manner known per se) Plant material Active ingredient Increase in the amount examined of active ingredient SteamOing at ~oiling by 100 C for microwave :-10 min trleOtmient for ; ~;
Cynosbati pseudofructus vitamin C 20 15.6 dry material content 20 18 :~
Malus pumila auct. vitamin C 25 20.8 :~
Lycopersica esculentum vitamin C 15 10.8 carotenoids 10 8 Citrus limonum vitamin C 25 20 Capslci fructus vitamin C 15 14 carotenoids 8 B
Ribes nigrum total flavonoids26 24.5 dry material content Chamomillae anthodium dry material content 15 14.5 30 Lini semen dry material content 20.2 20 vaccinium myrtilli anthocyanidines 19.5 18.2 Verbasci flos total flavonoids 5 4.6 dry material content 20 20 ~ ~ :~
35 Tiliae flos dry material content 20.5 18.8 Sambuci ilos total flavonoids35 33 :~
,"",~,~", ~ ," .,s,,,~
Z0081~5 : ., Plant material Active ingredient Increase in the amount examined of active ingredient : ~
SteaOming at Boiling by ~ ~:
100 C for microwave ~::
lû min treatment for 10 min :-%
Chinae cortex total alkaloids expressed 30 25.5 , ,.
as quinine base Ipecacuanhae radix t~tal alkaloids expressed 25.0 23 as emetine base Secale cornutum ergotamine content B
Solanum laciniatum total terpenes as 22 lB
solasodine Digitalis lanatae lanatozide ABC 43.06 41.6 fol. "'~
Strophanthi semen k-strophanthoside 40.82 lB.l9 :::~
Amsonia species tabersonine 15 15 Chelidonium majus sanguinarine 18 Sophora japonica rutin 37.5 ' ' "
Table 3 Re-binding of active ingredients to the plant material ::~
(The recovery of the active ingredient is performed accord~
ing to Example 5, except that the plant material is not treated with steam; the rebinding is investigated after the step stirring with methanol) - : ~
~ ~
. .
, .:
Z008~35 , Plant extracted Active ingredient (lanatoside A8C) Recovery content measured %
-,,. ,:. ", . . .
Digitalis lanata foliage ~ :-~
Standing between ex-traction and separation ., - . , ,, ~
5 min 2.88 o/oo 67.28 - ;
15 min 3.92 o/oo 91.98 ~ -20 min 4.28 o/oo 100 40 min 3.37 o/oo 85.74 1 hour 3.52 o/oo 82.24 ,, : ~
The examinations were carried out by using an Elektronika (Soviet Union) microwave oven and a Janetzky centrifuge. ~ :
The quantitative determinations of the active ;~
ingredients were performed according to the methods described in the references cited hereinafter.
1. Pharmacopoea Hungarica VII. Volumes I to III, Medicina Konyvkiado, Budapest 1986:
Volume I: Chromatographic Determinations page 180: HPLC determinations pages 213 to 21a and 394 to 395: determination of alkaloids page 3a9: examinations of plant materials , -: . ~
page 390: determination of the extracted substances page 397: determination of ethereal oils.
Volume III:
page 1593: quantitative determination of Chinae ~
cortex ~-. ~
~"~''"'"~
page 1603: quantitative determination of ;
Cynosbati pseudofructus - :~
page 1673: determination of the total flavonoid -content.
2. Arzneibuch der Deutschen Demokratischen Republik 2nd Ed., Volume III, Akademie Verlag, Berlin 1975 Digitalis lanata foliage: determination of digoxin and lanatoside ABC
Digitalis purpurea foliage: determination of digitoxin 3. Deutsches Arzneibuch, 9th Ed. l9a6; Amtliche Ausgabe 1986 page 730: Digitalis lanata foliage: determination of digoxin ; ~ ~-
The lanatoside ABC and digoxin content were determinedby using the method described in: Europaisches Arzneibuch I, page 274; or: Deutsches Arzneibuch, Amtliche Ausgabe 25 Deutscher Apotheker Verlag, Stuttgart, Gori Verlag GmbH, ;
Frankfurt 1986, Ed. 9, page 730.
Exame~ 7 , ~ : `
Recoverv of the total alkaloids from Chinae cortex -~
100 9 of dried and ground plant material falling-~
through on a sieve with diameter of openings of 0.8 to 1.2 mm is heated together with 250 9 of water and 100 ml of a 50%
methanolic trichloroacetic acid solution twice to boiling in a microwave oven. The mixture is allowed to cool, then is mixed with 300 ml of concentrated ammonia .-, , ~, : ", 20()8135 solution and extracted with benzene in a Lorincz-Szasz ~ .
type alkaloid-extracting equipment. The extract is extracted twice each with 100 ml of û.2 mol/litre sulfuric acid solution then is alkalinized up to pH 9-10 by adding ;
6 mol/litre ammonia solution, is extracted 3 times each with 100 ml of chloroform, then evaporated. The residue is recrystallized from ethanol.
Example B -Recovery of k-strophanthoside from Strophanthi semen 100 9 of ground plant material falling through on a sieve with diameter of openings of 0.8 to 1.2 mm is steamed ;
at 100 C for 10 minutes, then extracted 3 times each with 400 ml of ethanol, filtered and pressed. The ethanolic parts are combined, evaporated and after adding 100 ml of water the residue is extracted 3 times with a 3:1 mixture of chloroform/methanol. After evaporation of the combined chloroform/methanol extracts the solution is evaporated and the residue is recrystallized from ethanol to obtain k-strophanthoside.
Example 9 Recoverv of solasodine from Solanum laciniatum ~ 8 5.00 9 of powdered Solanum laciniatum plant material falling through on a sieve with diameter of openings of 0.8 to 1.2 mm is steamed at 100 C for 10 minutes, then extracted with 100 ml of 80% aqueous methanol under stirring for 15 minutes and pressed. The solid residue is extracted 30 with 300 ml of 80% aqueous methanol in a Soxhlet equipment for 3 hours and the combined extracts are evaporated. 200 ml of 5N hydrochloric acid is added to the residue and the mixture is hydrolyzed on a water bath for 3 hours. After adjusting the pH value of the hydrolysate to 9 to 10 with ~ ~
35 5N sodium hydroxide solution, the mixture is extracted with ; ~ ~-~: . .
n-heptane, the solvent phase is evaporated and the residue :
is recrystallized from n-hexane. ~:
, .
Table 1 ; :
Recovery of vitamin C from hips by using various ~ ~ -extracting agents and processes .
Vitamin C content was determined according to the 10 method described in: Pharmacopoea Hungarica VII., Medicina ~ :: -Konyvkiado, Vol. III, page 1603 (1986).
The highest recovery of vitamin C (table 1, process 5) is considered to be lûû%; the other results are related to this value.
Extracting solvent, Recovery Total recovery :~
temperature (duration % of vitamin C ,i, of the extraction) %
._ ._ .. . .. _ . .. ' ,"',.' i ,' 2û 1. Deionized water, 25 C 13.52 Deionized water, 25 C 11.03 89.6]. -,~
(20 min) Deionized water, 100 C 65.06 -.. -,.-^,- -(20 min) ,-~. ,:.:-. .-25 2. Deionizgd water, standing 20.21 at 100 C (2û min) Deioniz&d water, standing 13.01 95.6 ..
at 100 C (20 min) Deionized water, 100 C 62.74 in microwave oven (10 min) 3. Deionized water, 100 C 52.74 (20 min) . ,~
Deionized water, boiled on 26.50 ~4.24 a water bath (20 min) Deionized water, boiled on 15.0 . .:--a water bath (20 min) .- ~ -. .. : . : ~:
": ':" :' ~ """ '" ~', i''' " , ' ' ' ~"' ' ' ' ,'','''"'.'' "' '' '.'' ' Extracting solvent, Recovery Total recovery of .
temperature (duration % vitamin C :.
of the extraction) % .
.. ._ .,,:
5 4. Deionized water, boiled 52.59 - , .-. .--over a gas flame at 100 C
(20 min) Deionized water, boiled 25.56 92.95 over a gas flame at 100 C
(20 min) Deionized water, boiled 14.8 : -over a gas flame at 100 C
(20 min) :
5. PretOeatment with steam of 100 C for 5 minutes Deiogized water, boiled at 57.06 100 C (15 min) DeioOized water, boiled at 33.B0 100.00 100 C (20 min) :~
Deiogized water, boiled at 9.14 100 C (20 min) 6. Deionized water, boiled in a 20.21 .
microwave oven (3 min) Deionized water, boiled in a 13.01 97.96 microwave oven (3 min) Deionized water, boiled in a 64.74 microwave oven (10 min) 7. 10% glucose solution 12.48 :~
conOaining 0.9% of NaCl, 25 C (20 min) ::~
10% glucose solution 12.40 77.37 conOaining 0.9% of NaCl, .
25 C (20 min) 10% glucose solution 52.49 containOng 0.9% of NaCl, at 100 C in a microwave oven (10 min) . .
~ .
.. .: ~
.,",, ,,. ,; .,, ~,, .:; ., ",,, ,"~ ,, ",, , .,~ "", ,,., ", ..... ...
, " "," "",~ , ", ~ :- , , ,, , , " ~,"" " , ~ -. :
Extracting solvent, Recovery Total recovery of temperature (duration % vitamin C
of the extraction) %
. . . _ _ _ . . . _ _ .
8. 5% citric acid solution 10.38 containing 0.9% of NaCl saturated by C0~ (C0 is generated by adding ~aHC03 to Ohe acidic solution) C (20 min) 5% citric acid solution8.62 71.73 containing 0.9% of NaCl ~ --saturated by C0 (C0 is generated by ad~ing ~aHC03 -- ~
to ~he acidic solution) : ~ -25 UC (20 min) -~
5% citric acid solution52.73 -~
containing 0.9% of NaCl saturated by C0 (C0 is .~: -generated by ad~ing ~aHC03 to thOe acidic solution) --100 C in a microwave oven (10 min) 9. 3% Ocetic acid solution,9.48 25 C (20 min) 3%.Ocetic acid solution,8.21 53.19 25 C (20 min) 3% agetic acid solution,35.5 ~~;
100 C in a microwave ~ -`
oven (10 min) . ~ -It is obvious from the data of the above Table 1 that the treatment by steam or treatment in a microwave oven, respectively, as well as the use of deionized water ~.;
as extracting solvent are favourable. ~ ; -: :
,~ "' ' ' ". " ' ~ ' ' . ,' ' ' ,. ' ' ~ ' . .
Table 2 ~, , Percentage increase in the recovery of active ingredient by using steaming or treatment in a -microwave oven according to the invention, consider- -ing the active ingredient extracted frnm the un-treated plant material as 100% (except of the above ~:
treatment the extraction of each sample is carried out in a manner known per se) Plant material Active ingredient Increase in the amount examined of active ingredient SteamOing at ~oiling by 100 C for microwave :-10 min trleOtmient for ; ~;
Cynosbati pseudofructus vitamin C 20 15.6 dry material content 20 18 :~
Malus pumila auct. vitamin C 25 20.8 :~
Lycopersica esculentum vitamin C 15 10.8 carotenoids 10 8 Citrus limonum vitamin C 25 20 Capslci fructus vitamin C 15 14 carotenoids 8 B
Ribes nigrum total flavonoids26 24.5 dry material content Chamomillae anthodium dry material content 15 14.5 30 Lini semen dry material content 20.2 20 vaccinium myrtilli anthocyanidines 19.5 18.2 Verbasci flos total flavonoids 5 4.6 dry material content 20 20 ~ ~ :~
35 Tiliae flos dry material content 20.5 18.8 Sambuci ilos total flavonoids35 33 :~
,"",~,~", ~ ," .,s,,,~
Z0081~5 : ., Plant material Active ingredient Increase in the amount examined of active ingredient : ~
SteaOming at Boiling by ~ ~:
100 C for microwave ~::
lû min treatment for 10 min :-%
Chinae cortex total alkaloids expressed 30 25.5 , ,.
as quinine base Ipecacuanhae radix t~tal alkaloids expressed 25.0 23 as emetine base Secale cornutum ergotamine content B
Solanum laciniatum total terpenes as 22 lB
solasodine Digitalis lanatae lanatozide ABC 43.06 41.6 fol. "'~
Strophanthi semen k-strophanthoside 40.82 lB.l9 :::~
Amsonia species tabersonine 15 15 Chelidonium majus sanguinarine 18 Sophora japonica rutin 37.5 ' ' "
Table 3 Re-binding of active ingredients to the plant material ::~
(The recovery of the active ingredient is performed accord~
ing to Example 5, except that the plant material is not treated with steam; the rebinding is investigated after the step stirring with methanol) - : ~
~ ~
. .
, .:
Z008~35 , Plant extracted Active ingredient (lanatoside A8C) Recovery content measured %
-,,. ,:. ", . . .
Digitalis lanata foliage ~ :-~
Standing between ex-traction and separation ., - . , ,, ~
5 min 2.88 o/oo 67.28 - ;
15 min 3.92 o/oo 91.98 ~ -20 min 4.28 o/oo 100 40 min 3.37 o/oo 85.74 1 hour 3.52 o/oo 82.24 ,, : ~
The examinations were carried out by using an Elektronika (Soviet Union) microwave oven and a Janetzky centrifuge. ~ :
The quantitative determinations of the active ;~
ingredients were performed according to the methods described in the references cited hereinafter.
1. Pharmacopoea Hungarica VII. Volumes I to III, Medicina Konyvkiado, Budapest 1986:
Volume I: Chromatographic Determinations page 180: HPLC determinations pages 213 to 21a and 394 to 395: determination of alkaloids page 3a9: examinations of plant materials , -: . ~
page 390: determination of the extracted substances page 397: determination of ethereal oils.
Volume III:
page 1593: quantitative determination of Chinae ~
cortex ~-. ~
~"~''"'"~
page 1603: quantitative determination of ;
Cynosbati pseudofructus - :~
page 1673: determination of the total flavonoid -content.
2. Arzneibuch der Deutschen Demokratischen Republik 2nd Ed., Volume III, Akademie Verlag, Berlin 1975 Digitalis lanata foliage: determination of digoxin and lanatoside ABC
Digitalis purpurea foliage: determination of digitoxin 3. Deutsches Arzneibuch, 9th Ed. l9a6; Amtliche Ausgabe 1986 page 730: Digitalis lanata foliage: determination of digoxin ; ~ ~-
4. The Dispensatory of the United States of America 25th Edition J. B. Lippincott Company, Philadelphia Montreal 1950.
5. Kommentar zur Pharmacopoea Helvetica Editio Sexta, Selbstverlag des Schweizerischen Apotheker-Vereins, ;~
Bern, 1975
Bern, 1975
6. European Pharmacopoea I-II. Council of Europa, Maisonneuve S. A. France 1971
7. 8ritish Pharmacopoea 1973 ,
Claims (11)
ROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. Process for the complex extraction of the utilizable ingredients of fresh, frozen or dried plant materials, which c o m p r i s e s optionally pretreating the fresh, frozen or dried plant materials or their mixtures after a suitable purification and crushing, then extracting once or several times with an extracting agent taken in a 1 to 40-fold, particularly 1 to 20-fold weight ratio, optionally by using additives and before at least one extraction stage, digesting the plant material to be extracted by streaming steam, vapour of aqueous acid or solvent vapour through the plant material or by boiling it with water, aqueous acid or a solvent in a microwave oven and when a dried plant material is used wetting the material with the agent to be employed for digestion before the digestion, and immediately separating the extract from the plant material extracted after each stage of the extraction, optionally adjusting the pH of the mixture to be extracted to the desired value in the separate stages of extraction and/or optionally adding a reducing agent to the mixture and/or optionally using deionized or distilled water in all operations and using the same or different extracting solvent(s) in the succesive stages of the extraction.
2. A process as claimed in claim 1 for the prepara-tion of extracts rich in vitamin C, which c o m p r i s e s using deionized or distilled water as extracting agent, employing reduced auxiliaries for promoting the digestion, carrying out the extraction after steaming the material to be extracted, or, if desired, after one or two cold or hot extraction(s), boiling it with deionized water in a microwave oven or extracting it after boiling in a microwave oven.
3. A process as claimed in claim 1 for the recovery of anthocyans, polysaccharides and colouring substances, which c o m p r i s e s extracting the suitably pretreated raw material with ethanolic hydrochloric acid, treating the residue with steam and extracting with water, then extracting the solid residue remaining after the aqueous extraction with petroleum ether and recovering protein and polysaccharides from the aqueous filtrates; colouring substances from the petroleum ether extract and anthocyans from the ethanolic hydrochloric acid extract.
4. A process as claimed in claim 1, which c o m p r i s e s using deionized or distilled water as extracting agent.
5. A process as claimed in claim 1 for the prepara-tion of an extract rich in vitamins, proteins and free amino acids, which c o m p r i s e s steaming the suitably pretreated raw materials with vapours of aqueous formic acid, extracting with water, boiling the solid residue once or several times with water in a microwave oven, filter-ing the extract and after oxidation, preferably after a treatment with hydrogen peroxide partially or completely evaporating the solution obtained and adsorbing it onto or mixing it with a carrier, preferably onto or with a carbohydrate-base substance or zeolite.
6. A process as claimed in claim 1 for the recovery of lanatoside ABC from the foliage of Digitalis lanata, which c o m p r i s e s treating the ground plant material by steam, pressing the solid residue and, if desired, repeating this operation, evaporating the extracts, taking up the residue in a buffer, extracting it with a 3:1 mixture of chloroform/methanol, evaporating the extracts and re-crystallizing the residue from methanol.
7. Use of the preparations prepared by using the process according to claim 1 as active ingredients of human and veterinary pharmaceutical compositions.
8. Use of the preparations prepared by using the process according to claim 1 for enriching, flavouring and/or colouring food products.
9. Use of the preparations prepared by using the process according to claim 1 for enriching, flavouring and/or colouring fodders.
10. Use of the preparations prepared by using the process according to claim 1 as active ingredients and/or colouring agents of cosmetic compositions.
11. Use of the preparations prepared by using the process according to claim 1 for the preparation of composi-tions of the paint industry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA002008135A CA2008135A1 (en) | 1990-01-19 | 1990-01-19 | Process for the complex extraction of plant materials and use of the extracts and residues obtained |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA002008135A CA2008135A1 (en) | 1990-01-19 | 1990-01-19 | Process for the complex extraction of plant materials and use of the extracts and residues obtained |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA2008135A1 true CA2008135A1 (en) | 1991-07-19 |
Family
ID=4144067
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA002008135A Abandoned CA2008135A1 (en) | 1990-01-19 | 1990-01-19 | Process for the complex extraction of plant materials and use of the extracts and residues obtained |
Country Status (1)
| Country | Link |
|---|---|
| CA (1) | CA2008135A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117050208A (en) * | 2023-09-14 | 2023-11-14 | 成都大学 | Young kiwi fruit polysaccharide extract and preparation method and application thereof |
-
1990
- 1990-01-19 CA CA002008135A patent/CA2008135A1/en not_active Abandoned
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117050208A (en) * | 2023-09-14 | 2023-11-14 | 成都大学 | Young kiwi fruit polysaccharide extract and preparation method and application thereof |
| CN117050208B (en) * | 2023-09-14 | 2024-03-22 | 成都大学 | Young kiwi fruit polysaccharide extract and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4886665A (en) | Compositions of oats and nettle extracts to be used as a food additive or pharmaceutical preparation in human health care | |
| Inglett et al. | Taste modifiers, taste-modifying properties of miracle fruit (Synsepalum dulcificum) | |
| KR100895110B1 (en) | Black garlic fermented by natural herb, processes for the preparation thereof, and health food comprising the same | |
| AU714310B2 (en) | Plant extract | |
| KR950001449B1 (en) | Method of processing aloe | |
| KR102387371B1 (en) | Fermented Stauntonia hexaphylla with improved antioxidant activity and uses thereof | |
| JP2003135028A (en) | Functional food for health | |
| WO1997025884A1 (en) | Ginseng processing method and processed ginseng prepared by the same | |
| JPS63283552A (en) | Health food mainly containing kind of sweet potato originating from brazil | |
| US3933789A (en) | Extraction of sterolins from plant material | |
| WO2002066041A1 (en) | Natural composition | |
| CN109053849B (en) | Comprehensive utilization method of dogwood | |
| CA2008135A1 (en) | Process for the complex extraction of plant materials and use of the extracts and residues obtained | |
| KR100200534B1 (en) | Cosmetics containing browned composition of grapes and ginseng | |
| JP2001192342A (en) | Method for producing mixture of liquid formulation of concentrated stevia with ripe punica granatum | |
| KR20220087888A (en) | Black bellflower syrup and method of preparing therefor | |
| JP3208531B2 (en) | Cosmetics containing grape and ginseng browned compositions | |
| KR101111288B1 (en) | Functional red pepper paste and manufacturing method thereof | |
| JPH0349553B2 (en) | ||
| KR100232987B1 (en) | Tonic composition and tonic including the same | |
| WO1990001270A1 (en) | Process for producing light- and heat-resistant, biologically active extracts, juices and products rich in vitamin c, flavour, aroma and colouring substances, as well as for producing pharmaceuticals, cosmetics, foodstuff, nutriments, fodder and materials yielding biological protection containing the above extracts, juices | |
| KR102478941B1 (en) | Bioactive composition for health promotion containing arginine and octacosanol | |
| KR102599866B1 (en) | Manufacturing Method of Chestnut inner Shell Tea | |
| KR102627124B1 (en) | Manufacturing method of Jelly Stick using Wood Cultivated Ginseng | |
| KR102451742B1 (en) | How the composition and manufacturing functional foods containing immature apples |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| FZDE | Dead |