WO2017195220A1 - Process for extraction of curcuminoids - Google Patents

Process for extraction of curcuminoids Download PDF

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Publication number
WO2017195220A1
WO2017195220A1 PCT/IN2017/050174 IN2017050174W WO2017195220A1 WO 2017195220 A1 WO2017195220 A1 WO 2017195220A1 IN 2017050174 W IN2017050174 W IN 2017050174W WO 2017195220 A1 WO2017195220 A1 WO 2017195220A1
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Prior art keywords
curcuminoids
solvent
turmeric
acetic acid
ranging
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PCT/IN2017/050174
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French (fr)
Inventor
Rajendra Sham DESHPANDE
Roshan Rajan Kulkarni
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Deshpande Rajendra Sham
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Publication of WO2017195220A1 publication Critical patent/WO2017195220A1/en

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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)
    • A61K36/88—Liliopsida (monocotyledons)
    • A61K36/906—Zingiberaceae (Ginger family)
    • A61K36/9066—Curcuma, e.g. common turmeric, East Indian arrowroot or mango ginger
    • 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

Definitions

  • the present invention generally relates to a process for extraction of bioactives and nutraceuticals and more particularly to a process for extraction of solvent and heavy metal free bioactives and nutraceuticals such as curcuminoids in a powder form which can be in micro or nano size range.
  • Nutraceuticals such as curcuminoids or simply curcumin that comprise of curcumin I, II, and III are extracted industrially using a two stage process that involves following general steps: i) Treating powdered turmeric with a non polar solvent such as hexane followed by treatment of the turmeric powder with a medium polar solvent such as ethyl acetate; or ii) Treating powdered turmeric with a medium polar solvent such as ethyl acetate followed by treatment of the extract with another medium polar solvent such as isopropyl alcohol.
  • a non polar solvent such as hexane
  • a medium polar solvent such as ethyl acetate
  • Another medium polar solvent such as isopropyl alcohol
  • An object of the present invention is to extract curcuminoids using green solvents, specifically those with a time tested human use.
  • the present invention provides a process for extraction of curcuminoids.
  • the process comprises treating finely powdered turmeric with any one of supercritical fluid alone and supercritical fluid in combination with co-solvent at temperature ranging between 35 to 150 °C, at pressure ranging from 80- 900 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric to remove essential oils therefrom and obtain de-oiled turmeric.
  • the supercritical fluid is selected from any one of supercritical C0 2i propane, butane, R22, R134, N 2 0 and combinations thereof, the supercritical fluid is preferably supercritical C0 2 .
  • the process further comprises pumping of co-solvent over the de-oiled turmeric in three steps while continuing the step of supercritical fluid extraction at a temperature ranging between 32 to 150 °C, pressure ranging from 80-900 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric to remove non curcuminoids from the de-oiled turmeric while selectively keeping curcuminoids therein.
  • the co-solvent is selected from any one of acetic acid, hexane, ether, ethyl acetate, acetone, methanol, ethanol, isopropyl alcohol or a combination of water with the above mentioned solvents wherein water concentration can be up to 50%, the co-solvent is preferably acetic acid pumped at a concentration of about 3% of the de -oiled turmeric over a period ranging from 0.5 to 10 minutes.
  • the process further comprises extracting remaining residue from the product of above step in solvent preferably acetic acid to obtain an extract containing curcuminoids, wherein acetic acid is used at a concentration of 1 to 10 times by weight, at temperature ranging from 35 to 80 °C, under stirring for a duration of 15 minutes to 2 hours.
  • solvents that can be used include any one of hexane, ether, ethyl acetate, acetone, methanol, ethanol, isopropyl alcohol or a combination of water with the above mentioned solvents wherein water concentration can be up to 50%.
  • the process involves repeating the previous step to combine, filter and concentrate resulting extracts.
  • the process comprises crystallizing the curcuminoids from the extract at a temperature ranging between 18 -3 0 °C. Thereafter, the process comprises filtering the crystallized curcuminoids, washing for example with cold acetic acid at a temperature ranging between 18 - 30 °C and drying to obtain totally solvent and heavy metal free dried curcuminoids.
  • the process for extraction of curcuminoids comprises treating finely powdered turmeric with any one of supercritical fluid alone and supercritical fluid in combination with co-solvent at temperature ranging between 35 to 150 °C, at pressure ranging from 80-900 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric to remove essential oils therefrom and obtain de-oiled turmeric.
  • the supercritical fluid is selected from any one of supercritical C0 2, propane, butane, R22, R134, N 2 0 and combinations thereof, the supercritical fluid is preferably supercritical C0 2 .
  • the process further comprises pumping of co-solvent over the de-oiled turmeric in three steps while continuing the step of supercritical fluid extraction at a temperature ranging between 32 to 150 °C, pressure ranging from 80-900 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric to remove non curcuminoids from the de-oiled turmeric while selectively keeping curcuminoids therein.
  • the co-solvent is selected from any one of acetic acid, hexane, ether, ethyl acetate, acetone, methanol, ethanol, isopropyl alcohol, or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50%, the co-solvent is preferably acetic acid pumped at a concentration of about 3% of the de -oiled turmeric over a period ranging from 0.5 to 10 minutes.
  • the process further comprises extracting remaining residue from the product of above step in solvent preferably acetic acid to obtain an extract containing curcuminoids, wherein acetic acid is used at a concentration of 1 to 10 times by weight, at temperature ranging from 35 to 80 °C, under stirring for a duration of 15 minutes to 2 hours.
  • solvents that can be used include any one of hexane, ether, ethyl acetate, acetone, methanol, ethanol, isopropyl alcohol or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50%.
  • the process further comprises adding extract obtained from the previous step in any one of cold water and hot water as a continuous flowing stream to precipitate curcuminoids and to remove water soluble impurities therefrom at a temperature ranging from 0 to 100 °C.
  • the process comprises separating the precipitated curcuminoids and washing repeatedly with any one of cold water and hot water as a continuous flowing stream to obtain partially purified curcuminoids; drying the partially purified curcuminoids and thereafter putting in an extractor; pumping co-solvent with supercritical fluid over the dried curcuminoids in three steps to precipitate almost pure curcuminoids in the extractor; and finally washing the pure curcuminoids for example with cold acetic acid to finally obtain totally solvent and heavy metal free dried curcuminoids.
  • the process for extraction of curcuminoids comprises treating finely powdered turmeric with any one of supercritical fluid alone and supercritical fluid in combination with co-solvent at temperature ranging between 35 to 150 °C, at pressure ranging from 80-900 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric to remove essential oils therefrom and obtain de-oiled turmeric.
  • the supercritical fluid is selected from any one of supercritical C0 2, propane, butane, R22, R134, N 2 0 and combinations thereof, the supercritical fluid is preferably supercritical C0 2 .
  • the process further comprises extracting the de-oiled turmeric with solvent preferably acetic acid , wherein acetic acid is used at a concentration of 1 to 10 times by weight, at temperature ranging from 35 to 80 °C, under stirring for a duration of 15 minutes to 2 hours.
  • solvent preferably acetic acid
  • Other solvent that can be used alternatively include any one of hexane, ether, ethyl acetate, acetone, methanol, ethanol, isopropyl alcohol or a combination of water with the above mentioned solvents wherein water concentration can be up to 50%.
  • the process comprises adding extract obtained from above step to water to precipitate the curcuminoids along with impurities such as non curcuminoids.
  • the process in subsequent steps comprises filtering the precipitated curcuminoids and impurities and washing repeatedly with any one of cold water and hot water as a continuous flowing stream to obtain partially purified curcuminoids; drying the partially purified curcuminoids and thereafter putting in an extractor; pumping co- solvent with supercritical fluid over the dried curcuminoids in three steps to precipitate almost pure curcuminoids in the extractor
  • the co-solvent is selected from any one of acetic acid, hexane, ether, ethyl acetate, acetone, methanol, ethanol, isopropyl alcohol, or a combination of water with the above mentioned solvents wherein water concentration can be up to 50%, the co-solvent is preferably acetic acid pumped at a concentration of about 3% of the de -oiled turmeric over a period ranging from 0.5 to 10 minutes.
  • the process involves washing the almost pure curcuminoids for example with cold acetic acid at a temperature ranging between 18-30 °C to finally obtain totally solvent free
  • the process comprises treating finely powdered turmeric with any one of supercritical fluid alone and supercritical fluid in combination with co-solvent at temperature ranging between 35 to 150 °C, at pressure ranging from 80- 900 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric to remove essential oils therefrom and obtain de-oiled turmeric.
  • the supercritical fluid is selected from any one of supercritical C0 2, propane, butane, R22, R134, N 2 0 and combinations thereof, the supercritical fluid is preferably supercritical C0 2 .
  • the process further comprises pumping of co-solvent over the de-oiled turmeric in three steps while continuing the step of supercritical fluid extraction at a temperature ranging between 32 to 150 °C, pressure ranging from 80-900 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric to remove non curcuminoids from the de-oiled turmeric while selectively keeping curcuminoids therein.
  • the co-solvent is selected from any one of acetic acid, hexane, ether, ethyl acetate, acetone, methanol, ethanol, isopropyl alcohol or a combination of water with the above mentioned solvents wherein water concentration can be up to 50%, the co-solvent is preferably acetic acid pumped at a concentration of about 3% of the de -oiled turmeric over a period ranging from 0.5 to 10 minutes.
  • the process in a next step comprises extracting remaining residue from the product of above step in in solvent to obtain an extract containing curcuminoids, wherein the solvent is preferably acetic acid used at a concentration of 1 to 10 times by weight, at temperature ranging from 35 to 80 °C, under stirring for a duration of 15 minutes to 2 hours such that the resulting extract having solvent preferably acetic acid ranging from 5 to 99.5 % of the total mass.
  • the process involves repeating the previous step to combine, filter and concentrate resulting extracts having acetic acid ranging from 5 to 95.5 % of the total mass.
  • solvents that can be alternatively used include any one of hexane, ether, ethyl acetate, acetone, methanol, ethanol, isopropyl alcohol or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50%.
  • the process in a further step comprises re-extracting the extract obtained from previous step with supercritical fluid in an extractor at temperatures between 35 to 150 °C, pressure ranging from 80-700 bars, at a flow rate ranging from 10 to 250 kg/kg of turmeric to remove non curcuminoids and acetic acid and precipitating almost pure curcuminoids.
  • the process in subsequent steps involves washing the precipitated almost pure curcuminoids for example with cold acetic acid at a temperature ranging between 18- 30 °C to obtain almost pure curcuminoids; and finally drying the almost pure curcuminoids to obtain a totally solvent and heavy metal free dried curcuminoids.
  • the present invention provides a process for extraction of nutraceuticals.
  • the process of the present invention extracts solvent and heavy metal free nutraceuticals such as curcuminoids using green solvents, specifically those with a time tested human use.
  • the present invention provides a process (100) for extraction of curcuminoids and specifically, the process (100) for extraction of solvent and heavy metal free curcuminoids from finely powdered turmeric as a raw material which is described in detailed step-wise manner herein below:
  • the process (100) begins at step (10).
  • the process (100) involves supercritical fluid extraction which involves treating the finely powdered turmeric (herein after 'the turmeric') with supercritical fluid to remove essential oils therefrom and obtain de-oiled turmeric.
  • the supercritical fluid is selected from but not limiting to supercritical C0 2 , propane, butane, R22, R134, and N 2 0 alone or in various combinations thereof.
  • the turmeric is treated with supercritical C0 2 at a temperature ranging between 35 to 150 °C, preferably between 37-70 °C, more preferably between 40 to 55 °C, pressure ranging from 80-900 bars, preferably ranging from 100-500 bars, more preferably between 130 to 180 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric.
  • step (20) can also be accomplished by using co solvents such as hexane, ether, ethyl acetate, acetone, acetic acid, methanol, ethanol, isopropyl alcohol and the like in combination with supercritical fluids as per various alternate embodiments of the process (100).
  • co solvents such as hexane, ether, ethyl acetate, acetone, acetic acid, methanol, ethanol, isopropyl alcohol and the like in combination with supercritical fluids as per various alternate embodiments of the process (100).
  • the process (100) involves pumping the co-solvent in a periodic/segmented manner over the de -oiled turmeric in three steps while continuing the step of supercritical fluid extraction to remove non curcuminoids including but not limited to resinous material and other medium polar impurities from the de-oiled turmeric while selectively keeping curcuminoids therein.
  • co-solvent pumping is repeated 2 more times after an interval ranging from 5 to 30 minutes, preferably 15 minutes till 1 hour.
  • the co- solvent is acetic acid pumped at a concentration of about 3% of the de-oiled turmeric over a period ranging from 0.5 to 10 min, preferably, 1 min at a temperature ranging between 32 to 150 °C, preferably between 37 to 70 °C, more preferably between 40 to 55 °C, pressure ranging from 80-900 bars, preferably ranging from 100 to 150 bars, more preferably between 130 to 180 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric.
  • the co-solvent can also be selected from any of the common organic solvents such as acetone, ethyl acetate, methanol, ethanol, isopropyl alcohol and the like or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50% as per various alternate embodiments of the process (100).
  • the co solvent can be pumped in a continuous manner in which case the percentage of co-solvent may range from 1 to 40 % of the turmeric quantum and for a period ranging from 2 minutes to 2 hours depending upon the quantum of curcuminoids present in the feed as well as on the flow rate of supercritical fluid.
  • the process (100) involves solvent extraction which involves extracting the remaining residue from the product of step (30) in a solvent to obtain an extract containing curcuminoids for further processing.
  • solvent is preferably acetic acid used at a concentration of 1 to 10 times by weight, preferably 5 times at temperature ranging from 35 to 80 °C, preferably 60 °C under stirring for a duration of 15 minutes to 2 hours, preferably 30 minutes or for a duration of 30 minutes to 2 hours, preferably 1 hour.
  • solvents such as hexane, ether, ethyl acetate, acetone, methanol, ethanol, and isopropyl alcohol or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50% can also be used in alternate embodiments of the process (100).
  • the process (100) involves optionally repeating the step (40) 2-3 times, thereafter combining the extracts, filtering and concentrating the extracts under vacuum at lower temperatures, preferably 40 °C.
  • the process (100) involves crystallizing the curcuminoids from the concentrated extract at a temperature ranging between 18-30 U C, preferably 20 U C.
  • the process (100) involves filtering the crystallized curcuminoids under a filter press followed by washing for example with cold acetic acid at a temperature ranging between 18-30 °C, preferably 20 °C and thereafter drying using conventional methods of drying to obtain totally solvent and heavy metal free dried curcuminoids.
  • the totally solvent and heavy metal free curcuminoids are obtained in nanoparticle forms with 95 % purity and having following composition.
  • the process (100) ends at step (80).
  • the present invention provides the process (200) for extraction of curcuminoids and specifically, the process (200) for extraction of solvent and heavy metal free curcuminoids from finely powdered turmeric as a raw material which is described in detailed step-wise manner herein below:
  • the process (200) begins at step (110).
  • the process (200) involves supercritical fluid extraction which involves treating the finely powdered turmeric (herein after 'the turmeric') with supercritical fluid to remove essential oils therefrom and obtain de-oiled turmeric.
  • the supercritical fluid is selected from but not limiting to supercritical C0 2 , propane, butane, R22, R134, and N 2 0 alone or in various combinations thereof.
  • the turmeric is treated with supercritical C0 2 at a temperature ranging between 35 to 150 °C, preferably between 37-70 °C, more preferably between 40 to 55 °C, pressure ranging from 80-900 bars, preferably ranging from 100-500 bars, more preferably between 130 to 180 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric.
  • step (120) can also be accomplished by using co solvents such as hexane, ether, ethyl acetate, acetone, acetic acid, methanol, ethanol, isopropyl alcohol, or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50%, and the like in combination with supercritical fluids as per various alternate embodiments of the process (200).
  • the process (200) involves pumping the co-solvent in a periodic/segmented manner over the de -oiled turmeric in three steps while continuing the step of supercritical fluid extraction to remove non curcuminoids including but not limited to resinous material and other medium polar impurities from the de-oiled turmeric while selectively keeping curcuminoids therein.
  • co-solvent pumping is repeated 2 more times after an interval ranging from 5 to 30 minutes, preferably 15 minutes till 1 hour.
  • the co- solvent is acetic acid pumped at a concentration of about 3% of the de-oiled turmeric over a period ranging from 0.5 to 10 min, preferably, 1 min at a temperature ranging between 32 to 150 C, preferably between 37 to 70 C, more preferably between 40 to 55 °C, pressure ranging from 80-900 bars, preferably ranging from 100 to 150 bars, more preferably between 130 to 180 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric.
  • the co-solvent can also be selected from any of the common organic solvents such as acetone, ethyl acetate, methanol, ethanol, isopropyl alcohol and the like or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50% as per various alternate embodiments of the process (200).
  • the co solvent can be pumped in a continuous manner in which case the percentage of co-solvent may range from 1 to 40 % of the turmeric quantum and for a period ranging from 2 minutes to 2 hours depending upon the quantum of curcuminoids present in the feed as well as on the flow rate of supercritical fluid.
  • the process (200) involves solvent extraction wherein the remaining residue from the product of step (130) is extracted in solvent to obtain an extract containing curcuminoids for further processing.
  • the solvent is preferably acetic acid is used at a concentration of 1 to 10 times by weight, preferably 5 times at temperature ranging from 35 to 80 °C, preferably 60 °C under stirring for a duration of 15 minutes to 2 hours, preferably 30 minutes or for a duration of 30 minutes to 2 hours, preferably 1 hour.
  • the process (200) involves optionally repeating the step ( 140) 2-3 times, thereafter combining the extracts, filtering and concentrating the extracts under vacuum at lower temperatures, preferably 40 °C.
  • the process (200) involves pouring/adding concentrated extract obtained from step (150) in any one of cold water and hot water as a continuous flowing stream to precipitate curcuminoids and to remove water soluble impurities.
  • the temperature of the water ranges from 0 to 100 °C, preferably between 15 °C to 70 °C.
  • the process (200) is such that precipitation under colder or hotter conditions would lead to curcumin in powder form which can be in nano or micro sizes.
  • the process (200) involves separating the precipitated curcuminoids for example by filtering under a filter press or centrifuging the precipitated curcuminoids and washing repeatedly with any one of fresh cold water and hot water as a continuous flowing stream at a temperature of 15 °C to obtain partially purified curcuminoids.
  • the process (200) involves drying the partially purified curcuminoids using conventional drying methods and thereafter putting in an extractor.
  • the process (200) involves pumping co-solvent such as acetic acid with supercritical fluid such as supercritical C0 2 over the dried curcuminoids in three steps to precipitate almost pure curcuminoids in the extractor.
  • co-solvents such as hexane, ether, ethyl acetate, acetone, methanol, ethanol, isopropyl alcohol, or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50% can also be used in other embodiments of the process (200).
  • the process (200) involves washing the pure curcuminoids for example with cold acetic acid at a temperature ranging between 18-30 °C to finally obtain totally solvent and heavy metal free dried curcuminoids.
  • the totally solvent free curcuminoids are obtained in nanoparticle forms with 95 % purity.
  • the process (200) ends at step (190).
  • the present invention provides the process (300) for extraction of curcuminoids and specifically, the process (300) for extraction of solvent and heavy metal free curcuminoids from finely powdered turmeric as a raw material which is described in detailed step-wise manner herein below:
  • the process (300) begins at step (210).
  • the process (300) involves supercritical fluid extraction which involves treating the finely powdered turmeric (herein after 'the turmeric') with supercritical fluid to remove essential oils therefrom and obtain de-oiled turmeric.
  • the supercritical fluid is selected from but not limiting to supercritical C0 2 , propane, butane, R22, R134, and N 2 0 alone or in various combinations thereof.
  • the turmeric is treated with supercritical C0 2 at a temperature ranging between 35 to 150 °C, preferably between 37-70 °C, more preferably between 40 to 55 °C, pressure ranging from 80-900 bars, preferably ranging from 100-500 bars, more preferably between 130 to 180 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric.
  • step (220) can also be accomplished by using co solvents such as hexane, ether, ethyl acetate, acetone, acetic acid, methanol, ethanol, isopropyl alcohol and the like or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50% in combination with supercritical fluids as per various alternate embodiments of the process (300).
  • the process (300) involves extracting the de-oiled turmeric powder with a solvent.
  • the solvent is preferably acetic acid used at a concentration of 1 to 10 times by weight, preferably 5 times at temperature ranging from 35 to 80 °C, preferably 60 °C under stirring for a duration of 15 minutes to 2 hours, preferably 30 minutes or for a duration of 30 minutes to 2 hours, preferably 1 hour.
  • other solvents such as hexane, ether, ethyl acetate, acetone, methanol, ethanol, and isopropyl alcohol, or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50% can also be used in alternate embodiments of the process (300).
  • the process (300) involves optionally repeating the step (230) 2-3 times, thereafter combining the extracts, filtering and concentrating the extracts under vacuum at lower temperatures, preferably 40 °C.
  • the process (300) involves adding the concentrated extract to water to precipitate the curcuminoids along with impurities such as non curcuminoids including but not limited to resinous material and other medium polar impurities.
  • the process (300) involves filtering the precipitated curcuminoids and impurities and washing repeatedly with any one of fresh cold water and hot water as a continuous flowing stream at a temperature of 15 °C to obtain partially purified curcuminoids.
  • the process (300) involves drying the partially purified curcuminoids using conventional drying methods and thereafter putting in the extractor.
  • the process (300) involves pumping a co-solvent such as acetic acid as along with supercritical fluid such as supercritical C0 2 over the dried curcuminoids in three steps to precipitate almost pure curcuminoids in the extractor.
  • a co-solvent such as acetic acid
  • supercritical fluid such as supercritical C0 2
  • the process (300) involves washing the almost pure curcuminoids for example with cold acetic acid to finally obtain a totally solvent and heavy metal free dried curcuminoids.
  • the totally solvent and heavy metal free dried curcuminoids are obtained in nanoparticle forms with 95 % purity.
  • the process (100) ends at step (90).
  • the process (300) ends at step (290).
  • the present invention provides the process (400) for extraction of curcuminoids and specifically, the process (400) for extraction of solvent and heavy metal free curcuminoids from finely powdered turmeric as a raw material which is described in detailed step-wise manner herein below:
  • the process (400) begins at step (310).
  • the process (400) involves supercritical fluid extraction which involves treating the finely powdered turmeric (herein after 'the turmeric') with supercritical fluid to remove essential oils therefrom and obtain de-oiled turmeric.
  • the supercritical fluid is selected from but not limiting to supercritical C0 2 , propane, butane, R22, R134, and N 2 0 alone or in various combinations thereof.
  • the turmeric is treated with supercritical C0 2 at a temperature ranging between 35 to 150 °C, preferably between 37-70 °C, more preferably between 40 to 55 °C, pressure ranging from 80-900 bars, preferably ranging from 100-500 bars, more preferably between 130 to 180 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric.
  • step (320) can also be accomplished by using co solvents such as hexane, ether, ethyl acetate, acetone, acetic acid, methanol, ethanol, isopropyl alcohol and the like or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50% in combination with supercritical fluids as per various alternate embodiments of the process (400).
  • co solvents such as hexane, ether, ethyl acetate, acetone, acetic acid, methanol, ethanol, isopropyl alcohol and the like or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50% in combination with supercritical fluids as per various alternate embodiments of the process (400).
  • the process (400) involves pumping the co-solvent in a periodic/segmented manner in three steps over the de-oiled turmeric while continuing the step of supercritical fluid extraction to remove non curcuminoids including but not limited to resinous material and other medium polar impurities from the de-oiled turmeric while selectively keeping curcuminoids therein.
  • co-solvent pumping is repeated 2 more times after an interval ranging from 5 to 30 minutes, preferably 15 minutes till 1 hour.
  • the co- solvent is acetic acid pumped at a concentration of about 3% of the de-oiled turmeric over a period ranging from 0.5 to 10 min, preferably, 1 min at a temperature ranging between 32 to 150 °C, preferably between 37 to 70 °C, more preferably between 40 to 55 °C, pressure ranging from 80-900 bars, preferably ranging from 100 to 150 bars, more preferably between 130 to 180 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric.
  • the co-solvent can also be selected from any of the common organic solvents such as acetone, ethyl acetate, methanol, ethanol, isopropyl alcohol and the like or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50% as per various alternate embodiments of the process (400).
  • the co solvent can be pumped in a continuous manner in which case the percentage of co-solvent may range from 1 to 40 % of the turmeric quantum and for a period ranging from 2 minutes to 2 hours depending upon the quantum of curcuminoids present in the feed as well as on the flow rate of supercritical fluid.
  • the process (400) involves solvent extraction wherein the remaining residue from the product of step (330) is extracted in solvent to obtain an extract containing curcuminoids for further processing.
  • the solvent is preferably acetic acid used at a concentration of 1 to 10 times by weight, preferably 5 times at temperature ranging from 35 to 80 °C, preferably 60 °C under stirring for a duration of 15 minutes to 2 hours, preferably 30 minutes or for a duration of 30 minutes to 2 hours, preferably 1 hour.
  • solvents such as hexane, ether, ethyl acetate, acetone, methanol, ethanol, and isopropyl alcohol or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50% can also be used in alternate embodiments of the process (400).
  • the process (400) involves optionally repeating the step (40) 2-3 times, thereafter combining the extracts, filtering and concentrating the extracts under vacuum at lower temperatures, preferably 40 °C to result at the end the extract with acetic acid ranging from 5 to 99.5 % of the total mass.
  • the process (400) involves re-extracting the concentrated extract obtained from step (350) with supercritical fluid such as supercritical C0 2 in the extractor at temperatures between 35 to 150 °C, preferably 50 °C and pressure ranging from 80-700 bars, preferably 150 bars at a flow rate ranging from 10 to 250 kg/kg of turmeric to remove non curcuminoids and acetic acid and precipitating almost pure curcuminoids.
  • supercritical fluid such as supercritical C0 2 in the extractor at temperatures between 35 to 150 °C, preferably 50 °C and pressure ranging from 80-700 bars, preferably 150 bars at a flow rate ranging from 10 to 250 kg/kg of turmeric to remove non curcuminoids and acetic acid and precipitating almost pure curcuminoids.
  • supercritical fluid such as supercritical C0 2 in the extractor at temperatures between 35 to 150 °C, preferably 50 °C and pressure ranging from 80-700 bars, preferably 150 bars at a flow rate ranging from 10 to 250 kg/kg of turmeric.
  • the process (400) involves washing the precipitated almost pure curcuminoids with cold acetic acid to obtain almost pure curcuminoids.
  • the process (400) involves drying the almost pure curcuminoids using conventional drying methods to obtain a totally solvent and heavy metal free dried curcuminoids.
  • the totally solvent and heavy metal free curcuminoids are obtained in nanoparticle forms with 95 % purity.
  • the process (400) ends at step (390).
  • the processes (100), (200), (300) and (400) can also be used for preparation of solvent and heavy metal free curcumin from commercially available curcumin as per an alternate embodiment thereof.
  • the processes (100), (200), (300) and (400) involve following steps:
  • Step 1 Re-dissolving commercially available curcumin containing harmful solvent traces in acetic acid from 1 to 10 times the weight of curcumin, preferably 3 to 6 times, more preferably 5 times at temperature ranging from 25 to 90 °C, preferably between 35 to 75 °C, more preferably at 50 °C.
  • Step 2 Re -precipitating the solution in cold or hot water or using supercritical fluid such as supercritical C0 2 with temperature ranging from 0 to 100 °C, preferably at 15 or 65 °C to render it completely free of harmful solvents.
  • Step 3 Filtering and drying curcumin using conventional methods to obtain solvent free curcumin.
  • Example 1 for the first embodiment (process (100)):
  • Finely powdered turmeric 3 kg was extracted with supercritical C02 at 45 °C and 150 bars at a flow rate of 40 kg/kg of turmeric for 1 hour.
  • acetic acid total 300 mL
  • the acetic acid treated turmeric powder was then extracted with 9 L of acetic acid at 60 C for 30 minutes. The acetic acid was filtered and concentrated under vacuum to 500 mL volume. The concentrated extract was then allowed to crystallize curcuminoids at 20 °C.
  • the crystallized curcuminoids were then filtered and washed with cold acetic acid at a temperature of 20 °C.
  • the curcuminoids were dried under hot air to obtain totally solvent and heavy metal free dried curcuminoids, 75 g containing, 95 % purity.
  • Finely powdered turmeric 3 kg was extracted with supercritical C0 2 at 45 °C and 150 bars at a flow rate of 40 kg/kg of turmeric for 1 hour.
  • acetic acid total 300 mL
  • the acetic acid treated turmeric powder was then extracted with 9 L of acetic acid at 60 °C for 30 minutes. The acetic acid was filtered and concentrated under vacuum to 500 mL volume. The concentrated extract was then added to water, 5 L at 15 °C.
  • Finely powdered turmeric 3 kg was extracted with supercritical C0 2 at 45 °C and 150 bars at a flow rate of 40 kg/kg of turmeric for 1 hour.
  • the de-oiled turmeric powder was then extracted with 9 L of acetic acid at 60 °C for 30 5 minutes.
  • the acetic acid was filtered and concentrated under vacuum to 500 mL volume.
  • the concentrated extract was then added to water, 5 L at 15 °C.
  • the precipitated curcuminoids were then filtered and washed repeatedly with 500 mL fresh cold water at a temperature of 15 °C.
  • the partially purified curcuminoids were air dried and put in the extractor.
  • acetic acid was pumped over a period of 1 minute. This step was repeated 2 more times to precipitate almost pure curcuminoids in the extractor. They were then washed with cold acetic acid to finally obtain and heavy metal curcuminoids 95 % pure, 75 g.
  • Finely powdered turmeric 3 kg was extracted with supercritical C0 2 at 45 °C and 150 bars at a flow rate of 40 kg/kg of turmeric for 1 hour.
  • acetic acid total 300 mL
  • the acetic acid treated turmeric powder was then extracted with 9 L of acetic acid at 60 °C for 30 minutes. The acetic acid was filtered and concentrated under vacuum to 500 mL volume.
  • the concentrated extract was then fed to the extractor and subjected to extraction with supercritical C0 2 at 45 °C and 150 bars to remove non curcuminoids and acetic acid leaving curcuminoids 95% pure in the extractor. They were finally washed with cold acetic acid and dried to obtain and heavy metal curcuminoids 95 % pure, 75 g.
  • Each process (100), (200), (300) and (400) uses green solvents that are used as food additives since time immemorial.
  • C0 2 in the supercritical phase is a green solvent that leaves no trace in the extract after conversion to the gaseous state.
  • Each process (100), (200), (300) and (400) uses acetic acid that has a significant effect on the acceptability by regulatory authorities and consumers alike.
  • Each process (100), (200), (300) and (400) involves acetic acid dissolution and re-precipitation in water that removes all previous traces of organic solvents and heavy metals from the extracted curcuminoids.

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Abstract

A process (100/200/300/400) for extraction of curcuminoids is disclosed. The process (100/200/300/400) extracts curcuminoids finely powdered turmeric as a raw material using solvents such as supercritical fluid and acetic acid with a time tested human use that leaves no trace in the extract after conversion to the gaseous state. The process (100/200/300/400) results in extraction of solvent and heavy metal free nutraceuticals such as curcuminoids which may also be in a nanoparticle form.

Description

PROCESS FOR EXTRACTION OF CURCUMINOIDS
FIELD OF THE INVENTION The present invention generally relates to a process for extraction of bioactives and nutraceuticals and more particularly to a process for extraction of solvent and heavy metal free bioactives and nutraceuticals such as curcuminoids in a powder form which can be in micro or nano size range. BACKGROUND OF THE INVENTION
Nutraceuticals such as curcuminoids or simply curcumin that comprise of curcumin I, II, and III are extracted industrially using a two stage process that involves following general steps: i) Treating powdered turmeric with a non polar solvent such as hexane followed by treatment of the turmeric powder with a medium polar solvent such as ethyl acetate; or ii) Treating powdered turmeric with a medium polar solvent such as ethyl acetate followed by treatment of the extract with another medium polar solvent such as isopropyl alcohol. Current state of the art uses solvents that may pose significant health risks over longer run. Although solvents such as ethyl acetate are considered as safe, exposure to humans is relatively new and their full drawbacks are yet to emerge. Curcumin has one of the highest consumption among populations across demographic distribution for its medicinal and nutraceutical values. Hence, a process for extraction of curcumin is needed that uses green solvents, specifically those with a time tested human use. Hence, there exists a need to provide a process for extraction of solvent and heavy metal free curcuminoids that overcomes the above mentioned drawbacks of the prior art. OBJECT OF THE INVENTION
An object of the present invention is to extract curcuminoids using green solvents, specifically those with a time tested human use. SUMMARY OF THE INVENTION
Accordingly, the present invention provides a process for extraction of curcuminoids. As per a first embodiment, the process comprises treating finely powdered turmeric with any one of supercritical fluid alone and supercritical fluid in combination with co-solvent at temperature ranging between 35 to 150 °C, at pressure ranging from 80- 900 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric to remove essential oils therefrom and obtain de-oiled turmeric. The supercritical fluid is selected from any one of supercritical C02i propane, butane, R22, R134, N20 and combinations thereof, the supercritical fluid is preferably supercritical C02.
The process further comprises pumping of co-solvent over the de-oiled turmeric in three steps while continuing the step of supercritical fluid extraction at a temperature ranging between 32 to 150 °C, pressure ranging from 80-900 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric to remove non curcuminoids from the de-oiled turmeric while selectively keeping curcuminoids therein. The co-solvent is selected from any one of acetic acid, hexane, ether, ethyl acetate, acetone, methanol, ethanol, isopropyl alcohol or a combination of water with the above mentioned solvents wherein water concentration can be up to 50%, the co-solvent is preferably acetic acid pumped at a concentration of about 3% of the de -oiled turmeric over a period ranging from 0.5 to 10 minutes.
The process further comprises extracting remaining residue from the product of above step in solvent preferably acetic acid to obtain an extract containing curcuminoids, wherein acetic acid is used at a concentration of 1 to 10 times by weight, at temperature ranging from 35 to 80 °C, under stirring for a duration of 15 minutes to 2 hours. Other solvents that can be used include any one of hexane, ether, ethyl acetate, acetone, methanol, ethanol, isopropyl alcohol or a combination of water with the above mentioned solvents wherein water concentration can be up to 50%. The process involves repeating the previous step to combine, filter and concentrate resulting extracts.
Further, the process comprises crystallizing the curcuminoids from the extract at a temperature ranging between 18 -3 0 °C. Thereafter, the process comprises filtering the crystallized curcuminoids, washing for example with cold acetic acid at a temperature ranging between 18 - 30 °C and drying to obtain totally solvent and heavy metal free dried curcuminoids. In a second embodiment, the process for extraction of curcuminoids comprises treating finely powdered turmeric with any one of supercritical fluid alone and supercritical fluid in combination with co-solvent at temperature ranging between 35 to 150 °C, at pressure ranging from 80-900 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric to remove essential oils therefrom and obtain de-oiled turmeric. The supercritical fluid is selected from any one of supercritical C02, propane, butane, R22, R134, N20 and combinations thereof, the supercritical fluid is preferably supercritical C02. The process further comprises pumping of co-solvent over the de-oiled turmeric in three steps while continuing the step of supercritical fluid extraction at a temperature ranging between 32 to 150 °C, pressure ranging from 80-900 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric to remove non curcuminoids from the de-oiled turmeric while selectively keeping curcuminoids therein. The co-solvent is selected from any one of acetic acid, hexane, ether, ethyl acetate, acetone, methanol, ethanol, isopropyl alcohol, or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50%, the co-solvent is preferably acetic acid pumped at a concentration of about 3% of the de -oiled turmeric over a period ranging from 0.5 to 10 minutes.
The process further comprises extracting remaining residue from the product of above step in solvent preferably acetic acid to obtain an extract containing curcuminoids, wherein acetic acid is used at a concentration of 1 to 10 times by weight, at temperature ranging from 35 to 80 °C, under stirring for a duration of 15 minutes to 2 hours. Other solvents that can be used include any one of hexane, ether, ethyl acetate, acetone, methanol, ethanol, isopropyl alcohol or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50%. The process further comprises adding extract obtained from the previous step in any one of cold water and hot water as a continuous flowing stream to precipitate curcuminoids and to remove water soluble impurities therefrom at a temperature ranging from 0 to 100 °C. In a next step, the process comprises separating the precipitated curcuminoids and washing repeatedly with any one of cold water and hot water as a continuous flowing stream to obtain partially purified curcuminoids; drying the partially purified curcuminoids and thereafter putting in an extractor; pumping co-solvent with supercritical fluid over the dried curcuminoids in three steps to precipitate almost pure curcuminoids in the extractor; and finally washing the pure curcuminoids for example with cold acetic acid to finally obtain totally solvent and heavy metal free dried curcuminoids.
In a third embodiment, the process for extraction of curcuminoids comprises treating finely powdered turmeric with any one of supercritical fluid alone and supercritical fluid in combination with co-solvent at temperature ranging between 35 to 150 °C, at pressure ranging from 80-900 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric to remove essential oils therefrom and obtain de-oiled turmeric. The supercritical fluid is selected from any one of supercritical C02, propane, butane, R22, R134, N20 and combinations thereof, the supercritical fluid is preferably supercritical C02. The process further comprises extracting the de-oiled turmeric with solvent preferably acetic acid , wherein acetic acid is used at a concentration of 1 to 10 times by weight, at temperature ranging from 35 to 80 °C, under stirring for a duration of 15 minutes to 2 hours. Other solvent that can be used alternatively include any one of hexane, ether, ethyl acetate, acetone, methanol, ethanol, isopropyl alcohol or a combination of water with the above mentioned solvents wherein water concentration can be up to 50%.
In a next step, the process comprises adding extract obtained from above step to water to precipitate the curcuminoids along with impurities such as non curcuminoids.
The process in subsequent steps comprises filtering the precipitated curcuminoids and impurities and washing repeatedly with any one of cold water and hot water as a continuous flowing stream to obtain partially purified curcuminoids; drying the partially purified curcuminoids and thereafter putting in an extractor; pumping co- solvent with supercritical fluid over the dried curcuminoids in three steps to precipitate almost pure curcuminoids in the extractor The co-solvent is selected from any one of acetic acid, hexane, ether, ethyl acetate, acetone, methanol, ethanol, isopropyl alcohol, or a combination of water with the above mentioned solvents wherein water concentration can be up to 50%, the co-solvent is preferably acetic acid pumped at a concentration of about 3% of the de -oiled turmeric over a period ranging from 0.5 to 10 minutes. In the last step, the process involves washing the almost pure curcuminoids for example with cold acetic acid at a temperature ranging between 18-30 °C to finally obtain totally solvent free dried curcuminoids.
As per a fourth embodiment, the process comprises treating finely powdered turmeric with any one of supercritical fluid alone and supercritical fluid in combination with co-solvent at temperature ranging between 35 to 150 °C, at pressure ranging from 80- 900 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric to remove essential oils therefrom and obtain de-oiled turmeric. The supercritical fluid is selected from any one of supercritical C02, propane, butane, R22, R134, N20 and combinations thereof, the supercritical fluid is preferably supercritical C02.
The process further comprises pumping of co-solvent over the de-oiled turmeric in three steps while continuing the step of supercritical fluid extraction at a temperature ranging between 32 to 150 °C, pressure ranging from 80-900 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric to remove non curcuminoids from the de-oiled turmeric while selectively keeping curcuminoids therein. The co-solvent is selected from any one of acetic acid, hexane, ether, ethyl acetate, acetone, methanol, ethanol, isopropyl alcohol or a combination of water with the above mentioned solvents wherein water concentration can be up to 50%, the co-solvent is preferably acetic acid pumped at a concentration of about 3% of the de -oiled turmeric over a period ranging from 0.5 to 10 minutes.
The process in a next step comprises extracting remaining residue from the product of above step in in solvent to obtain an extract containing curcuminoids, wherein the solvent is preferably acetic acid used at a concentration of 1 to 10 times by weight, at temperature ranging from 35 to 80 °C, under stirring for a duration of 15 minutes to 2 hours such that the resulting extract having solvent preferably acetic acid ranging from 5 to 99.5 % of the total mass. The process involves repeating the previous step to combine, filter and concentrate resulting extracts having acetic acid ranging from 5 to 95.5 % of the total mass. Other solvents that can be alternatively used include any one of hexane, ether, ethyl acetate, acetone, methanol, ethanol, isopropyl alcohol or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50%.
The process in a further step comprises re-extracting the extract obtained from previous step with supercritical fluid in an extractor at temperatures between 35 to 150 °C, pressure ranging from 80-700 bars, at a flow rate ranging from 10 to 250 kg/kg of turmeric to remove non curcuminoids and acetic acid and precipitating almost pure curcuminoids.
The process in subsequent steps involves washing the precipitated almost pure curcuminoids for example with cold acetic acid at a temperature ranging between 18- 30 °C to obtain almost pure curcuminoids; and finally drying the almost pure curcuminoids to obtain a totally solvent and heavy metal free dried curcuminoids.
DETAILED DESCRIPTION OF THE INVENTION The foregoing objects of the invention are accomplished and the problems and shortcomings associated with the prior art techniques and approaches are overcome by the present invention as described below in the preferred embodiment. The present invention provides a process for extraction of nutraceuticals. The process of the present invention extracts solvent and heavy metal free nutraceuticals such as curcuminoids using green solvents, specifically those with a time tested human use.
Specifically, a process for extraction of curcuminoids is described in accordance with the present invention. More specifically, the process is described for extraction of solvent and heavy metal free nutraceuticals such as curcuminoids/ curcumin. However, it is understood that the process can be used for extraction of other nutraceuticals known in the art. In a first embodiment, the present invention provides a process (100) for extraction of curcuminoids and specifically, the process (100) for extraction of solvent and heavy metal free curcuminoids from finely powdered turmeric as a raw material which is described in detailed step-wise manner herein below: The process (100) begins at step (10). At step (20), the process (100) involves supercritical fluid extraction which involves treating the finely powdered turmeric (herein after 'the turmeric') with supercritical fluid to remove essential oils therefrom and obtain de-oiled turmeric. The supercritical fluid is selected from but not limiting to supercritical C02, propane, butane, R22, R134, and N20 alone or in various combinations thereof. Specifically, the turmeric is treated with supercritical C02 at a temperature ranging between 35 to 150 °C, preferably between 37-70 °C, more preferably between 40 to 55 °C, pressure ranging from 80-900 bars, preferably ranging from 100-500 bars, more preferably between 130 to 180 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric. Optionally, step (20) can also be accomplished by using co solvents such as hexane, ether, ethyl acetate, acetone, acetic acid, methanol, ethanol, isopropyl alcohol and the like in combination with supercritical fluids as per various alternate embodiments of the process (100).
At step (30), the process (100) involves pumping the co-solvent in a periodic/segmented manner over the de -oiled turmeric in three steps while continuing the step of supercritical fluid extraction to remove non curcuminoids including but not limited to resinous material and other medium polar impurities from the de-oiled turmeric while selectively keeping curcuminoids therein. Thus, after the first step of co-solvent pumping, co-solvent pumping is repeated 2 more times after an interval ranging from 5 to 30 minutes, preferably 15 minutes till 1 hour. Specifically, the co- solvent is acetic acid pumped at a concentration of about 3% of the de-oiled turmeric over a period ranging from 0.5 to 10 min, preferably, 1 min at a temperature ranging between 32 to 150 °C, preferably between 37 to 70 °C, more preferably between 40 to 55 °C, pressure ranging from 80-900 bars, preferably ranging from 100 to 150 bars, more preferably between 130 to 180 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric. However, it is understood that the co-solvent can also be selected from any of the common organic solvents such as acetone, ethyl acetate, methanol, ethanol, isopropyl alcohol and the like or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50% as per various alternate embodiments of the process (100). Similarly, it is understood that the co solvent can be pumped in a continuous manner in which case the percentage of co-solvent may range from 1 to 40 % of the turmeric quantum and for a period ranging from 2 minutes to 2 hours depending upon the quantum of curcuminoids present in the feed as well as on the flow rate of supercritical fluid. At step (40), the process (100) involves solvent extraction which involves extracting the remaining residue from the product of step (30) in a solvent to obtain an extract containing curcuminoids for further processing. In an embodiment, solvent is preferably acetic acid used at a concentration of 1 to 10 times by weight, preferably 5 times at temperature ranging from 35 to 80 °C, preferably 60 °C under stirring for a duration of 15 minutes to 2 hours, preferably 30 minutes or for a duration of 30 minutes to 2 hours, preferably 1 hour. However, other solvents such as hexane, ether, ethyl acetate, acetone, methanol, ethanol, and isopropyl alcohol or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50% can also be used in alternate embodiments of the process (100).
At step (50), the process (100) involves optionally repeating the step (40) 2-3 times, thereafter combining the extracts, filtering and concentrating the extracts under vacuum at lower temperatures, preferably 40 °C.
At step (60), the process (100) involves crystallizing the curcuminoids from the concentrated extract at a temperature ranging between 18-30 UC, preferably 20 UC.
At step 70), the process (100) involves filtering the crystallized curcuminoids under a filter press followed by washing for example with cold acetic acid at a temperature ranging between 18-30 °C, preferably 20 °C and thereafter drying using conventional methods of drying to obtain totally solvent and heavy metal free dried curcuminoids. In an embodiment, the totally solvent and heavy metal free curcuminoids are obtained in nanoparticle forms with 95 % purity and having following composition. The process (100) ends at step (80).
In a second embodiment, the present invention provides the process (200) for extraction of curcuminoids and specifically, the process (200) for extraction of solvent and heavy metal free curcuminoids from finely powdered turmeric as a raw material which is described in detailed step-wise manner herein below:
The process (200) begins at step (110). At step (120), the process (200) involves supercritical fluid extraction which involves treating the finely powdered turmeric (herein after 'the turmeric') with supercritical fluid to remove essential oils therefrom and obtain de-oiled turmeric. The supercritical fluid is selected from but not limiting to supercritical C02, propane, butane, R22, R134, and N20 alone or in various combinations thereof. Specifically, the turmeric is treated with supercritical C02 at a temperature ranging between 35 to 150 °C, preferably between 37-70 °C, more preferably between 40 to 55 °C, pressure ranging from 80-900 bars, preferably ranging from 100-500 bars, more preferably between 130 to 180 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric. Optionally, step (120) can also be accomplished by using co solvents such as hexane, ether, ethyl acetate, acetone, acetic acid, methanol, ethanol, isopropyl alcohol, or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50%, and the like in combination with supercritical fluids as per various alternate embodiments of the process (200). At step (130), the process (200) involves pumping the co-solvent in a periodic/segmented manner over the de -oiled turmeric in three steps while continuing the step of supercritical fluid extraction to remove non curcuminoids including but not limited to resinous material and other medium polar impurities from the de-oiled turmeric while selectively keeping curcuminoids therein. Thus, after the first step of co-solvent pumping, co-solvent pumping is repeated 2 more times after an interval ranging from 5 to 30 minutes, preferably 15 minutes till 1 hour. Specifically, the co- solvent is acetic acid pumped at a concentration of about 3% of the de-oiled turmeric over a period ranging from 0.5 to 10 min, preferably, 1 min at a temperature ranging between 32 to 150 C, preferably between 37 to 70 C, more preferably between 40 to 55 °C, pressure ranging from 80-900 bars, preferably ranging from 100 to 150 bars, more preferably between 130 to 180 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric. However, it is understood that the co-solvent can also be selected from any of the common organic solvents such as acetone, ethyl acetate, methanol, ethanol, isopropyl alcohol and the like or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50% as per various alternate embodiments of the process (200). Similarly, it is understood that the co solvent can be pumped in a continuous manner in which case the percentage of co-solvent may range from 1 to 40 % of the turmeric quantum and for a period ranging from 2 minutes to 2 hours depending upon the quantum of curcuminoids present in the feed as well as on the flow rate of supercritical fluid.
At step (140), the process (200) involves solvent extraction wherein the remaining residue from the product of step (130) is extracted in solvent to obtain an extract containing curcuminoids for further processing. In an embodiment, the solvent is preferably acetic acid is used at a concentration of 1 to 10 times by weight, preferably 5 times at temperature ranging from 35 to 80 °C, preferably 60 °C under stirring for a duration of 15 minutes to 2 hours, preferably 30 minutes or for a duration of 30 minutes to 2 hours, preferably 1 hour. However, other solvents such as hexane, ether, ethyl acetate, acetone, methanol, ethanol, and isopropyl alcohol, or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50%, can also be used in alternate embodiments of the process (200). At step (150), the process (200) involves optionally repeating the step ( 140) 2-3 times, thereafter combining the extracts, filtering and concentrating the extracts under vacuum at lower temperatures, preferably 40 °C. At step (160), the process (200) involves pouring/adding concentrated extract obtained from step (150) in any one of cold water and hot water as a continuous flowing stream to precipitate curcuminoids and to remove water soluble impurities. The temperature of the water ranges from 0 to 100 °C, preferably between 15 °C to 70 °C. The process (200) is such that precipitation under colder or hotter conditions would lead to curcumin in powder form which can be in nano or micro sizes.
At step (170), the process (200) involves separating the precipitated curcuminoids for example by filtering under a filter press or centrifuging the precipitated curcuminoids and washing repeatedly with any one of fresh cold water and hot water as a continuous flowing stream at a temperature of 15 °C to obtain partially purified curcuminoids.
At step (180), the process (200) involves drying the partially purified curcuminoids using conventional drying methods and thereafter putting in an extractor.
At step (182), the process (200) involves pumping co-solvent such as acetic acid with supercritical fluid such as supercritical C02 over the dried curcuminoids in three steps to precipitate almost pure curcuminoids in the extractor. However, it is understood that other co-solvents such as hexane, ether, ethyl acetate, acetone, methanol, ethanol, isopropyl alcohol, or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50% can also be used in other embodiments of the process (200). At step (184), the process (200) involves washing the pure curcuminoids for example with cold acetic acid at a temperature ranging between 18-30 °C to finally obtain totally solvent and heavy metal free dried curcuminoids. In an embodiment, the totally solvent free curcuminoids are obtained in nanoparticle forms with 95 % purity. The process (200) ends at step (190).
In a third embodiment, the present invention provides the process (300) for extraction of curcuminoids and specifically, the process (300) for extraction of solvent and heavy metal free curcuminoids from finely powdered turmeric as a raw material which is described in detailed step-wise manner herein below:
The process (300) begins at step (210). At step (220), the process (300) involves supercritical fluid extraction which involves treating the finely powdered turmeric (herein after 'the turmeric') with supercritical fluid to remove essential oils therefrom and obtain de-oiled turmeric. The supercritical fluid is selected from but not limiting to supercritical C02, propane, butane, R22, R134, and N20 alone or in various combinations thereof. Specifically, the turmeric is treated with supercritical C02 at a temperature ranging between 35 to 150 °C, preferably between 37-70 °C, more preferably between 40 to 55 °C, pressure ranging from 80-900 bars, preferably ranging from 100-500 bars, more preferably between 130 to 180 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric. Optionally, step (220) can also be accomplished by using co solvents such as hexane, ether, ethyl acetate, acetone, acetic acid, methanol, ethanol, isopropyl alcohol and the like or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50% in combination with supercritical fluids as per various alternate embodiments of the process (300). At step (230), the process (300) involves extracting the de-oiled turmeric powder with a solvent. In an embodiment, the solvent is preferably acetic acid used at a concentration of 1 to 10 times by weight, preferably 5 times at temperature ranging from 35 to 80 °C, preferably 60 °C under stirring for a duration of 15 minutes to 2 hours, preferably 30 minutes or for a duration of 30 minutes to 2 hours, preferably 1 hour. However, other solvents such as hexane, ether, ethyl acetate, acetone, methanol, ethanol, and isopropyl alcohol, or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50% can also be used in alternate embodiments of the process (300).
At step (240), the process (300) involves optionally repeating the step (230) 2-3 times, thereafter combining the extracts, filtering and concentrating the extracts under vacuum at lower temperatures, preferably 40 °C.
At step (250), the process (300) involves adding the concentrated extract to water to precipitate the curcuminoids along with impurities such as non curcuminoids including but not limited to resinous material and other medium polar impurities. At step (260), the process (300) involves filtering the precipitated curcuminoids and impurities and washing repeatedly with any one of fresh cold water and hot water as a continuous flowing stream at a temperature of 15 °C to obtain partially purified curcuminoids. At step (270), the process (300) involves drying the partially purified curcuminoids using conventional drying methods and thereafter putting in the extractor.
At step (280), the process (300) involves pumping a co-solvent such as acetic acid as along with supercritical fluid such as supercritical C02 over the dried curcuminoids in three steps to precipitate almost pure curcuminoids in the extractor.
At step (285), the process (300) involves washing the almost pure curcuminoids for example with cold acetic acid to finally obtain a totally solvent and heavy metal free dried curcuminoids. In an embodiment, the totally solvent and heavy metal free dried curcuminoids are obtained in nanoparticle forms with 95 % purity. The process (100) ends at step (90). The process (300) ends at step (290). In a fourth embodiment, the present invention provides the process (400) for extraction of curcuminoids and specifically, the process (400) for extraction of solvent and heavy metal free curcuminoids from finely powdered turmeric as a raw material which is described in detailed step-wise manner herein below: The process (400) begins at step (310). At step (320), the process (400) involves supercritical fluid extraction which involves treating the finely powdered turmeric (herein after 'the turmeric') with supercritical fluid to remove essential oils therefrom and obtain de-oiled turmeric. The supercritical fluid is selected from but not limiting to supercritical C02, propane, butane, R22, R134, and N20 alone or in various combinations thereof. Specifically, the turmeric is treated with supercritical C02 at a temperature ranging between 35 to 150 °C, preferably between 37-70 °C, more preferably between 40 to 55 °C, pressure ranging from 80-900 bars, preferably ranging from 100-500 bars, more preferably between 130 to 180 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric. Optionally, step (320) can also be accomplished by using co solvents such as hexane, ether, ethyl acetate, acetone, acetic acid, methanol, ethanol, isopropyl alcohol and the like or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50% in combination with supercritical fluids as per various alternate embodiments of the process (400).
At step (330), the process (400) involves pumping the co-solvent in a periodic/segmented manner in three steps over the de-oiled turmeric while continuing the step of supercritical fluid extraction to remove non curcuminoids including but not limited to resinous material and other medium polar impurities from the de-oiled turmeric while selectively keeping curcuminoids therein. Thus, after the first step of co-solvent pumping, co-solvent pumping is repeated 2 more times after an interval ranging from 5 to 30 minutes, preferably 15 minutes till 1 hour. Specifically, the co- solvent is acetic acid pumped at a concentration of about 3% of the de-oiled turmeric over a period ranging from 0.5 to 10 min, preferably, 1 min at a temperature ranging between 32 to 150 °C, preferably between 37 to 70 °C, more preferably between 40 to 55 °C, pressure ranging from 80-900 bars, preferably ranging from 100 to 150 bars, more preferably between 130 to 180 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric. However, it is understood that the co-solvent can also be selected from any of the common organic solvents such as acetone, ethyl acetate, methanol, ethanol, isopropyl alcohol and the like or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50% as per various alternate embodiments of the process (400). Similarly, it is understood that the co solvent can be pumped in a continuous manner in which case the percentage of co-solvent may range from 1 to 40 % of the turmeric quantum and for a period ranging from 2 minutes to 2 hours depending upon the quantum of curcuminoids present in the feed as well as on the flow rate of supercritical fluid. At step (340), the process (400) involves solvent extraction wherein the remaining residue from the product of step (330) is extracted in solvent to obtain an extract containing curcuminoids for further processing. In an embodiment, the solvent is preferably acetic acid used at a concentration of 1 to 10 times by weight, preferably 5 times at temperature ranging from 35 to 80 °C, preferably 60 °C under stirring for a duration of 15 minutes to 2 hours, preferably 30 minutes or for a duration of 30 minutes to 2 hours, preferably 1 hour. However, other solvents such as hexane, ether, ethyl acetate, acetone, methanol, ethanol, and isopropyl alcohol or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50% can also be used in alternate embodiments of the process (400).
At step (350), the process (400) involves optionally repeating the step (40) 2-3 times, thereafter combining the extracts, filtering and concentrating the extracts under vacuum at lower temperatures, preferably 40 °C to result at the end the extract with acetic acid ranging from 5 to 99.5 % of the total mass.
At step (360), the process (400) involves re-extracting the concentrated extract obtained from step (350) with supercritical fluid such as supercritical C02 in the extractor at temperatures between 35 to 150 °C, preferably 50 °C and pressure ranging from 80-700 bars, preferably 150 bars at a flow rate ranging from 10 to 250 kg/kg of turmeric to remove non curcuminoids and acetic acid and precipitating almost pure curcuminoids. In the case of acetic acid being 99.5 to 80 % of the total mass, treatment with the supercritical C02 may result in curcuminoids precipitating in the nano sized form while simultaneously getting rid of non curcuminoids and acetic acid.
At step (370), the process (400) involves washing the precipitated almost pure curcuminoids with cold acetic acid to obtain almost pure curcuminoids.
At step (380), the process (400) involves drying the almost pure curcuminoids using conventional drying methods to obtain a totally solvent and heavy metal free dried curcuminoids. In an embodiment, the totally solvent and heavy metal free curcuminoids are obtained in nanoparticle forms with 95 % purity. The process (400) ends at step (390). Besides extracting solvent and heavy metal free curcumin from turmeric, the processes (100), (200), (300) and (400) can also be used for preparation of solvent and heavy metal free curcumin from commercially available curcumin as per an alternate embodiment thereof. The processes (100), (200), (300) and (400) involve following steps:
• Step 1: Re-dissolving commercially available curcumin containing harmful solvent traces in acetic acid from 1 to 10 times the weight of curcumin, preferably 3 to 6 times, more preferably 5 times at temperature ranging from 25 to 90 °C, preferably between 35 to 75 °C, more preferably at 50 °C. · Step 2: Re -precipitating the solution in cold or hot water or using supercritical fluid such as supercritical C02 with temperature ranging from 0 to 100 °C, preferably at 15 or 65 °C to render it completely free of harmful solvents.
• Step 3: Filtering and drying curcumin using conventional methods to obtain solvent free curcumin.
Examples
The process of the present invention will be described in more details below by means of an example. The following example is provided in order to demonstrate and further illustrate the embodiments and aspects of the present invention and is not to be construed as limiting the scope thereof.
Example 1 for the first embodiment (process (100)):
Finely powdered turmeric, 3 kg, was extracted with supercritical C02 at 45 °C and 150 bars at a flow rate of 40 kg/kg of turmeric for 1 hour. To the turmeric, now de- oiled, acetic acid, total 300 mL, was pumped as co-solvent (with supercritical C02) in three steps. At each step 100 mL acetic acid was pumped over a period of 1 minute. This step was repeated 2 more times. The acetic acid treated turmeric powder was then extracted with 9 L of acetic acid at 60 C for 30 minutes. The acetic acid was filtered and concentrated under vacuum to 500 mL volume. The concentrated extract was then allowed to crystallize curcuminoids at 20 °C. The crystallized curcuminoids were then filtered and washed with cold acetic acid at a temperature of 20 °C. The curcuminoids were dried under hot air to obtain totally solvent and heavy metal free dried curcuminoids, 75 g containing, 95 % purity.
Example 2 for the second embodiment (process (200)):
Finely powdered turmeric, 3 kg, was extracted with supercritical C02 at 45 °C and 150 bars at a flow rate of 40 kg/kg of turmeric for 1 hour. To the turmeric, now de- oiled, acetic acid, total 300 mL, was pumped as co-solvent (with supercritical C02) in three steps. At each step 100 mL acetic acid was pumped over a period of 1 minute. This step was repeated 2 more times. The acetic acid treated turmeric powder was then extracted with 9 L of acetic acid at 60 °C for 30 minutes. The acetic acid was filtered and concentrated under vacuum to 500 mL volume. The concentrated extract was then added to water, 5 L at 15 °C. The precipitated curcuminoids were then filtered and washed repeatedly with 500 mL fresh cold water at a temperature of 15 °C. The partially purified curcuminoids were air dried and put in the extractor. Acetic acid, total 300 mL, was pumped as co-solvent (with supercritical C02) in three steps. At each step 100 mL acetic acid was pumped over a period of 1 minute. This step was repeated 2 more times to precipitate almost pure curcuminoids in the extractor. They were then washed with cold acetic acid to finally obtain and heavy metal curcuminoids 95 % pure, 75 g. Example 3 for the third embodiment (process (300)):
Finely powdered turmeric, 3 kg, was extracted with supercritical C02 at 45 °C and 150 bars at a flow rate of 40 kg/kg of turmeric for 1 hour. The de-oiled turmeric powder was then extracted with 9 L of acetic acid at 60 °C for 30 5 minutes. The acetic acid was filtered and concentrated under vacuum to 500 mL volume. The concentrated extract was then added to water, 5 L at 15 °C. The precipitated curcuminoids were then filtered and washed repeatedly with 500 mL fresh cold water at a temperature of 15 °C. The partially purified curcuminoids were air dried and put in the extractor. Acetic acid, total 300 mL, was pumped as co-solvent (with supercritical C02) in three steps. At each step 100 mL acetic acid was pumped over a period of 1 minute. This step was repeated 2 more times to precipitate almost pure curcuminoids in the extractor. They were then washed with cold acetic acid to finally obtain and heavy metal curcuminoids 95 % pure, 75 g.
Example 4 for the fourth embodiment (process (400)):
Finely powdered turmeric, 3 kg, was extracted with supercritical C02 at 45 °C and 150 bars at a flow rate of 40 kg/kg of turmeric for 1 hour. To the turmeric, now de- oiled, acetic acid, total 300 mL, was pumped as co-solvent (with supercritical C02) in three steps. At each step 100 mL acetic acid was pumped over a period of 1 minute. This step was repeated 2 more times. The acetic acid treated turmeric powder was then extracted with 9 L of acetic acid at 60 °C for 30 minutes. The acetic acid was filtered and concentrated under vacuum to 500 mL volume. The concentrated extract was then fed to the extractor and subjected to extraction with supercritical C02 at 45 °C and 150 bars to remove non curcuminoids and acetic acid leaving curcuminoids 95% pure in the extractor. They were finally washed with cold acetic acid and dried to obtain and heavy metal curcuminoids 95 % pure, 75 g.
Advantages of the invention
1. Each process (100), (200), (300) and (400) uses green solvents that are used as food additives since time immemorial. C02 in the supercritical phase is a green solvent that leaves no trace in the extract after conversion to the gaseous state.
Each process (100), (200), (300) and (400) uses acetic acid that has a significant effect on the acceptability by regulatory authorities and consumers alike.
Each process (100), (200), (300) and (400) involves acetic acid dissolution and re-precipitation in water that removes all previous traces of organic solvents and heavy metals from the extracted curcuminoids.
The foregoing objects of the invention are accomplished and the problems and shortcomings associated with prior art techniques and approaches are overcome by the present invention described in the present embodiment. Detailed descriptions of the preferred embodiment are provided herein; however, it is to be understood that the present invention may be embodied in various forms. Therefore, specific details disclosed herein are not to be interpreted as limiting, but rather as a basis for the claims and as a representative basis for teaching one skilled in the art to employ the present invention in virtually any appropriately detailed system, structure, or matter. The embodiments of the invention as described above and the methods disclosed herein will suggest further modifications and alterations to those skilled in the art. Such further modifications and alterations may be made without departing from the spirit and scope of the invention.

Claims

I CLAIM:
1. A process (100) for extraction of curcuminoids, the process (100) comprising: a) treating finely powdered turmeric with any one of supercritical fluid alone and supercritical fluid in combination with co-solvent at temperature ranging between
35 to 150 °C, at pressure ranging from 80-900 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric to remove essential oils therefrom and obtain de-oiled turmeric; b) pumping of co-solvent over the de-oiled turmeric in three steps while continuing the step of supercritical fluid extraction at a temperature ranging between
32 to 150 °C, pressure ranging from 80-900 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric to remove non curcuminoids from the de-oiled turmeric while selectively keeping curcuminoids therein; c) extracting remaining residue from the product of step (b) in a solvent to obtain an extract containing curcuminoids, wherein the solvent is preferably acetic acid used at a concentration of 1 to 10 times by weight, at temperature ranging from 35 to 80 0C, under stirring for a duration of 15 minutes to 2 hours; d) crystallizing the curcuminoids from the extract at a temperature ranging between 18-30 °C; and e) filtering the crystallized curcuminoids, washing and drying to obtain totally solvent and heavy metal free dried curcuminoids.
2. The process (100) as claimed in claim 1, further comprising repeating the step (c) to combine, filter and concentrate resulting extracts.
3. The process (100) as claimed in claim 1, wherein the supercritical fluid used in step (a) is selected from any one of supercritical C02, propane, butane, R22, R134, N20 and combinations thereof, the supercritical fluid is preferably supercritical C02.
4. The process (100) as claimed in claim 1, wherein the co-solvent used in step (a) and step (b) is selected from any one of acetic acid, hexane, ether, ethyl acetate, acetone, methanol, ethanol, isopropyl alcohol or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50%, the co- solvent is preferably acetic acid pumped at a concentration of about 3% of the de- oiled turmeric over a period ranging from 0.5 to 10 minutes.
5. The process (100) as claimed in claim 1, wherein the solvent used in step (c) is selected from any one of acetic acid, hexane, ether, ethyl acetate, acetone, methanol, ethanol, isopropyl alcohol or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50%.
6. The process (100) as claimed in claim 1, wherein the washing at step (e) is done with cold acetic acid at a temperature ranging between 18-30 °C.
7. A process (200) for extraction of curcuminoids, the process (200) comprising: a) treating finely powdered turmeric with any one of supercritical fluid alone and supercritical fluid in combination with co-solvent at temperature ranging between 35 to 150 °C, at pressure ranging from 80-900 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric to remove essential oils therefrom and obtain de-oiled turmeric; b) pumping of co-solvent over the de-oiled turmeric in three steps while continuing the step of supercritical fluid extraction at a temperature ranging between 32 to 150 °C, pressure ranging from 80-900 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric to remove non curcuminoids from the de-oiled turmeric while selectively keeping curcuminoids therein; c) extracting remaining residue from the product of step (b) in a solvent to obtain an extract containing curcuminoids, wherein the solvent is preferably acetic acid used at a concentration of 1 to 10 times by weight, at temperature ranging from 35 to 80 °C, under stirring for a duration of 15 minutes to 2 hours; d) adding extract obtained from step (c) in any one of cold water and hot water as a continuous flowing stream to precipitate curcuminoids and to remove water soluble impurities therefrom at a temperature ranging from 0 to 100 °C; e) separating the precipitated curcuminoids and washing repeatedly with any one of cold water and hot water as a continuous flowing stream to obtain partially purified curcuminoids ; f) drying the partially purified curcuminoids and thereafter putting in an extractor; g) pumping co-solvent with supercritical fluid over the dried curcuminoids in three steps to precipitate almost pure curcuminoids in the extractor; and h) washing the pure curcuminoids to finally obtain totally solvent and heavy metal free dried curcuminoids.
8. The process (200) as claimed in claim 1, further comprising repeating the step (c) to combine, filter and concentrate resulting extracts.
9. The process (200) as claimed in claim 1, wherein the solvent used in step (c) is selected from any one of acetic acid, hexane, ether, ethyl acetate, acetone, methanol, ethanol, isopropyl alcohol or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50%.
10. The process (200) as claimed in claim 1, wherein the supercritical fluid used in step (a) and (g) is selected from any one of supercritical C02, propane, butane, R22, R134, N20 and combinations thereof, the supercritical fluid is preferably supercritical C02.
11. The process (200) as claimed in claim 1, wherein the co-solvent used in step (a), (b) and (g) is selected from any one of acetic acid, hexane, ether, ethyl acetate, acetone, methanol, ethanol, isopropyl alcohol, or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50%, the co- solvent is preferably acetic acid pumped at a concentration of about 3% of the de- oiled turmeric over a period ranging from 0.5 to 10 minutes.
12. The process (200) as claimed in claim 1, wherein the washing at step (h) is done with cold acetic acid at a temperature ranging between 18-30 °C.
13. A process (300) for extraction of curcuminoids, the process (300) comprising: a) treating finely powdered turmeric with any one of supercritical fluid alone and supercritical fluid in combination with co-solvent at temperature ranging between 35 to 150 °C, at pressure ranging from 80-900 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric to remove essential oils therefrom and obtain de-oiled turmeric; b) extracting the de-oiled turmeric with solvent, wherein the solvent is preferably acetic acid used at a concentration of 1 to 10 times by weight, at temperature ranging from 35 to 80 °C, under stirring for a duration of 15 minutes to 2 hours; c) adding extract obtained from step (b) to water to precipitate the curcuminoids along with impurities such as non curcuminoids; d) filtering the precipitated curcuminoids and impurities and washing repeatedly with any one of cold water and hot water as a continuous flowing stream to obtain partially purified curcuminoids; e) drying the partially purified curcuminoids and thereafter putting in an extractor; f) pumping co-solvent with supercritical fluid over the dried curcuminoids in three steps to precipitate almost pure curcuminoids in the extractor; and g) washing the almost pure curcuminoids to finally obtain totally solvent and heavy metal free dried curcuminoids.
14. The process (300) as claimed in claim 1, further comprising repeating the step (b) to combine, filter and concentrate resulting extracts.
15. The process (300) as claimed in claim 1, wherein the solvent used in step (b) is selected from any one of acetic acid, hexane, ether, ethyl acetate, acetone, methanol, ethanol, isopropyl alcohol or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50%.
16. The process (300) as claimed in claim 1, wherein the supercritical fluid used in step (a) and (f) is selected from any one of supercritical C02, propane, butane, R22, R134, N20 and combinations thereof, the supercritical fluid is preferably supercritical C02.
17. The process (300) as claimed in claim 1, wherein the co-solvent used in step (a) and (f) is selected from any one of acetic acid, hexane, ether, ethyl acetate, acetone, methanol, ethanol, isopropyl alcohol or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50%, the co- solvent is preferably acetic acid pumped at a concentration of about 3% of the de- oiled turmeric over a period ranging from 0.5 to 10 minutes.
18. The process (300) as claimed in claim 1, wherein the washing at step (g) is done with cold acetic acid at a temperature ranging between 18-30 °C.
19. A process (400) for extraction of curcuminoids, the process (400) comprising: a) treating finely powdered turmeric with any one of supercritical fluid alone and supercritical fluid in combination with co-solvent at temperature ranging between 35 to 150 °C, at pressure ranging from 80-900 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric to remove essential oils therefrom and obtain de-oiled turmeric; b) pumping of co-solvent over the de-oiled turmeric in three steps while continuing the step of supercritical fluid extraction at a temperature ranging between 32 to 150 °C, pressure ranging from 80-900 bars, and at a flow rate ranging from 10 to 250 kg/kg of the turmeric to remove non curcuminoids from the de-oiled turmeric while selectively keeping curcuminoids therein; c) extracting remaining residue from the product of step (b) in solvent to obtain an extract containing curcuminoids, wherein the solvent is preferably acetic acid used at a concentration of 1 to 10 times by weight, at temperature ranging from 35 to 80 °C, under stirring for a duration of 15 minutes to 2 hours such that the resulting extract having solvent preferably acetic acid ranging from 5 to 99.5 % of the total mass; d) re-extracting the extract obtained from step (c) with supercritical fluid in an extractor at temperatures between 35 to 150 °C, pressure ranging from 80-700 bars, at a flow rate ranging from 10 to 250 kg/kg of turmeric to remove non curcuminoids and acetic acid and precipitating almost pure curcuminoids; e) washing the precipitated almost pure curcuminoids to obtain almost pure curcuminoids; and f) drying the almost pure curcuminoids to obtain a totally solvent and heavy metal free dried curcuminoids.
20. The process (400) as claimed in claim 1, further comprising repeating the step (c) to combine, filter and concentrate resulting extracts.
21. The process (400) as claimed in claim 1, wherein the supercritical fluid used in step (a) and step (d) is selected from any one of supercritical C02, propane, butane,
R22, R134, N20 and combinations thereof, the supercritical fluid is preferably supercritical C02.
22. The process (400) as claimed in claim 1, wherein the co-solvent used in step (a) and (b) is selected from any one of acetic acid, hexane, ether, ethyl acetate, acetone, methanol, ethanol, isopropyl alcohol, or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50%, the co- solvent is preferably acetic acid pumped at a concentration of about 3% of the de- oiled turmeric over a period ranging from 0.5 to 10 minutes.
23. The process (400) as claimed in claim 1, wherein the solvent used in step (c) is selected from any one of acetic acid, hexane, ether, ethyl acetate, acetone, methanol, ethanol, isopropyl alcohol, or a combination of water with the above mentioned solvents, wherein water concentration can be up to 50%.
24. The process (400) as claimed in claim 1, wherein the washing at step (e) is done with cold acetic acid at a temperature ranging between 18-30 °C.
PCT/IN2017/050174 2016-05-11 2017-05-10 Process for extraction of curcuminoids WO2017195220A1 (en)

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