WO2015065214A1 - Method of producing plant extracts - Google Patents

Method of producing plant extracts Download PDF

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Publication number
WO2015065214A1
WO2015065214A1 PCT/PL2014/050071 PL2014050071W WO2015065214A1 WO 2015065214 A1 WO2015065214 A1 WO 2015065214A1 PL 2014050071 W PL2014050071 W PL 2014050071W WO 2015065214 A1 WO2015065214 A1 WO 2015065214A1
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WIPO (PCT)
Prior art keywords
extract
porosity
mpa
pressure
under
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PCT/PL2014/050071
Other languages
French (fr)
Inventor
Magdalena NIEWIADOMSKA
Michał JANKOWSKI
Anna KARCZEWSKA
Katarzyna KICIAK
Original Assignee
Biopoint M Jankowski M Niewiadomska Spółka Jawna
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Application filed by Biopoint M Jankowski M Niewiadomska Spółka Jawna filed Critical Biopoint M Jankowski M Niewiadomska Spółka Jawna
Priority to EP14815454.5A priority Critical patent/EP3076803A1/en
Publication of WO2015065214A1 publication Critical patent/WO2015065214A1/en

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
    • B01D61/025—Reverse osmosis; Hyperfiltration
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K10/00—Animal feeding-stuffs
    • A23K10/30—Animal feeding-stuffs from material of plant origin, e.g. roots, seeds or hay; from material of fungal origin, e.g. mushrooms
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K20/00—Accessory food factors for animal feeding-stuffs
    • A23K20/10—Organic substances
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/105—Plant extracts, their artificial duplicates or their derivatives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/14—Ultrafiltration; Microfiltration
    • B01D61/145—Ultrafiltration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/14—Ultrafiltration; Microfiltration
    • B01D61/147—Microfiltration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/58—Multistep processes
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
    • 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

Definitions

  • the object of the invention is a method of producing plant extracts.
  • the invention applies to supplementation, human nutrition or medicine, as well as to productive animals breeding .
  • a method is known, from polish patent application. PL398673, to obtain dry extract from plants of Rosaceae family, from the fruits of black raspberry Rubus Occidentalls or from the sprouts of red raspberry Rubus idaeus, of specified chemical composition, which is obtained in the following steps: (i) crushing the raw material to the particle size of 0.5 mm to 1 mm, (ii) extraction with a solvent, (iii) removal of the solvent, (iiii) freeze-drying of the extract. From polish patent application PL307550, a method of obtaining extract from Sambucus nigra fruit by means of extraction with liquid or supercritical carbon dioxide is known, wherein dried Sambucus nigra fruit or marc.
  • the extraction is performed at the temperature of 20 - 100°C, preferably 40 - 60°C and the pressure of 80 - 300 bar, preferably 200 - 250 bar, possibly with the addition of 1 - 15 %wt . of additional solvent, the so called "entrainer".
  • a method is known, from polish patent application PL335989, to obtain extract from plant raw material applying two solvents, in an extractor containing the plant raw material, characterized in that at the temperature of 293 to 450 K and under the pressure of 5 to 5 MPa, gaseous solvent with critical temperature not exceeding 425 K, in the amount of 0.5 - 40 times the weight of the raw material being extracted, is introduced into the lower part of the extractor preferably containing inert filling above and below the raw material stratum, and a liquid solvent whose solubility in the supercritical gas in extraction conditions does not exceed 35 %wt .
  • the object of the invention is a method of producing plant extracts, characterized in that it comprises a) crushing the plant material, preferably in a homogenizer and demineralized water; b) maceration of homogenized material of step a), preferably for 24 hours in closed periodical extractors with water jacket at 20 °C; c) fractionation and concentration of the extract of step b) , using membrane techniques at the temperature from 20 °C to 25°C comprising:
  • the method according to the present invention is characterized in that at step a) the weight ratio of the plant raw material to water is at 0.1.
  • the macerating in step b) additionally comprises treatment with ultrasounds.
  • filtration in step c) also includes additional microfiltration, preferably with filters of 0.3 pm porosity, with the initial flow rate of 700 1/h, and final flow of 100 1/h, under 0.5 MPa pressure.
  • the second object of the invention is a plant extract with increased stability of active substances and lowered allergenicity, characterized in that it contains no more than 10 pg/ml of compounds with molecular mass from 10 kDa to 40 kDa. Equally preferably, the extract according to the present invention is characterized in that the maximum a w is 0.8 at 20°C.
  • the method according to the present invention enables fractioning of biologically active components from plant extracts in mild conditions, e.g. chelidonine in extract from greater celandine, carvone in extract from caraway, anethole in extract from fennel, salicin and salicylic acid from extract from willow bark, coumarine in extract from coriander, allicin in extract from garlic. Due to mild extraction (maceration) , fractionation and concentration process conditions, 2-4 times higher concentration of biologically active substances is achieved as compared to extracts obtained with membrane techniques. Still further, due to water removal from extracts, the water activity coefficient (a w ) is lowered, and such extracts are characterized with greater stability of bioactive compounds and microbiological durability.
  • mild conditions e.g. chelidonine in extract from greater celandine, carvone in extract from caraway, anethole in extract from fennel, salicin and salicylic acid from extract from willow bark, coumarine in extract from coriander, allici
  • the ultrafiltration process results in concentrating and selectively separating biologically active extract components from protein, polysaccharides, viruses, and some colorants.
  • the products obtained with the method according to the present invention are characterized with lower allergenicity. Extracts obtained with the method according to the present invention find their application in supplementation, human nutrition or medicine, as well as to productive animals breeding.
  • Garlic crushed with a mechanical homogenizer was added to demineralized water in the amount of 100 kg of garlic per 1000 kg of water. Maceration was carried out for 24 hours in closed periodical extractors with water jacket at 20°C. The applied process yielded extract containing 10 mg allicin racemate in 1 liter. Fractioning and concentration of the extract was carried out at the temperatures from 20°C to 25°C using membrane techniques according to the following sequence: 1. Preliminary filtration in order to remove solid impurities and colloid fragments - three filters with the porosity of: 20, 5 and 0.3 pm; 2.
  • Microfiltration enabling removal of colloidal impurities and germs, through filters with the porosity of 0.3 pm, with the initial flow rate of 700 1/h and final flow of 100 1/h under 5 bar (0.5 MPa) pressure; 3. Ultrafiltration allowing concentration and selective separation of biologically active substances from ballast substances, through semipermeable membranes with the porosity of 0.03 pm under 0.8 MPa pressure; 4. Reverse osmosis enabling triple concentration of the extract, with the initial at 200 1/h and the final feed flow 100 at 1/h and under 2.5 MPa pressure in Polymem membrane technique equipment, to the allicin content of 30 mg/1.
  • the extract contains residues of protein, i.e. below 10 pg/l, and water activity is at 0.7.
  • the garlic extract was added, and after mixing, the emulsion was dispersed using spray nozzle with jet diameter of 0.7 mm, heated up to 70°C. The dispersion was carried out in a chamber with the temperature of 10°C. The finished product was packed in unit packages .
  • Plant raw material was steeped with demineralized water in the proportion of 100 kg dried plants for 1000 kg of water. Maceration was carried out in closed periodical extractors for 24h, with periodical mixing, at the temperature of 20°C. Fractioning and concentration of extracts was carried out at the temperatures from 20°C to 25°C using membrane techniques according to the following sequence: 1. Preliminary filtration in order to remove solid impurities and colloid fragments - three filters with the porosity of: 20, 5 and 0.3 pm; 2. Microfiltration enabling removal of colloidal impurities and germs, through filters with the porosity of 0.3 pm, with the initial flow rate of 700 1/h and final flow of 100 1/h under 0.5 MPa pressure; 3.
  • the applied process yields greater celandine extract containing up to 80 mg/1 chelidonine or caraway extract containing up to 8.00 g/1 of carvone, or fennel extract containing up to 3.50 g/1 of anethole, or willow bark extract containing up to 0.80 g/1 of salicin and up to 1.50 g/1 of salicylic acid, or coriander extract containing up to 0.90 g/1 of coumarine.
  • the extract contains residues of protein, i.e. below 10 pg/l, and water activity is at 0.7.
  • the amount of proteins in concentrated extract is 3-4 times lower than in traditionally obtained plant extracts.
  • the concentrated extracts with the increased content of biologically active substance were micro-encapsulated in lipid matrix.
  • the plant extracts were added, and after mixing, the emulsion was fed onto a spray nozzle with jet diameter of 0.7 mm, heated up to 70°C.
  • the dispersion was carried out in a chamber with the temperature of 10°C.
  • the finished product was packed in unit packages .
  • Plant raw material was steeped with demineralized water in the proportion of 100 kg dried plants for 1000 kg of water. Maceration was carried out in closed periodical extractors for 5-10 mins, with mixing at 50-150 rpm, at the temperature of 20°C. Next, the dispersion was treated with ultrasounds twice for 5 mins with 5 mins interval. The process was carried out in pulses, with ultrasound pulse having the power of 200-500 W, frequency of 20-40 kHZ, duration of 2 seconds and interval of 1 second, and amplitude of 60%. During the process, the temperature of the dispersion did not exceed 50°C. Fractioning and concentration of extracts was carried out at the temperatures from 20°C to 25°C using membrane techniques according to the following sequence: 1.
  • Preliminary filtration in order to remove solid impurities and colloid fragments - three filters with the porosity of: 20, 5 and 0.3 ⁇ ; 2. Microfiltration enabling removal of colloidal impurities and germs, through filters with the porosity of 0.3 pm, with the initial flow of 700 1/h and final flow of 100 1/h under 0.5 MPa pressure; 3. Ultrafiltration allowing concentration and selective separation of biologically active substances from ballast substances, through semipermeable membranes with the porosity of 0.03 pm under 0.8 MPa pressure; 4. Reverse osmosis enabling triple concentration of the extract, with the initial at 200 1/h and the final feed flow 100 at 1/h and under 2.5 MPa pressure in Polymem membrane technique equipment, until obtaining quadruple concentration of extracts.
  • the extracts from willow bark or spiraea contained 6,000-9,000 pg/l and 3,000-5,000 pg/l, respectively, of polyphenol compounds.
  • willow bark extract was obtained containing 5 to 0.80 g/1 of salicin, up to 1.50 g/1 of salicylic acid, and 0.5 to 0.1 g/1 of quercetin, or spiraea exctract containing 4 to 0.50 g/1 of salicin, 1.50 g/1 of salicylic acid, and 0.6 to 0.2 g/1 of quercetin.
  • the extracts contained residues of protein, i.e. below 10 pg/l, and water activity is at 0.7.
  • the amount of proteins in concentrated extract is 3-4 times lower than in traditionally obtained plant extracts.
  • the concentrated extracts with the increased content of biologically active substance were micro-encapsulated in lipid matrix.
  • plant extracts were added, and after mixing with a two-step mechanical homogenizer, emulsion was obtained, which was fed to the dispersing jet or ultrasonic disperser with the jet diameter of 0.7 mm and heated up to the temperature of 70 °C.
  • the dispersion was carried out in a chamber with the temperature of 5°C.
  • the finished product was packed in unit packages .
  • Plant raw material was steeped with demineralized water in the proportion of 100 kg dried plants for 1000 kg of water. Maceration was carried out in closed periodical extractors for 5-10 mins, with mixing at 50-150 rpm, at the temperature of 20°C. Next, the dispersion was treated with ultrasounds twice for 5 mins with 5 mins interval. The process was carried out in pulses, with ultrasound pulse having the power of 200-500 W, frequency of 20-40 kHZ, and duration of 2 seconds with 1 second interval, and the amplitude of 60%. During the process, the temperature of the dispersion did not exceed 50°C. Fractioning and concentration of extracts was carried out at the temperatures from 20°C to 25°C using membrane techniques according to the following sequence: 1.
  • Preliminary filtration in order to remove solid impurities and colloid fragments - three filters with the porosity of: 20, 5 and 0.3 ⁇ ; 2. Microfiltration enabling removal of colloidal impurities and germs, through filters with the porosity of 0.3 pm, with the initial flow of 700 1/h and final flow of 100 1/h under 0.5 MPa pressure; 3. Ultrafiltration allowing concentration and selective separation of biologically active substances from ballast substances, through semipermeable membranes with the porosity of 0.03 pm under 0.8 MPa pressure; 4. Reverse osmosis enabling triple concentration of the extract, with the initial at 200 1/h and the final feed flow 100 at 1/h and under 2.5 MPa pressure in Polymem membrane technique equipment, until obtaining quadruple concentration of extracts.
  • the extracts from Echinacea or common dandelion contained 1,000-3,000 pg/l and 2,000-4,000 pg/l, respectively, of polyphenol compounds.
  • Echinacea extract was obtained containing 0.5 to 0.05 g/1 of cichoric acid or dandelion extract containing 1 to 0.20 g/1 of cichoric acid and up to 0.1 g/1 of luteolin-7-O-glucoside .
  • the extracts contained residues of protein, i.e. below 10 pg/l, and water activity is at 0.7.
  • the amount of proteins in concentrated extract is 3-4 times lower than in traditionally obtained plant extracts.
  • the concentrated extracts with the increased content of biologically active substance were micro-encapsulated in lipid matrix.
  • plant extracts were added, and after mixing with a two-step mechanical homogenizer, emulsion was obtained, which was fed to the dispersing jet or ultrasonic disperser with the jet diameter of 0.7 mm and heated up to the temperature of 70 °C.
  • the dispersion was carried out in a chamber with the temperature of 5°C.
  • the finished product was packed in unit packages .
  • the molecular masses corresponding to specific peaks, average molecular masses (molar and weight), and polydispersion were determined.
  • the determined molecular masses of the sample are relative values, and they should be treated as molecular masses equivalent to polystyrene masses.
  • the obtained GPC chromatograms and polydispersity of the examined sample are presented in Figure 1.
  • the ratio molecules with high atomic mass ranging from 3,350 to 9, 350 Dalton is ca. 2.5% for willow bark extract after ultrafiltration.
  • Example 6 Stability of salicin extract, obtained in Example 1, encapsulated in lipid matrix was examined with accelerated method. For that purpose, examination in climatic chamber (accelerated experiment) was carried out, stimulating artificial desired climatic conditions (temperature, air humiditiy, light intensity) for 6 months, at 40°C ⁇ 2° and 75%RH ⁇ 5%RH. Table 2 presents the results of salicin in lipid matrix stability analysis in the conditions of: 40°C ⁇ 2°C, 75%RH ⁇ 5%RH.

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Abstract

The object of the invention is a method of producing plant extracts, characterized in that it comprises a) crushing the plant material, preferably in a homogenizer and demineralized water; b) maceration of homogenized material of step a), preferably for 24 hours in closed periodical extractors with water jacket at the temperature of 20°C; c) fractionation and concentration of the extract of step b), using membrane techniques at the temperature from 20°C to 25°C comprising: - preliminary filtering of solid impurities and colloids by means of a set of filters, preferably with the porosity of μm, 5 μm and 0.3 μm, and with the initial flow rate of 700 l/h, and the final of 100 l/h under the pressure of 0.5 MPa; - ultra-filtration of the permeate after preliminary filtration, preferably by means of semipermeable membranes with the porosity of 0.03 μm under 0.8 MPa pressure; d) carrying out reverse osmosis of the solution obtained in step d), preferably with the initial and final feed flow at 200 l/h and 100 l/h, respectively, and under 2.5 MPa pressure, and plant extract of reduced allergenicity and aw.

Description

Method of producing plant extracts
The object of the invention is a method of producing plant extracts. The invention applies to supplementation, human nutrition or medicine, as well as to productive animals breeding .
A method is known, from polish patent application. PL398673, to obtain dry extract from plants of Rosaceae family, from the fruits of black raspberry Rubus Occidentalls or from the sprouts of red raspberry Rubus idaeus, of specified chemical composition, which is obtained in the following steps: (i) crushing the raw material to the particle size of 0.5 mm to 1 mm, (ii) extraction with a solvent, (iii) removal of the solvent, (iiii) freeze-drying of the extract. From polish patent application PL307550, a method of obtaining extract from Sambucus nigra fruit by means of extraction with liquid or supercritical carbon dioxide is known, wherein dried Sambucus nigra fruit or marc. The extraction is performed at the temperature of 20 - 100°C, preferably 40 - 60°C and the pressure of 80 - 300 bar, preferably 200 - 250 bar, possibly with the addition of 1 - 15 %wt . of additional solvent, the so called "entrainer". A method is known, from polish patent application PL335989, to obtain extract from plant raw material applying two solvents, in an extractor containing the plant raw material, characterized in that at the temperature of 293 to 450 K and under the pressure of 5 to 5 MPa, gaseous solvent with critical temperature not exceeding 425 K, in the amount of 0.5 - 40 times the weight of the raw material being extracted, is introduced into the lower part of the extractor preferably containing inert filling above and below the raw material stratum, and a liquid solvent whose solubility in the supercritical gas in extraction conditions does not exceed 35 %wt . is introduced into the upper part in the amount of 1 to 10 times the weight of the of the raw material being extracted, and the extract in gaseous solvent is received at the top of the extractor above the liquid solvent delivery point, while the extract in liquid solvent is received at the bottom of the extractor below the gaseous solvent delivery point. From polish patent application PL204867 a method of producing extract from Ginkgo biloba leaves is known, characterized in that it comprises the following consecutives steps: (i) extraction of dry parts of Ginkgo biloba leaves with ethanol containing up to 20 %wt . of water; (ii) concentration of the extract in vacuum in the presence of water solution of sodium chloride, and removal of dark oil residues from clear extract; (iii) washing the remaining water solution by means of liquid-liquid extraction with n-hexane, n-heptane, or cyclohexane; (iv) liquid-liquid extraction of the water phase with ethyl acetate; (v) washing the ethyl acetate phase obtained in step (iv) with sodium chloride, and then evaporating the washed ethyl acetate phase until dry. All the above complex methods of obtaining plant extracts are characterized with the necessity to apply techniques utilizing chemical reactants, which are often toxic, and often in drastic physical and chemical conditions. Therefore, a simple method is sought, that would be carried out in mild conditions in absence of toxic substances in such a way as to obtain concentrated extracts of high active substances concentration and low allergenicity . The desired product obtained with the method sought for should be characterized with low water activity, i.e. be an extract that limit growth of microorganisms, thus with lower microbiological hazard risk. Unexpectedly, the problems mentioned above have been solved by the present invention.
The object of the invention is a method of producing plant extracts, characterized in that it comprises a) crushing the plant material, preferably in a homogenizer and demineralized water; b) maceration of homogenized material of step a), preferably for 24 hours in closed periodical extractors with water jacket at 20 °C; c) fractionation and concentration of the extract of step b) , using membrane techniques at the temperature from 20 °C to 25°C comprising:
- preliminary filtering of solid impurities and colloids by means of a set of filters, preferably with the porosity of 20 pm, 5 pm and 0.3 pm, with the initial flow rate of 700 1/h, the final of 100 1/h and the back pressure of 0.5 MPa;
- ultra-filtration of the permeate after preliminary filtration, preferably by means of semipermeable membranes with the porosity of 0.03 pm and the pressure of 0.8 MPa; d) carrying out reverse osmosis of the solution obtained in step d) , preferably with the initial and final feed flow at 200 1/h and 100 1/h, respectively, and under 2.5 MPa pressure . Equally preferably, the method according to the present invention is characterized in that at step a) the weight ratio of the plant raw material to water is at 0.1. In another preferable embodiment of the invention, the macerating in step b) additionally comprises treatment with ultrasounds. In another preferred embodiment of the invention, filtration in step c) also includes additional microfiltration, preferably with filters of 0.3 pm porosity, with the initial flow rate of 700 1/h, and final flow of 100 1/h, under 0.5 MPa pressure.
The second object of the invention is a plant extract with increased stability of active substances and lowered allergenicity, characterized in that it contains no more than 10 pg/ml of compounds with molecular mass from 10 kDa to 40 kDa. Equally preferably, the extract according to the present invention is characterized in that the maximum aw is 0.8 at 20°C.
The method according to the present invention enables fractioning of biologically active components from plant extracts in mild conditions, e.g. chelidonine in extract from greater celandine, carvone in extract from caraway, anethole in extract from fennel, salicin and salicylic acid from extract from willow bark, coumarine in extract from coriander, allicin in extract from garlic. Due to mild extraction (maceration) , fractionation and concentration process conditions, 2-4 times higher concentration of biologically active substances is achieved as compared to extracts obtained with membrane techniques. Still further, due to water removal from extracts, the water activity coefficient (aw) is lowered, and such extracts are characterized with greater stability of bioactive compounds and microbiological durability. The ultrafiltration process results in concentrating and selectively separating biologically active extract components from protein, polysaccharides, viruses, and some colorants. The products obtained with the method according to the present invention are characterized with lower allergenicity. Extracts obtained with the method according to the present invention find their application in supplementation, human nutrition or medicine, as well as to productive animals breeding.
Exemplary embodiments of the invention have been presented in the drawings, wherein fig. 1 presents chromatograms obtained after gel permeation chromatography (GPC) and dispersity of willow bark extract under the conditions presented in Table 1 below Table 1
Peak* Ret. Time Area Height Area % Height %
1 15.500 12862 591 2.464 2.569
2 16.008 29199 1341 5.594 5.823
3 16.317 67130 2528 12.860 10.980
4 17.073 412807 18562 79.082 80.628
Total 521999 23021 100.000 100.000
Time(min) Volume(mL) Molecular Weight Height
Peak #1
Start 14.658 14.658 9347
Top 15.500 15.500 3369
End 15.508 15.508 3326
Area : 12862
Area%: 2.4641
Average Molecular 6428
Welaht(Mw)
Peak #2
Start 15.508 15.508 3326
Top 16.008 16.008 1631
End 16.017 16.017 1613
Area : 29199
Area%: 5.5938
Average Molecular 2220
Welaht(Mw)
Peak #3
Start 16.017 16.017 1613
Top 16.317 16.317 1 104
End 16.658 16.658 747
Area : 67130
Area%: 12.8602
Averaqe Molecular 1 133
Welaht(Mw)
Peak #4
Start 16.658 16.658 747
Top 17.073 17.073 490
End 18.000 18.000 231
Area : 412807
Area%: 79.0819
Average Molecular
Welaht(Mw)
Example 1.
Garlic crushed with a mechanical homogenizer was added to demineralized water in the amount of 100 kg of garlic per 1000 kg of water. Maceration was carried out for 24 hours in closed periodical extractors with water jacket at 20°C. The applied process yielded extract containing 10 mg allicin racemate in 1 liter. Fractioning and concentration of the extract was carried out at the temperatures from 20°C to 25°C using membrane techniques according to the following sequence: 1. Preliminary filtration in order to remove solid impurities and colloid fragments - three filters with the porosity of: 20, 5 and 0.3 pm; 2. Microfiltration enabling removal of colloidal impurities and germs, through filters with the porosity of 0.3 pm, with the initial flow rate of 700 1/h and final flow of 100 1/h under 5 bar (0.5 MPa) pressure; 3. Ultrafiltration allowing concentration and selective separation of biologically active substances from ballast substances, through semipermeable membranes with the porosity of 0.03 pm under 0.8 MPa pressure; 4. Reverse osmosis enabling triple concentration of the extract, with the initial at 200 1/h and the final feed flow 100 at 1/h and under 2.5 MPa pressure in Polymem membrane technique equipment, to the allicin content of 30 mg/1. The concentrated extract with the increased content of biologically active substance, fixed by means of membrane filtration method, was micro-encapsulated in lipid matrix. The extract contains residues of protein, i.e. below 10 pg/l, and water activity is at 0.7. After liquefaction of fat at the temperature of ca. 50°C, the garlic extract was added, and after mixing, the emulsion was dispersed using spray nozzle with jet diameter of 0.7 mm, heated up to 70°C. The dispersion was carried out in a chamber with the temperature of 10°C. The finished product was packed in unit packages .
Example 2.
Plant raw material was steeped with demineralized water in the proportion of 100 kg dried plants for 1000 kg of water. Maceration was carried out in closed periodical extractors for 24h, with periodical mixing, at the temperature of 20°C. Fractioning and concentration of extracts was carried out at the temperatures from 20°C to 25°C using membrane techniques according to the following sequence: 1. Preliminary filtration in order to remove solid impurities and colloid fragments - three filters with the porosity of: 20, 5 and 0.3 pm; 2. Microfiltration enabling removal of colloidal impurities and germs, through filters with the porosity of 0.3 pm, with the initial flow rate of 700 1/h and final flow of 100 1/h under 0.5 MPa pressure; 3. Ultrafiltration allowing concentration and selective separation of biologically active substances from ballast substances, through semipermeable membranes with the porosity of 0.03 pm under 0.8 MPa pressure; 4. Reverse osmosis enabling triple concentration of the extract, with the initial at 200 1/h and the final feed flow 100 at 1/h and under 2.5 MPa pressure in Polymem membrane technique equipment, until obtaining quadruple concentration of extracts. The applied process yields greater celandine extract containing up to 80 mg/1 chelidonine or caraway extract containing up to 8.00 g/1 of carvone, or fennel extract containing up to 3.50 g/1 of anethole, or willow bark extract containing up to 0.80 g/1 of salicin and up to 1.50 g/1 of salicylic acid, or coriander extract containing up to 0.90 g/1 of coumarine. The extract contains residues of protein, i.e. below 10 pg/l, and water activity is at 0.7. The amount of proteins in concentrated extract is 3-4 times lower than in traditionally obtained plant extracts.
The concentrated extracts with the increased content of biologically active substance, fixed by means of membrane filtration method, were micro-encapsulated in lipid matrix. After liquefaction of fat at the temperature of ca. 50°C, the plant extracts were added, and after mixing, the emulsion was fed onto a spray nozzle with jet diameter of 0.7 mm, heated up to 70°C. The dispersion was carried out in a chamber with the temperature of 10°C. The finished product was packed in unit packages .
Example 3
Plant raw material was steeped with demineralized water in the proportion of 100 kg dried plants for 1000 kg of water. Maceration was carried out in closed periodical extractors for 5-10 mins, with mixing at 50-150 rpm, at the temperature of 20°C. Next, the dispersion was treated with ultrasounds twice for 5 mins with 5 mins interval. The process was carried out in pulses, with ultrasound pulse having the power of 200-500 W, frequency of 20-40 kHZ, duration of 2 seconds and interval of 1 second, and amplitude of 60%. During the process, the temperature of the dispersion did not exceed 50°C. Fractioning and concentration of extracts was carried out at the temperatures from 20°C to 25°C using membrane techniques according to the following sequence: 1. Preliminary filtration in order to remove solid impurities and colloid fragments - three filters with the porosity of: 20, 5 and 0.3 μπι; 2. Microfiltration enabling removal of colloidal impurities and germs, through filters with the porosity of 0.3 pm, with the initial flow of 700 1/h and final flow of 100 1/h under 0.5 MPa pressure; 3. Ultrafiltration allowing concentration and selective separation of biologically active substances from ballast substances, through semipermeable membranes with the porosity of 0.03 pm under 0.8 MPa pressure; 4. Reverse osmosis enabling triple concentration of the extract, with the initial at 200 1/h and the final feed flow 100 at 1/h and under 2.5 MPa pressure in Polymem membrane technique equipment, until obtaining quadruple concentration of extracts. Before concentration, the extracts from willow bark or spiraea contained 6,000-9,000 pg/l and 3,000-5,000 pg/l, respectively, of polyphenol compounds. As the result of the concentration process applied, willow bark extract was obtained containing 5 to 0.80 g/1 of salicin, up to 1.50 g/1 of salicylic acid, and 0.5 to 0.1 g/1 of quercetin, or spiraea exctract containing 4 to 0.50 g/1 of salicin, 1.50 g/1 of salicylic acid, and 0.6 to 0.2 g/1 of quercetin. The extracts contained residues of protein, i.e. below 10 pg/l, and water activity is at 0.7. The amount of proteins in concentrated extract is 3-4 times lower than in traditionally obtained plant extracts.
The concentrated extracts with the increased content of biologically active substance, fixed by means of membrane filtration method, were micro-encapsulated in lipid matrix. After liquefaction of fat at the temperature of ca. 50°C, plant extracts were added, and after mixing with a two-step mechanical homogenizer, emulsion was obtained, which was fed to the dispersing jet or ultrasonic disperser with the jet diameter of 0.7 mm and heated up to the temperature of 70 °C. The dispersion was carried out in a chamber with the temperature of 5°C. The finished product was packed in unit packages .
Example 4
Plant raw material was steeped with demineralized water in the proportion of 100 kg dried plants for 1000 kg of water. Maceration was carried out in closed periodical extractors for 5-10 mins, with mixing at 50-150 rpm, at the temperature of 20°C. Next, the dispersion was treated with ultrasounds twice for 5 mins with 5 mins interval. The process was carried out in pulses, with ultrasound pulse having the power of 200-500 W, frequency of 20-40 kHZ, and duration of 2 seconds with 1 second interval, and the amplitude of 60%. During the process, the temperature of the dispersion did not exceed 50°C. Fractioning and concentration of extracts was carried out at the temperatures from 20°C to 25°C using membrane techniques according to the following sequence: 1. Preliminary filtration in order to remove solid impurities and colloid fragments - three filters with the porosity of: 20, 5 and 0.3 μπι; 2. Microfiltration enabling removal of colloidal impurities and germs, through filters with the porosity of 0.3 pm, with the initial flow of 700 1/h and final flow of 100 1/h under 0.5 MPa pressure; 3. Ultrafiltration allowing concentration and selective separation of biologically active substances from ballast substances, through semipermeable membranes with the porosity of 0.03 pm under 0.8 MPa pressure; 4. Reverse osmosis enabling triple concentration of the extract, with the initial at 200 1/h and the final feed flow 100 at 1/h and under 2.5 MPa pressure in Polymem membrane technique equipment, until obtaining quadruple concentration of extracts. Before concentration, the extracts from Echinacea or common dandelion contained 1,000-3,000 pg/l and 2,000-4,000 pg/l, respectively, of polyphenol compounds. As the result of the applied concentration process, Echinacea extract was obtained containing 0.5 to 0.05 g/1 of cichoric acid or dandelion extract containing 1 to 0.20 g/1 of cichoric acid and up to 0.1 g/1 of luteolin-7-O-glucoside . The extracts contained residues of protein, i.e. below 10 pg/l, and water activity is at 0.7. The amount of proteins in concentrated extract is 3-4 times lower than in traditionally obtained plant extracts.
The concentrated extracts with the increased content of biologically active substance, fixed by means of membrane filtration method, were micro-encapsulated in lipid matrix. After liquefaction of fat at the temperature of ca. 50°C, plant extracts were added, and after mixing with a two-step mechanical homogenizer, emulsion was obtained, which was fed to the dispersing jet or ultrasonic disperser with the jet diameter of 0.7 mm and heated up to the temperature of 70 °C. The dispersion was carried out in a chamber with the temperature of 5°C. The finished product was packed in unit packages .
Example 5
Willow bark extract was subjected to examination for ballast protein presence. Determination of molecular mass and molecular mass distribution of the sample was carried out using GPC method; examination methodology adapted individually to the sample. GPC chromatograms were recorded on SPV20-AV chromatograph from Schimadzu. Chromatographic separation conditions :
- Phenomenex column, temperature of the column: 40 °C,
- eluent: tetrahydrofuran (THF) - flow rate: 1 ml/min,
- flow: isocratic
- refractometric detector. Qualitative parameters:
- retention time deviation below 0.2%,
- column separation efficiency, determined for benchmarks: PS 5120 and PS 1620 is at 4.32.
The molecular masses corresponding to specific peaks, average molecular masses (molar and weight), and polydispersion were determined. The determined molecular masses of the sample are relative values, and they should be treated as molecular masses equivalent to polystyrene masses. The obtained GPC chromatograms and polydispersity of the examined sample are presented in Figure 1. The ratio molecules with high atomic mass ranging from 3,350 to 9, 350 Dalton is ca. 2.5% for willow bark extract after ultrafiltration.
Example 6 Stability of salicin extract, obtained in Example 1, encapsulated in lipid matrix was examined with accelerated method. For that purpose, examination in climatic chamber (accelerated experiment) was carried out, stimulating artificial desired climatic conditions (temperature, air humiditiy, light intensity) for 6 months, at 40°C ± 2° and 75%RH ± 5%RH. Table 2 presents the results of salicin in lipid matrix stability analysis in the conditions of: 40°C ± 2°C, 75%RH ± 5%RH.
Figure imgf000013_0001
Table 2
The following method to determine mark salicin in willow extract was applied:
RP18 Column (250 mm/4 pm) ,
Detector wave length: 213 nm Flow rate of the mobile phase: lmL/min
Mobile phase composition: A-acetonitrile, B-water
Flow gradient:
0-5min - 100% B 5-30min from 0%A+100%B to 80%A+20%B
Examination in the climatic chamber for six months demonstrated insignificant (below 10%) loss of concentration of the active substances as compared to the initial concentration. Based on the examination results, it can be assumed that the product is stable and retains proper activity during the observation period.

Claims

Claims
1. Method of producing plant extracts, characterized in that it comprises a) crushing the plant material, preferably in a homogenizer and demineralized water; b) maceration of homogenized material of step a), preferably for 24 hours in closed periodical extractors with water jacket at 20 °C; c) fractionation and concentration of the extract of step b) , using membrane techniques at the temperature from 20 °C to 25°C comprising:
- preliminary filtering of solid impurities and colloids by means of a set of filters, preferably with the porosity of 20 pm, 5 pm and 0.3 pm, with the initial flow rate of 700 1/h, the final of 100 1/h and the back pressure of 0.5 MPa;
- ultra-filtration of the permeate after preliminary filtration, preferably by means of semipermeable membranes with the porosity of 0.03 pm and the pressure of 0.8 MPa pressure ; d) carrying out reverse osmosis of the solution obtained in step d) , preferably with the initial and final feed flow at 200 1/h and 100 1/h, respectively, and under 2.5 MPa pressure.
2. The method of claim 1 characterized in that at step a) the weight ratio of the plant raw material to water is at 0.1.
3. The method of claim 1 or 2, characterized in that the maceration in step b) additionally comprises treatment with ultrasounds .
4. The method of any of claims 1 to 3, characterized in that at step c) the filtration comprises also microfiltration, preferably with filters of 0.3 pm porosity, with the initial flow rate of 700 1/h, and final flow of 100 1/h, under 0.5 MPa pressure.
5. Plant extract with increased stability of active substances, and reduced allergenicity , characterized in that it contains no more than 10 pg/ml of compounds with molecular mass from 10 kDa to 40 kDa.
6. Extract of claim 5 characterized in that the maximum aw is 0.8 at 20°C
PCT/PL2014/050071 2013-10-30 2014-10-30 Method of producing plant extracts WO2015065214A1 (en)

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PL245420B1 (en) 2022-03-03 2024-07-22 Fortifruits Spolka Z Ograniczona Odpowiedzialnoscia Method for producing fruit or plant powder with fruit or plant extract with increased content of bioactive compounds and fruit or plant powder with fruit or plant extract with increased content of bioactive compounds

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