WO2013141723A1 - Préparation de pectine et de compositions polyphénoliques à partir de pelures de mangue - Google Patents

Préparation de pectine et de compositions polyphénoliques à partir de pelures de mangue Download PDF

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WO2013141723A1
WO2013141723A1 PCT/PH2013/000009 PH2013000009W WO2013141723A1 WO 2013141723 A1 WO2013141723 A1 WO 2013141723A1 PH 2013000009 W PH2013000009 W PH 2013000009W WO 2013141723 A1 WO2013141723 A1 WO 2013141723A1
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pectin
mango
composition
alcohol
peel powder
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Evelyn TABOADA
Francis Dave SIACOR
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Taboada Evelyn
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
    • C08B37/0045—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Galacturonans, e.g. methyl ester of (alpha-1,4)-linked D-galacturonic acid units, i.e. pectin, or hydrolysis product of methyl ester of alpha-1,4-linked D-galacturonic acid units, i.e. pectinic acid; Derivatives thereof
    • 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
    • A23K10/37—Animal feeding-stuffs from material of plant origin, e.g. roots, seeds or hay; from material of fungal origin, e.g. mushrooms from waste material
    • 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
    • A23K20/111—Aromatic compounds
    • 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
    • A23K20/163—Sugars; Polysaccharides
    • 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
    • A23L19/00—Products from fruits or vegetables; Preparation or treatment thereof
    • A23L19/03—Products from fruits or vegetables; Preparation or treatment thereof consisting of whole pieces or fragments without mashing the original pieces
    • A23L19/07—Fruit waste products, e.g. from citrus peel or seeds
    • 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
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/231—Pectin; Derivatives thereof
    • 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
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
    • A23L3/3463—Organic compounds; Microorganisms; Enzymes
    • A23L3/3472—Compounds of undetermined constitution obtained from animals or plants
    • 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
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00—Medicinal preparations containing organic active ingredients
    • A61K31/70—Carbohydrates; Sugars; Derivatives thereof
    • A61K31/715—Polysaccharides, i.e. having more than five saccharide radicals attached to each other by glycosidic linkages; Derivatives thereof, e.g. ethers, esters
    • A61K31/732—Pectin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/22—Anacardiaceae (Sumac family), e.g. smoketree, sumac or poison oak
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783—Angiosperms [Magnoliophyta]
    • A61K8/9789—Magnoliopsida [dicotyledons]
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A61Q19/10—Washing or bathing preparations
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
    • C08L5/06—Pectin; Derivatives thereof
    • 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
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/10—General cosmetic use
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
    • Y02P60/80—Food processing, e.g. use of renewable energies or variable speed drives in handling, conveying or stacking
    • Y02P60/87—Re-use of by-products of food processing for fodder production

Definitions

  • This invention pertains to the improved integrated processes in the recovery of pectin from mango peels and the subsequent preparation of polyphenolic compositions derived thereof.
  • Mango peels are commonly regarded as waste by-products in fruit processing; and in tropical countries, these are oftentimes simply dumped in landfills and open dumpsites.
  • Said mango peels also exhibit good antioxidative and antimicrobial activities which are attributed to its high polyphenolic content.
  • pectin and polyphenolic compositions can be recovered more efficiently from mango peels by the implementation of an improved integrated process.
  • the said compositions resulting from this improved process can readily be used as ingredients in food and functional food preparations, in nutraceuticals, cosmetics, and pharmaceutical applications.
  • Mango peel is a significant by-product or waste from mango processing industries. Studies showed that the mango (Mangifera indica L. Anacardiacea, Indian variety) peels contain a considerable amount of carbohydrates (20.8 -28.2%), crude fibre (3.28-7.4%), protein (1.45-2.05%), fat (2.16-2.66%), moisture (66.0-75.25%) and ash (1.30-3.0%) [Ajila CM, Bhat SG, Prasada Rao UJS, Valuable components of raw and ripe peels from two Indian mango varieties, Food Chemistry 2007a, 102, 1006-101 1].
  • mango peel of Indian variety is similar to the peels of mango (Mangifera indica L., Hayden Cuban variety), which has soluble dietary fiber - 21.6-28.1%, insoluble dietary - 12.8-23.8%, ash - 2.85%, protein - 5.25%, oil - 2.5%, total sugar (soluble fiber) - 21.6%, and total sugar (insoluble fiber) - 12.8% [Larrauri JA, Ruperez P, Borroto B, and Saura-Calixto F, Mango peels as a new tropical fibre: Preparation and characterization. Deutschen-Wissenschaft und -Technologie 1996, 29,729-733].
  • the bambangan fruit ⁇ Mangifera pajang K. which is three times as large as commercial mango (Mangifera indica), found in Malaysia, Brunei, and Indonesia, contain about 27% peels, which has a proximate analysis of: moisture - 3.9%, protein - 4.6%, fat - 2.9%, ash - 2.7 %, carbohydrate - 7.3% and total dietary fiber - 72.3% [Hassan FA, Ismail A, Hamid AA, Azlan A, Al-sheraji SH. Characterization of fibre-rich powder and antioxidant activity of Mangifera pajang K. fruit peels. Food Chemistry 2011, 126, 283-288]. Such examples show that mango peels contain indeed a considerable amount of carbohydrates and crude fiber, which are sources of sugars, soluble and insoluble dietary fiber and bioactive components, the latter of which is attributed to the antioxidant activity of the peels.
  • mango peels also contain a considerable amount of pectin, which is usually expressed in terms of galacturonic acid composition.
  • Pectin is a structural polysaccharide found in the primary cell walls of terrestrial plants. It is produced commercially as a white to light brown powder, mainly extracted from citrus and apple peels and is used in food as a gelling agent and as a source of beneficial dietary fiber, used in fillings, medicines, and sweets, and as a stabilizer in fruit juices and milk drinks. Peels of two Guinean mango varieties (Ceni and Springfield) has reportedly 24.5% and 22.3%» of pectin for Ceni and Springfield varieties, respectively [Kratchanova M, Benemou C, Kratchanov C.
  • Mango peels of Pakistan variety were also reported to have 21.0% pectin yield at optimum conditions investigated [Rehman ZU, Salariya AM, Habib F, Shah WH. Utilization of Mango Peels as a Source of Pectin. Journal Chemical Society of Pakistan 2004, 26(1), 73-76]. Similar findings are also obtained in other studies [Srirangarajan AN andshrikhande AJ, Mango peel waste as a source of pectin. Current Sciencel916, 45, 620- 621 ; Tandon DK and Garg N, Mango waste: A potential source of pectin, fiber, and starch.
  • mango peels are proven to be a good source of bioactive compounds.
  • bioactive compounds such as polyphenols (33.31-73.88 mg/g powder by alcohol extraction and 54.67-109.7 mg/g powder by acetone extraction), carotenoids (365-3,945 ⁇ g/g powder), vitamin C (188-392 ⁇ g/g powder), and vitamin E (205-509 ⁇ g/g peel powder)
  • polyphenols 33.31-73.88 mg/g powder by alcohol extraction and 54.67-109.7 mg/g powder by acetone extraction
  • carotenoids 365-3,945 ⁇ g/g powder
  • vitamin C 188-392 ⁇ g/g powder
  • vitamin E 205-509 ⁇ g/g peel powder
  • mango peel powder MPP
  • proximate analysis as shown in Table 1
  • bioactive components more specifically, its total polyphenolic and anthocyanin content, as shown in Table 2 below:
  • TMA Total Monomeric Anthocyanins
  • Said composition shows a considerable amount of fats/oils, which is an important composition, derived thereof and also crude fiber and carbohydrates.
  • the latter two components are the sources of dietary fibers, sugars, and polysaccharides which have reportedly good health benefits.
  • mango peel powder also contains 130 high total polyphenol content which is attributed to its good antioxidant and antimicrobial activities.
  • Beet pulp was tapped as source of pectin in a patent US 5,071,970 by Le Grand and 135 Stevens (1990).
  • beet pulp was reduced to small particle size and hydrolyzed in HCl at a low temperature for a long time and then peptized in hot water at 60-70°C for about one hours to produce an aqueous pulp slurry that is screened to recover the liquid which is filtered and mixed with aluminum chloride to lower the pH about 0.1 pH unit to the range of 1.8-2.25 pH.
  • Ammonium hydroxide is then added to 140 raise the pH to about 4.0-4.5 to form an aluminum pectinate precipitate, which is washed with an acidified alcoholic liquid to produce high-to-medium methoxyl pectin which is separated and dried to a stable powder. Waste streams are converted to animal feed or are recovered and recycled.
  • a EU patent 0664300 or US 6,143,346 by Glahn (1994) relates to pectin compositions and processes for preparing the same, obtained from lime, lemon, grapefruit, and orange.
  • Said pectin composition has a high degree of esterification greater than 60% and a ratio of calcium sensitive pectin to the sum of calcium sensitive pectin and non-calcium sensitive pectin greater than 0.65.
  • a patent WO 00/24921 by Banister et al. (1998) relates to methods and reagents for preparing pectin from tomato, banana, and orange, especially the high molecular weight pectin having a high methoxyl content which can form a gel or a viscous solution in the presence of polyvalent metal ions such as calcium ions.
  • a patent US 6,787,177 by Crandall and McCain (2000) also revealed a process for extracting pectin from waste hull/hypocotyl streams during soybean processing.
  • a soy pectin material was obtained comprising about 40% wt anhydrous galacturonic acid and about 8%wt protein.
  • Chemical extraction agents in addition to 160 or in conjunction with heat and agitation are used to extract pectin from the waste streams.
  • the pectin is then precipitated in alcohol, washed and dried. Yield reported was 5.6% of pectin material.
  • pectin from a group of pectin-containing materials such as citrus fruit, apple, sugar beet, sunflower soybean, and mixtures thereof, comprising the treatment of said materials in aqueous medium with cellulase and hemicellulase enzymes, to release pectin from said pectin-containing materials, thereby forming a pectin solution.
  • pectin-containing materials such as citrus fruit, apple, sugar beet, sunflower soybean, and mixtures thereof.
  • High-quality pectins may be extracted from pectin-containing plant materials with microwave energy under pressure as described in a patent WO 00/65929 by Fishman and Chau (1999).
  • the pectin obtained is characterized by increased molecular weight, size and intrinsic viscosity when compared to pectin extracted by conventional heating techniques.
  • a patent US 4,686,187 by Sakai and atsuragi (1981) revealed a different process for preparing pectin by subjecting a plant tissue containing pectic substances, such as Citrus unshiu and Citrus natsudaidai to the action of microorganism, which possesses an activity liberating pectin from a plant tissue, or of a culture broth or processed material thereof to liberate pectin from said plant tissue and subsequently recovering the pectin.
  • pectic substances such as Citrus unshiu and Citrus natsudaidai
  • Microorganisms used in said process belongs to the genus Endomyces, Endomycopsis, Saccharomyces, Shizosaccharomyces, Pichia, Hansenula, Debaryomyces, Hanseniaspora, Torulopsis, Candisa or Kluyveromyces. Although such a process is novel, it results in very low yield (up to 9% only) of the pectic material.
  • pectin 190
  • the processes for preparing pectin are well-known, as are the many uses for this product composition.
  • the typical pectin processes include the following steps:
  • the pectin-containing material which is usually a plant material, is treated with dilute acid solutions such as nitric, sulfuric, hydrochloric, or other inorganic or organic acids to remove the pectin from the cellulose components of the
  • the commonly used plant starting materials are citrus peels from juice production and apple pomace from apple juice and cider production.
  • the 205 are selected such that a majority of the pectin molecules contained in the plant material is extracted and transferred to the extracting medium.
  • the quantity and quality of the extracted pectin depends on the raw material source and the selection and control of the extraction conditions such as pH, temperature and extraction time.
  • a mixture containing the pectin-containing liquid and the spent plant material is formed.
  • This mixture is then subjected to further purification, which is the second step herein, in which the solid plant material is removed by filtration, centrifugation, or other conventional separation steps.
  • the 215 extract can, optionally, be further purified by ion-exchange, adsorption, and concentrated by evaporation of part of the water.
  • the purification step can be carried out by reverse osmosis, concentrating and purifying the extract in the same step.
  • the pectin in the acid extract can also be isolated by reacting with aluminum salts after adjusting the pH.
  • the aluminum pectinate gel thus formed is treated with alcohol/acid mixture to wash out the aluminum salt and transformed the pectin into pectic acid.
  • the pectic acid can then be neutralized and a substantial amount of the water is removed by washing with slightly alkaline alcohol.
  • the pectin is isolated by treating the pectin solution with appropriate alcohol to render the pectin insoluble in the ensuing blend of alcohol and water.
  • appropriate alcohol Any alcohol or other organic solvent miscible with water can be used, most often ethanol, methanol, or isopropyl alcohol.
  • the insolubilized pectin is separated from the 230 alcohol/water mixture by appropriate means such as filtration, centrifugation, etc.
  • the resulting pectin is dried and milled to the desired particle size.
  • Pectins produced industrially are made up primarily of polygalacturonic acid chains in which rhamnose may be found. Natural sugars may be attached to the rhamnose
  • the anhydrogalacturonic acid makes up at least 65% of the dry matter in commercial type pectins.
  • the galacturonic acids are partly esterified with methyl alcohol. According to convention, pectins with more than 50% of the carboxylic acid groups esterified with methyl alcohol are referred to as high methoxyl pectins, having a corresponding degree of esterification (% DE) of greater than 50%; whereas pectins
  • low methoxyl pectins with less than 50% of the carboxylic groups esterified with methyl alcohol are called low methoxyl pectins, with corresponding degree of esterification (% DE) of less than 50%.
  • the extract as obtained by the commercial production is composed of those molecules 245 that are soluble under the conditions of pH, temperature, and incubation time used during the extraction.
  • the extract is composed of a mixture of molecules which differ according to molecular weight, distribution of molecular weight, and degree of esterification.
  • Figure 1 shows a simple process flow diagram of the integrated process in the treatment of mango wastes of fruit processing described fully in a related invention, whereby the immediately resulting compositions in this process are indicated, namely: mango peel powder (MPP), mango seed kernel powder (MSKP), mango seed husks (MSH) or mango seed husk powder (MSHP), and the corresponding defatted or oil- extracted compositions from such compositions above.
  • MPP mango peel powder
  • MSKP mango seed kernel powder
  • MSH mango seed husks
  • MSHP mango seed husk powder
  • the corresponding fat/oil extracts from the plurality of compositions can also be in pure or combined form.
  • Figure 2 shows a process flow diagram which is a continuation of the integrated process in the treatment of mango wastes of fruit processing as shown in Figure 1, wherein process steps are added to treat further the defatted mango peel powder (MPP*) to obtain the mango pectin and the polyphenolic compositions.
  • MPP* defatted mango peel powder
  • mango peel powder which is obtained by treating mango ⁇ Mangifera indica L. Anacardiacea v. Philippine) peels, characterized by its proximate analysis: moisture 4-7%, ash 4-7%, protein 3-5%,
  • a composition referred to as mango peel oil extract characterized in that said 300 composition is composed mainly of fats/oils derived from the mango peel powder
  • composition referred to herein as polyphenolic concentrate A characterized in that said composition contains relatively very high concentrations of polyphenolic compounds derived from the mango peel powder (MPP), which is obtained earlier
  • the object of the invention is the improved process in the recovery of pectin and polyphenolic compositions, which can be combined with the integrated process, 310 which is the object of the related invention described in Figure 1 herein.
  • the said improved process is comprised of the following steps:
  • step (b) Separation of the filtrate or liquid extract resulting in step (a) from the spent mango peel powder, by simple decantation after settling of the spent MPP* or by simple filtration using cheesecloth, or a combination of these two steps,
  • step (c) Alcoholic precipitation of pectin from the filtrate or liquid extract obtained in step (b), combined with mixing-settling processes, whereby ethanol or
  • 320 methanol is employed, preferably ethanol at a volumetric ratio of 1 :5
  • step (d) Purification of the alcoholic solution obtained in step (c) after separation of the wet pectin precipitate, preferably combined with the recovery of the alcohol from the alcoholic solution obtained during the said process step (c), and 325 recycling said alcohol back to process step (c), and
  • the improved process in the recovery of pectin and polyphenolic compositions which is the object of this invention, is characterized in that the said improved process:
  • 330 i. employs the defatted mango peel powder derived from the mango peel powder (MPP), both of which are obtained in the integrated process of a related invention,
  • pectin yield is defined as the amount of pectin obtained based on the amount of defatted mango peel powder used as starting material for the process.
  • the degree of esterification (% DE) of pectin is defined as the number of methyl-esterified galacturonic acid units expressed as a percentage of the total galacturonic acid in the
  • pectin content is also expressed in terms of galacturonic acid content, using said galacturonic acid as standard.
  • the defatted mango peel powder (MPP*) undergoes further acid hydrolysis in process step 8 to extract pectin.
  • Two dilute acid solutions were considered in this process step, namely: sulfuric acid or hydrochloric acid, which are reported to give good pectin recovery.
  • a ratio of defatted mango peel powder (MPP*), which is the pectin- containing material, to water of 1 :10 to 1 :40 (w:v) is employed during said process, preferably at a ratio of 1 : 10— 1 :30, more preferably at a ratio of 1 :10-1 :20, and best at a ratio of 1 : 15.
  • the hydrolysis step is carried out by heating the mixture at 60-90°C, preferably 70-90°C, more preferably at 80-90°C and best at 80°C to facilitate faster and more efficient pectin extraction from the defatted mango peel powder for about 30 to 120 minutes.
  • Acid hydrolysis was preferably done at an incubation time of 60- 120 minutes, more preferably at 90-120 minutes, and best at 120 minutes.
  • the resulting mixture is then filtered in process step 9 to separate the filtrate and the spent defatted mango peel powder (spent MPP*).
  • simple decantation of the filtrate after a few minutes of settling of the spent MPP* works very well, especially that the filtrate has an increased viscosity with increasing amount of pectin extracted; however, the use of a simple filter cloth is also efficient and quick as the spent MPP* is easily removed by then.
  • a combination of a simple settling-decantation-filtration process step to separate the filtrate (liquid extract) from the spent solids is the most preferable step as this allows the full recovery of the said spent solid (mango peel powder) for recycling or further use.
  • the filtrate undergoes alcoholic precipitation, mixing and settling in process step 10; after which the obtained wet pectin precipitate is further dried and milled in process step 11, to further obtain an important composition herein which is the mango pectin powder.
  • alcoholic precipitation ethanol or methanol can be used. In this invention, ethanol is preferred as it is acceptably food-grade.
  • the mixture is then stirred thoroughly for a few minutes, during which time the pectin gel is visibly formed in the mixture. After which, the resulting pectin precipitate (which is semi-solid, having a gel-like form) is allowed to settle for a few minutes. This pectin gel-like material is then withdrawn as wet pectin precipitate. This is further dried and milled to the desired particle size in process step 11 to obtain the dry mango pectin powder.
  • the alcoholic solution obtained in process step 10 is another important composition, which is an extract with high polyphenol concentrations. This solution may be subjected to a further purification step in process step 12, which may
  • 395 include alcohol recovery, to obtain a more concentrated composition of polyphenolics.
  • the purification step may involve ion-exchange, adsorption or simple evaporation of the alcohol at reduced pressure.
  • the alcohol recovered in this process step is collected and recycled back to process step 10 where it is used again for the alcoholic precipitation-mixing-settling process.
  • An appropriate alcohol such as
  • the concentrate obtained after process step 12 is another important composition, referred to herein as polyphenolic concentrate, derived after the purification of the alcoholic solution and this said composition is characterized by its relatively very high concentration of
  • Pectin was extracted from the defatted mango peel powder (MPP) obtained by the integrated process described in a related invention.
  • the extraction process employs the acid hydrolysis and alcoholic precipitation methods.
  • a known amount of defatted MPP is mixed with water at different weight ratios (1 :10-1 :40) and the pH of the
  • 415 mixture was adjusted to a certain pH point (1.5-3.5) by adding a dilute solution of acid (using 0.1N sulfuric acid or 0. IN hydrochloric acid). The resulting mixture was stirred and heated at a certain temperature (60-90°C) for different time periods (30- 120 minutes). After which, the mixture was allowed to cool down, during which time, the spent solids were also settled down. When the mixture has cooled down to
  • the filtrate is decanted to another vessel. Then, the spent solids together with the remaining adhering filtrate is further filtered using an ordinary filter or alternatively using cheesecloth, to fully separate the filtrate from the spent solids (mango peel powder).
  • the filtrate collected in another vessel was further mixed with ethanol (95% pure) at a certain volumetric ratio of 1 :5 (ethanokfiltrate),
  • Table 3 shows some selected results at different operating conditions during acid hydrolysis and alcoholic precipitation of pectin from the defatted mango peel powder. Experimental trials and analysis were done in triplicates.
  • results showed that a notably high yield of 36.36% pectin was obtained when an MPP:water volumetric ratio of 1 : 15 and hydrochloric acid at pH 1.5 were employed during acid hydrolysis at 80°C for 120 minutes. Good yields of pectin were also obtained when an MPP:water volumetric ratio of 1 :20 was employed at the same conditions of pH, temperature, and incubation period.
  • the alcoholic filtrate obtained after filtration of pectin was analyzed for its total polyphenol (TP) and total monomelic anthocyanin (TMA) contents according to the procedures described earlier.
  • Results in Table 4 showed that the filtrate contains notably high contents of total polyphenols (TP) ranging from 850-1,350 mg per liter of alcoholic filtrate, but has negligible amounts of total monomeric anthocyanins (TMA).
  • TP total polyphenols
  • TMA total monomeric anthocyanins
  • Results indicate that the alcoholic filtrate obtained after pectin extraction and precipitation is a good source of polyphenolic substances, rendering it a good ingredient in nutraceuticals, functional foods, pharmaceuticals, and cosmetic applications, and therefore, is a valuable composition resulting from this invention.
  • Example 3 Analysis of the Spen Mango Peel Powder after Pectin Extraction
  • the spent mango peel powder collected after pectin extraction was collected and further analyzed for its proximate analysis by standard methods [AO AC, 2000] and its remaining total polyphenol contents by the methods described earlier. Results in Table 5 shows that (further explanations) ....
  • the spent mango peel powder still contains a considerable amount of polyphenolics, about 45-60 mg per gram of spent material, such that said composition could still be a good source of such bioactive compounds.

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Abstract

La présente invention concerne un procédé intégré amélioré de récupération de la pectine et de compositions polyphénoliques dans les pelures de mangue. Dans ce procédé amélioré, la substance contenant la pectine est soumise à hydrolyse acide pour extraire la pectine, le filtrat contenant la substance à pectine est séparé par une simple étape de décantation et/ou filtrage, et la substance à pectine est récupérée par précipitation alcoolique. Le précipité de pectine peut en outre être séché et broyé pour obtenir la poudre de la pectine. En outre, le procédé de l'invention amélioré se caractérise par son rendement en pectine de 30% ou plus. La pectine obtenue ici se caractérise également par sa teneur en acide galacturonique de 70% ou plus et par sa haute teneur en méthoxyle avec un degré d'estérification de 65% ou plus, car elle utilise la poudre de peau de mangue dégraissée obtenue dans le procédé intégré d'une invention connexe. De plus, le procédé amélioré permet d'obtenir une utilisation efficace de l'alcool en tant qu'agent de précipitation pour la pectine car il utilise des procédés de purification et de récupération de l'alcool combinés dans la préparation subséquente de la composition polyphénolique.
PCT/PH2013/000009 2012-03-22 2013-03-15 Préparation de pectine et de compositions polyphénoliques à partir de pelures de mangue WO2013141723A1 (fr)

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PT107607A (pt) * 2013-04-29 2014-10-29 Galina Ignatyeva Método de fabrico de pectina acromática, pectina e fibra modificada e pectina padronizada.
CN105998109A (zh) * 2016-06-24 2016-10-12 贺州学院 一种芒果核多酚提取物及其制备方法
CN106138130A (zh) * 2016-07-26 2016-11-23 贺州学院 一种芒果核黄酮提取物及其制备方法
CN112914012A (zh) * 2021-01-29 2021-06-08 广西壮族自治区农业科学院 一种芒果皮中键合态香气物质的提取方法及其应用
CN113024616A (zh) * 2021-03-22 2021-06-25 贺州学院 一种芒果核单宁酸的制备方法

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CN109874963A (zh) * 2019-04-12 2019-06-14 倪震丹 一种苹果果纸及其制备方法

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PT107607A (pt) * 2013-04-29 2014-10-29 Galina Ignatyeva Método de fabrico de pectina acromática, pectina e fibra modificada e pectina padronizada.
PT107607B (pt) * 2013-04-29 2015-06-03 Galina Ignatyeva Método de fabrico de pectina acromática de elevada e baixa esterificação, pectina acromática modificada, pectina acromática padronizada e fibra dietética acromática modificada
CN105998109A (zh) * 2016-06-24 2016-10-12 贺州学院 一种芒果核多酚提取物及其制备方法
CN106138130A (zh) * 2016-07-26 2016-11-23 贺州学院 一种芒果核黄酮提取物及其制备方法
CN112914012A (zh) * 2021-01-29 2021-06-08 广西壮族自治区农业科学院 一种芒果皮中键合态香气物质的提取方法及其应用
CN112914012B (zh) * 2021-01-29 2023-09-15 广西壮族自治区农业科学院 一种芒果皮中键合态香气物质的提取方法及其应用
CN113024616A (zh) * 2021-03-22 2021-06-25 贺州学院 一种芒果核单宁酸的制备方法

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