WO2021025650A2 - Method of obtaining powder mono,-di glyceride coated with dried milk and whey protein from bone waste oil obtained from a rendering (animal by-products) facility - Google Patents

Method of obtaining powder mono,-di glyceride coated with dried milk and whey protein from bone waste oil obtained from a rendering (animal by-products) facility Download PDF

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Publication number
WO2021025650A2
WO2021025650A2 PCT/TR2020/050671 TR2020050671W WO2021025650A2 WO 2021025650 A2 WO2021025650 A2 WO 2021025650A2 TR 2020050671 W TR2020050671 W TR 2020050671W WO 2021025650 A2 WO2021025650 A2 WO 2021025650A2
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Prior art keywords
mono
diglyceride
whey protein
dried milk
production method
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PCT/TR2020/050671
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French (fr)
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WO2021025650A3 (en
Inventor
Mahmut DOĞAN
Meryem GÖKSEL SARAÇ
Original Assignee
T.C. Erci̇yes Üni̇versi̇tesi̇
Cumhuri̇yet Üni̇versi̇tesi̇ Rektörlüğü
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Publication of WO2021025650A2 publication Critical patent/WO2021025650A2/en
Publication of WO2021025650A3 publication Critical patent/WO2021025650A3/en

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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B13/00Recovery of fats, fatty oils or fatty acids from waste materials
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00Refining fats or fatty oils
    • C11B3/003Refining fats or fatty oils by enzymes or microorganisms, living or dead
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/74Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes

Definitions

  • the invention is related to a method for obtaining powder mono-, diglyceride coated with dried milk and whey protein from bone waste oil obtained from a rendering facility that is to be used in the food sector.
  • Emulsifiers are agents that enable foodstuff to have a fine disperse structure by reducing surface tension, and the free energy located between two phases and by providing stability by creating a film adsorbed around the droplets that form the discontinuous phase.
  • Emulsifiers that provide positive effects related to the rheological, textural and sensory attributions that prevent physical flaws that can occur depending on the extended shelf lives of foodstuff are foodstuff additive agents that are prevalently used nowadays.
  • the mono-, diglycerides of fatty acids are included in this group.
  • Mono-, diglycerides that are commonly used to provide stability for products that contain both the oil and the water phase are usually obtained from vegetable oils.
  • Mono-, diglycerides that are estimated to be used as 500 hundred tons monthly in Turkey, are used primarily in mayonnaise, margarines and for the preparation of ice-cream to provide emulsion; in meat products such as sausages and salami in order to prevent the separation of oil, in bakery products in order to increase volume and prevent starch retro gradation and in products such as spices and instant soup in order to provide solubility.
  • Mono-, diglycerides are not only used in the food sector but they are also commonly used in the cosmetic and chemical sector in order to obtain the desired form of drug formulations in the pharmaceutical field.
  • the invention subject to the patent numbered WO9931043 is related to obtaining monoglyceride as a result of glycerolysis reaction of methyl ester. It has been noted that methyl ester can be animal or plant based. Similarly in this invention the production stages are different and the coating stage is not present.
  • EP1660668 The invention subject to the patent numbered EP1660668 is related to the production emulsifiers comprising mono and diacylglycerols through enzymatic reaction. I n this invention, it was stated that the oil was obtained from vegetable sources and the liquid form was solidified by a vacuum dryer. Any kind of a coating step is not present in said invention.
  • the powder mono-, diglyceride is produced by being coated with dried milk and whey protein from bone waste oil that is obtained from a rendering facility and this step constitutes the present art of the invention.
  • shelf life or the emulsifiers within the oil structure converted into powder form by means of the encapsulation technique has been extended and usage feasibility has been provided.
  • the reason for extending shelf life is to prevent the product that has been turned into power form from the oil form from coming into direct contact with oxidation increasing factors such as light, heat and oxygen, and therefore to prevent spoiling depending on oxidation.
  • the emulsifiers that are converted into powder form following encapsulation have superior properties such that the coating materials are cheap and easily accessible, the final product is easy to use as it is in powder form and that the shelf life is extended.
  • the extension of the shelf life has enabled for the emulsifier in liquid form to be durable in terms of sensory and oxidative properties. It is known that oxidation in oil occurs with direct metal contact of oil, or as a result of being treated with oxygen and light. The direct contact of the mono-, diglyceride emulsifier is cut off in said environments as a result of being coated with dried milk and whey protein and therefore its shelf life has been extended for 12 months.
  • Figure 1 Fluorescent microscope images of emulsions (C) prepared with ready mono- , diglyceride emulsifiers that are expressed as control and mono-, diglyceride samples obtained from rendering facility waste oils that were encapsulated with dried milk (A) and whey protein (B).
  • FIG. 1 Monoglyceride, Diglyceride and Triglyceride Peaks according to HPLC Device measurement results.
  • the mono-, diglyceride emulsifier obtained from the waste oil from rendering facilities, by being coated in a spray dryer with dried milk and whey protein is converted into powder form.
  • mono-, diglyceride in liquid form is produced.
  • Lipase Novozyme 4305 has been used as an enzyme for the production of liquid mono-, diglycerides.
  • Glycerol (15% of oil amount), enzyme (10% of oil amount) and waste oil from the rendering facility has been added to the reaction medium and reaction has been carried out in an agitation water bath at 70°C for 5 hours in sealed glass flasks. The reaction can also be carried out at a temperature between 50-80 °C for 2-8 hours in an agitation water bath.
  • the remaining amount following the enzyme removal process has been defined as mono- , diglyceride following the analysis thereof (50% monoglyceride, 40% diglyceride and 10% triglyceride) ( Figure 2).
  • the liquid emulsifier obtained was coated with milk powder and whey protein by microencapsulation method and it was obtained in powder form.
  • the process of encapsulation is basically defined as the coating of an agent with another agent.
  • the sizes of the coated agents may vary and if the particle size is between 0.2- 5000 pm the capsule is defined as a microcapsule.
  • the microencapsulation process is defined as the structure that is obtained by the coating of the active agent (core, core matter) with one or more agents (membrane, shell, coating material, and wall).
  • the microencapsulation method of the invention which is the conversion of the mono- , diglyceride that is obtained in liquid form with dried milk and whey protein by being coated with a spray drier, the dried milk and/or the whey protein and the mono- , diglyceride is mixed with emulsifier and potable water for 5 minutes at a speed of 24000 rpm with ULTRA-TURRAX® .
  • the emulsion has been prepared such that it contains 10 and 20 % dry matter (dried milk or whey protein that is the coating material and mono-, diglyceride) and water as the remaining part.
  • the dry matter section has been prepared to have a ratio of 1 :2 and 1 :3 mono-, diglyceride/ coating agent (dried milk or whey protein).
  • a spray dryer feeding is carried out with a spray dryer.
  • the spray drier that is used is a laboratory type dryer that has a nozzle diameter of 2.8 mm.
  • the operation conditions have been adjusted as, speed rate 8 mL/minute, dry air flow 600 Uhour, aspirator rate 100% , exit temperature 110-115 °C, input rate 180 °C and pump speed 30% .
  • a heated magnetic mixer is used during feeding in order to enable homogenous feeding and to ensure that the temperature is fixed to 35 °C.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Microbiology (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Biochemistry (AREA)
  • General Preparation And Processing Of Foods (AREA)
  • Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
  • Fodder In General (AREA)
  • Dairy Products (AREA)

Abstract

The invention is related to producing powder form of mono-, diglyceride emulsifiers, obtained from the waste oil from rendering facilities, by being coated in a spray dryer with dried milk and whey protein.

Description

METHOD OF OBTAI Nl NG POWDER MONO,-DI GLYCERI DE COATED Wl TH DRI ED Ml LK AND WHEY PROTEI N FROM BONE WASTE Ol L OBTAI NED FROM A RENDERI NG (ANI MAL BY-PRODUCTS) FACI LI TY
TECH N I CAL FI ELD
The invention is related to a method for obtaining powder mono-, diglyceride coated with dried milk and whey protein from bone waste oil obtained from a rendering facility that is to be used in the food sector.
PRI OR ART
Emulsifiers are agents that enable foodstuff to have a fine disperse structure by reducing surface tension, and the free energy located between two phases and by providing stability by creating a film adsorbed around the droplets that form the discontinuous phase. Emulsifiers that provide positive effects related to the rheological, textural and sensory attributions that prevent physical flaws that can occur depending on the extended shelf lives of foodstuff are foodstuff additive agents that are prevalently used nowadays. The mono-, diglycerides of fatty acids are included in this group. Mono-, diglycerides that are commonly used to provide stability for products that contain both the oil and the water phase are usually obtained from vegetable oils.
Mono-, diglycerides that are estimated to be used as 500 hundred tons monthly in Turkey, are used primarily in mayonnaise, margarines and for the preparation of ice-cream to provide emulsion; in meat products such as sausages and salami in order to prevent the separation of oil, in bakery products in order to increase volume and prevent starch retro gradation and in products such as spices and instant soup in order to provide solubility. Mono-, diglycerides are not only used in the food sector but they are also commonly used in the cosmetic and chemical sector in order to obtain the desired form of drug formulations in the pharmaceutical field.
These emulsifiers that are being used are imported from abroad and they are not produced in our country. Manufacturing companies produce mono-, diglycerides from vegetable and animal oils. Mono-, diglyceride production has been carried out globally by the application of enzymatic and chemical techniques for many years. However a powder form of mono-, diglycerides obtained from the waste oil from rendering facilities, by being coated in a spray dryer with dried milk and whey protein is not available.
When the prior art was searched the invention with the patent numbered WO2013122599 has been encountered which is related to the production of high purity monoglycerides through enzymatic reaction. A lipase enzyme has been used as an enzyme Vegetable oil, fish oil, animal oils such as rendering oils can be used as the oil source. When compared with the invention, the prior art has differences in terms of production stages and especially the coating stage of the liquid emulsifier that enables to obtain the technical effect is not available.
The invention subject to the patent numbered WO9931043 is related to obtaining monoglyceride as a result of glycerolysis reaction of methyl ester. It has been noted that methyl ester can be animal or plant based. Similarly in this invention the production stages are different and the coating stage is not present.
The invention subject to the patent numbered EP1660668 is related to the production emulsifiers comprising mono and diacylglycerols through enzymatic reaction. I n this invention, it was stated that the oil was obtained from vegetable sources and the liquid form was solidified by a vacuum dryer. Any kind of a coating step is not present in said invention.
I n the present invention the powder mono-, diglyceride is produced by being coated with dried milk and whey protein from bone waste oil that is obtained from a rendering facility and this step constitutes the present art of the invention.
BRI EF DESCRI PTI ON OF THE I NVENTI ON
The production of mono-, diglyceride emulsifiers from vegetable and animal sources are known in the prior art. The difference between the prior art and the subject matter of the present invention is that the mono-, diglycerides that have been obtained from rendering facility bone waste oils are coated with dried milk and whey protein. By means of this technical difference, unexpected effects have been obtained in the properties of food emulsifiers. It has been found that the emulsifiers that are coated have superior properties, primarily in terms of emulsion forming and rheological properties, when compared with the mono-, diglycerides that are being commercially sold in the market.
Especially when the fluorescent microscope images are examined, it has been observed that the powder samples coated in emulsion medium had more homogenous and stably distributed oil particles. It has been noted that in the emulsions prepared as such, the emulsion stabilities of the powder emulsifiers had better properties in comparison to the examples in the market and that a phase separation in emulsions was not determined (Figure 1 ).
Similarly, during the comparison of the emulsion examples that that were prepared as a result of rheological analyses that were carried out, it was noted that the viscosity values of the samples that were prepared with emulsifiers that are already being sold in the market, was approximately 10-15 m.Pa.s, whereas the value in emulsions prepared with emulsifiers coated with dried milk has been determined as 43-45 m.Pas and the value in emulsions prepared with emulsifiers coated with whey protein has been determined as 35-37 m.Pas. This situation shows that the coated emulsifier samples exhibit more viscous structures and the desired viscosity of the product can be achieved by using lower amounts of additives.
Moreover the shelf life or the emulsifiers within the oil structure converted into powder form by means of the encapsulation technique has been extended and usage feasibility has been provided. The reason for extending shelf life is to prevent the product that has been turned into power form from the oil form from coming into direct contact with oxidation increasing factors such as light, heat and oxygen, and therefore to prevent spoiling depending on oxidation.
The emulsifiers that are converted into powder form following encapsulation have superior properties such that the coating materials are cheap and easily accessible, the final product is easy to use as it is in powder form and that the shelf life is extended. The extension of the shelf life has enabled for the emulsifier in liquid form to be durable in terms of sensory and oxidative properties. It is known that oxidation in oil occurs with direct metal contact of oil, or as a result of being treated with oxygen and light. The direct contact of the mono-, diglyceride emulsifier is cut off in said environments as a result of being coated with dried milk and whey protein and therefore its shelf life has been extended for 12 months.
The emulsifier samples that have been obtained have been tried on model products that have commercial value and it has been determined following comparison with equivalent products that these new emulsifier samples were superior in terms of product structure as well. Studies were conducted on edible ice-cream as the model product. The most preferred products of consumers following sensory analysis were emulsifiers that were produced from powder coated waste oil obtained from rendering facilities. Definition of the Figures of the I nvention
Figure 1 : Fluorescent microscope images of emulsions (C) prepared with ready mono- , diglyceride emulsifiers that are expressed as control and mono-, diglyceride samples obtained from rendering facility waste oils that were encapsulated with dried milk (A) and whey protein (B).
Figure 2: Monoglyceride, Diglyceride and Triglyceride Peaks according to HPLC Device measurement results.
DETAI LED DESCRI PTI ON OF THE I NVENTI ON
The mono-, diglyceride emulsifier obtained from the waste oil from rendering facilities, by being coated in a spray dryer with dried milk and whey protein is converted into powder form. Before this process mono-, diglyceride in liquid form is produced. Lipase (Novozyme 435) has been used as an enzyme for the production of liquid mono-, diglycerides. Glycerol (15% of oil amount), enzyme (10% of oil amount) and waste oil from the rendering facility has been added to the reaction medium and reaction has been carried out in an agitation water bath at 70°C for 5 hours in sealed glass flasks. The reaction can also be carried out at a temperature between 50-80 °C for 2-8 hours in an agitation water bath. An ultrasound application (for 60 minutes with 40 kHz frequency) in the ultrasonic water bath was carried out on the medium during reaction and acetone (at a ratio of 1/1 oil/solvent) has been added as a solvent. The ultrasonic bath application provides support to increase enzyme efficiency under enzymatic glycerolysis reaction and therefore interaction of the enzyme and oil which is its substrate is increased and a more productive conversion is provided. Said conversion is the conversion of the rendering waste oil present in the triglyceride structure into mono-, diglyceride form.
By this means, 90% conversion has been provided in product yield by reaction.
The remaining amount following the enzyme removal process has been defined as mono- , diglyceride following the analysis thereof (50% monoglyceride, 40% diglyceride and 10% triglyceride) (Figure 2). The liquid emulsifier obtained was coated with milk powder and whey protein by microencapsulation method and it was obtained in powder form.
The process of encapsulation is basically defined as the coating of an agent with another agent. The sizes of the coated agents may vary and if the particle size is between 0.2- 5000 pm the capsule is defined as a microcapsule. The microencapsulation process is defined as the structure that is obtained by the coating of the active agent (core, core matter) with one or more agents (membrane, shell, coating material, and wall).
I n the microencapsulation method of the invention, which is the conversion of the mono- , diglyceride that is obtained in liquid form with dried milk and whey protein by being coated with a spray drier, the dried milk and/or the whey protein and the mono- , diglyceride is mixed with emulsifier and potable water for 5 minutes at a speed of 24000 rpm with ULTRA-TURRAX® . The emulsion has been prepared such that it contains 10 and 20 % dry matter (dried milk or whey protein that is the coating material and mono-, diglyceride) and water as the remaining part. The dry matter section has been prepared to have a ratio of 1 :2 and 1 :3 mono-, diglyceride/ coating agent (dried milk or whey protein).
Following this, a spray dryer feeding is carried out with a spray dryer. The spray drier that is used is a laboratory type dryer that has a nozzle diameter of 2.8 mm. I n order for the emulsifiers to be converted into powder form via the spray drying process, the operation conditions have been adjusted as, speed rate 8 mL/minute, dry air flow 600 Uhour, aspirator rate 100% , exit temperature 110-115 °C, input rate 180 °C and pump speed 30% .
When a drying process is carried out on the emulsion form, a heated magnetic mixer is used during feeding in order to enable homogenous feeding and to ensure that the temperature is fixed to 35 °C.
The following product properties of powder mono-, diglyceride emulsifiers were enabled as a result of production under these conditions;
Microencapsulation efficiency: 50-85%
Microencapsulation yield: 40-60%
Water activity: 0.1 -0.2 pH: 6-7

Claims

CLAI MS
1. A production method of mono-, diglycerides from bone waste oil obtained from rendering facilities, characterized in that it comprises the process step of coating the mono-, diglyceride obtained in liquid form in a spray drier with dried milk and whey protein and thereby converting it to powder form.
2. A production method of mono-, diglycerides according to claim 1 , characterized in that it comprises the process step of coating the mono-, diglyceride obtained in liquid form in a spray drier with dried milk and whey protein and thereby converting it to powder form by means of this microencapsulation method.
3. A production method of mono-, diglycerides according to claim 1 , characterized in that the conversion of the mono-, diglyceride obtained in liquid form into powder form by coating it in a spray dryer with dried milk and whey protein comprises the process steps of,
• mixing the mono-, diglyceride: with dried milk or whey protein and potable water to have a ratio of 1 : 2 or 1 :3,
• Carrying out spray dryer feeding with a spray dryer.
4. A mono-, diglyceride production method according to claim 3, characterized in that the mono-, diglyceride, dried milk or whey protein and potable water are mixed for 5 minutes at 24000 rpm speed.
5. A mono-, diglyceride production method according to claim 1 , characterized in that the atomizer nozzle diameter of the spray dryer used during the microencapsulation process is 2.8mm, the feed speed is 8 mL/minute, the dry air flow rate is 600 L/hour, the aspirator speed is 100% , the exit temperature is 110- 115°C, the input temperature is 180 °C and the pump speed is 30% .
6. A mono-, diglyceride production method according to claim 1 , characterized in that when the drying process is carried out on the emulsion form, a heated magnetic mixer is used during feeding in order to enable homogenous feeding.
PCT/TR2020/050671 2019-08-06 2020-07-29 Method of obtaining powder mono,-di glyceride coated with dried milk and whey protein from bone waste oil obtained from a rendering (animal by-products) facility WO2021025650A2 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
TR2019/11951A TR201911951A2 (en) 2019-08-06 2019-08-06 RENDERING (ANIMAL BY PRODUCT FACILITY) FACILITY POWDER MONO COATED WITH MILK POWDER AND CHEESE WATER PROTEIN FROM BONE WASTE OIL, -DIGLYCERIDE OBTAINING METHOD
TR2019/11951 2019-08-06

Publications (2)

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WO2021025650A2 true WO2021025650A2 (en) 2021-02-11
WO2021025650A3 WO2021025650A3 (en) 2021-09-23

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Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5601760A (en) * 1994-09-01 1997-02-11 The Regents Of The University Of California, A California Corporation Milk derived whey protein-based microencapsulating agents and a method of use
RU2305473C1 (en) * 2006-03-07 2007-09-10 Общество с ограниченной ответственностью "Артлайф" Method for microincapsulation of flavoring substances and flavoring product obtained by using the same
US9332774B2 (en) * 2007-06-27 2016-05-10 Bunge Oils, Inc. Microencapsulated oil product and method of making same

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WO2021025650A3 (en) 2021-09-23

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