DK179243B1 - Fremgangsmåde til fremstilling af syrlig 50 % koncentreret opløsning og tørpulver af peptider fra proteinprodukter og animalsk affald, fisk og akvakulturoprindelse - Google Patents

Description

PROCESS FOR PRODUCING ACIDULATED 50% CONCENTRATED SOLUTION AND DRY POWDER OF PEPTIDES FROM PROTEIN PRODUCTS AND WASTE OF ANIMAL, FISH AND AQUACULTURE ORIGIN

FIELD OF THE INVENTION

The present invention is directed to a process for producing an acidulated 50% concentrated solution and dry powder of peptides, from protein products and waste of animal, fish, and aquaculture origin.

It is based primarily in the process of enzymatic and chemical hydrolysis of protein products, generated in the processes of food production for human consumption.

BACKGROUND OF THE INVENTION

The procedures used up to date, for example, in the industry for fish flour or other types of flour fabrication, for example Chilean Patent N° 30380 (Comittee of Technological Research from the Corporation for the promotion of production,) considers the manipulation of solid and semi-solid matter in part of its process and oils. Said process allows obtaining from 10 to 14% of fat with a significant loss in the texture of the final product, due to the limited control on the parameters of the process. Said process, as well as the state of the art, consists basically in shredding the fish waste to the size of particles, partial homogenization of the shredded matter and being subjected to cooking, centrifugation and decantation, obtaining water, wet solids and oil, for animal consumption.

In one hand, it is known the procedure of acid-basic hydrolysis contemplating subjecting the raw material to an acid-basic hydrolysis producing the separation of lipids, obtaining a concentration subjected to drying and afterwards, to milling and packing.

On the other hand, the enzymatic hydrolysis process subjects the raw material to an enzymatic hydrolysis, where lipids are separated, obtaining a concentration of the product which is subjected to drying for further milling and packing.

Document WO 2006/096067 (Wahl) of 14 September 2006 discloses a method for the process of enzymatic hydrolysis of collagen and raw material containing proteins. The raw material suffers an enzymatic hydrolysis to produce three layers: a top layer containing fat, an intermediate layer comprising water-soluble components, and a bottom layer with non-soluble material, such as bones and non-soluble proteins. These layers are separated and the second layer is further processed for separation, by cooling during an appropriate time producing two layers: a bottom layer containing totally or partially the collagen, and a top layer of liquid containing the remaining water-soluble proteins. The last layer is withdrawn, and the other is heated until transformed in liquid. The facilities where this process is performed comprises an hydrolysis tank with a revolving agitation mechanism, and a heat exchange device; a reversible screw located at the bottom of the tank; a compensation collector for separation of collagen, including an inlet for the hydrolyzed supply; a heat exchange system comprising a heating jacket sourrounding the drain.

Document US 2004/038391 (Pyntikov) dated 26 february 2004, discloses a method of enzymatic hydrolysates of proteins of cold water animals, which is performed in a continuous mix and in very preciselly controlled conditions until very short aminoacids and proteins are produced. The enzimatic protein hydrolysate disclosed in this document is sterilized. The fish oil and solid particles are eliminated by centrifugation. The enzimatic protein hydrolysate contains up to 90% of free aminoacids, the oil of cold fish, hydroxylapathite (calcium ortophosphate,) proteins, high molecular concentration of aminoacids, vitamins, minerals, and calcium and phosphorous salts. The fabrication process comprises the mixing of waste products offish with a source of enzymes, comprising innards and entrails of cold-water fish, with a relatively aggressive content of enzymes, effective, even in a lightly alkaline medium. The industrial method provides a higher grade of refinement than existing technologies by using acid and steps of alkaline denaturalization, in combination with separation and advanced drying technologies.

Document FR 2835703 (Linder et al.) dated 15 August 2003, discloses a method for obtaining an oil and a protein hydrolysate from a protein-rich source from marine tissue of discarded filets, fish heads and tails, shellfish or whole fish of low commercial value, comprising enzymatic hydrolysis in no more than 60 °C providing an aqueous mixture comprising hydrolysates and a fat phase including oil, separation of phases, and stopping the hydrolysis in the aqueous phase.

Document US 5,053,234 (Anderson et al.) dated 1 October 1991, discloses a method for the preparation of a protein product from a raw protein source comprising animal parts. The method comprising the following steps: a) reducing the raw material of animal origin in parts in a confined condition; b) hydrolyze the proteins of the confined parts of the raw material of animals using proteolytic enzymes, wherein the hydrolysis is performed at a temperature in a range favorable for enzyme activity without denaturing the protein and for a period of time enough to achieve a predetermined grade of partial hydrolysis of the protein, to form an aqueous solution of parts of animals partially hydrolyzed; c) heat the aqueous suspension, enough to deactivate the proteolytic enzymes and converting fat into oils; d) separation and elimination of non-digestible soluds from the heated aqueous suspension; e) adding oil to the aqueous suspension heating until forming an oily protein suspension; f) pasteurization of the oily protein suspension; g) reduction of the concentration of water in the oily protein suspension to form a oleaginous suspension of partially hydrolyzed protein, and h) elimination of a part of the oil from the oleaginous suspension to form a partially hydrolyzed particulate, of a non-denatured protein product.

Document WO 2004/021797 discloses a method for recovering peptides/amino acids and oil/fat from one or more protein- containing raw materials characterized in that it comprises the following steps: a. grinding the raw materials; b. heating the ground raw materials to a temperature in the range of 40-62 °C, preferably 45-58°C; c. optionally before and /or after the heating step, separating oil/fat from the raw materials in order to obtain a first oil product; d. adding water, the water having approximately the same temperature as the raw materials, and wherein the pH of the water is adjusted by adding calcium; e. hydrolyzing the raw materials with endogenous enzymes in order to prepare a hydrolysate; f. optionally during the hydrolysation step, adding a pH adjuster in order to maintain the desired pH value of the hydrolysate; g. heating the hydrolysate to 75-IOO°C, preferably 85-95°C; h. removing large particles from the hydrolysate, including non-hydrolysed proteins, which can be returned to the hydrolysis; i. optionally separating off fat/oil in order to obtain a second oil product; j. coagulating the proteins; k. removing the coagulated proteins; l. optionally separating off fat/oil in order to obtain a third oil product; m. optionally concentrating the remaining amino acids and short peptides; and n. optionally drying the concentrate in order to obtain dry short peptides and amino acids (claim 1).

The materials can be pumped via either an "in-line" continuous heat exchanger, or a batch working heat exchanger to the fermentation tank (page 18, lines 19-25; fig. 1). The separation steps may be performed with a centrifuge (fig. 1, "103"), and the hydrolysis by enzymes is performed in a fermentation tank (fig. 1 "106"). The method may be used for producing a food product (claim 8) or a feed product (claim 9).

The method according to WO 2004/021797 is very similar to the method according to the present invention, however the technical difference between the invention and WO 2004/021797 is mainly the introduction of an acid or base hydrolysis step of nonhydrolyzed solids (step, i)) in claim 1 of the present invention. The technical effect of this difference is a more complete hydrolysis of the raw material and thereby also redundancy of the removal steps of larger particles/coagulated proteins. Hence, the present invention provides a more effective hydrolysis method, which avoid two steps of removing large particles, step h. of D1 and step k. of WO 2004/021797.

Document DE 2705671 A1 discloses breaking down machine leather scrap hydrolytically in a first step using alkaline proteinases in presence of urea and then in a second step, hydrolysis using weakly alkaline, neutral or acidic proteinases in pH range optimum for the enzyme or enzyme mixture used. Fat and protein hydrolysates are then separated by demixing at a temperature in the range of 80 to 100 degrees C. In other words; DE 2705671 A1 discloses two enzymatic hydrolysis steps, followed by a defatting step.

In contrast, the method according to the present invention recites first heating to 50 °C and defatting by centrifugation, then enzymatic hydrolysis, separation of solids, chemical hydrolysis of the separated non-hydrolyzable solids and neutralizing the chemical hydrolysis at low temperature in a descending film evaporator and/or in a spray dryer or air band dryer. The method according to the present invention defats the raw materials first, and then treats with an enzymatic hydrolysis; separates solids and chemically hydrolyzes solids, followed by neutralization.

According to the previously described, one of the objects of the present invention is to produce wet solutions of peptides (parts of proteins) at a 50% concentration or dry peptides, for human and animal consumption, using as source material secondary products generated in the production of protein food for direct human consumption.

Although the invention is directed to obtaining powder of meat products in general, the invention will be descried based on a simplyfied example, in which a protein food is obtained, wherein the basic steps differentiating the present invention from the state of the art are described.

The procedure is started by a licquefaction of raw material by milling, fat extraction at low temperature previous to the enzymatic action, which at present is distorted by the presence of fat and the enzymatic hydrolysis is combined with the acid hydrolysis, increasing the protein yield to nearly 100%, eliminating organic liquid industrial waste from industrialization.

It is of great importance that the raw material is received in good conservation conditions, in plastic bags and/or in bins isolated with polyurethane and ice cooled. The bins must be stored in an isotermic refrigerated facility.

The industry or plant for development of the process must be installed in a sanitary storehouse, hermetically sealed, with pressure control to maintain a constant small vacuum; the air needed for petroleum combustion in the vapor generating boiler will be obtained from the interior of the storehouse in processes and air evacuating ducts from air drying equipment at low temperature.

The bins and plastic bags are unloaded in a stainless steel hopper, the plastic bags are sent to authorized dumps and the bins are washed with high pressure pumps for re-utilization.

The raw material is milled and pumped to heat exchangers.

The raw material is heated to 50°C and subjected to centrifugation to decrease efficiently the percentage of fat, which is detrimental to the control of enzymatic hydrolysis.

The produce with lower fat percentage is pumped to digestion tanks of 8 m3, the pH is modified thorugh addition of acid and/or bases, the digestion tanks are heated and with continuous mixing systems, a mixture of proteolytic enzymes is added, the temperature is maintained at 50°C (+/- 3°C) throughout the process, controlling the pH for higher efficienct of hydrolysis for the mixture of enzymes selected.

Once the enzymatic process is completed, the material is pumped to a heat exchanger to increase the temperature to 96°C and processed in an horizontal centrifuge, tricanter (approximatelly 3,000 revolutions per minute) to extract the remaining oil, separating non-hydrolyzed solids and the liquid with soluble solids and peptides.

The remaining solids of the raw material are chemically hydrolyzed with acid and/or bases, then the process of hydrolysis is neutralized to subsequently concentrate to 50% in a descending film evaporator, producing the acidulated solution at 50%, and/or drying the solution in a spray dryer or an air band dryer at low temperature, milled and stored in impermeable bags of polypropylene ready for sale.

The remaining liquid with soluble solids and peptides is pumped to a heat exchanger to return to 96°C for the process of fine separation of remaining oil in a vertical separator (approximatelly at 6,000 revolutions per minute.)

The separator discharges fine solids to the screw of solids in the tricanters, continuing the same process of acid hydrolysis described before for solids.

The separator discharges raw oil in a common tank with the oil separated through previous centrifugations, from where is pumped to the storage tank and loaded in trucks for its delivery and/or final processing.

The liquid with solubles is concentrated to a 50% of solids in a vacuum descending film evaporator of various effects made of stainless steel, the acidulated product is stored in tanks for commercialization or further drying.

The 50% concentrate is pumped alternatively to a drum dryier of indirect heating by vapor or hot air spray, or to a heat exchanger, cooling the product to 2°C, to feed an extrusor which will allow the feeding of a band dryer, of 3 effects, with air recycling, where the dry solids to a 6% humidity are milled and stored, in polypropylene bags with an impervious film, with 50 kg each, for local sale and or export.

The following products are alternatively produced:

Peptides from enzymatic hydrolysis concentrated to 50%, acidulated.

Peptides from enzymatic hydrolysis, dry to 6% humidity.

Chemical hydrolysate concentrated to 50%, acidulated.

Chemical hydrolysate, dry to 6% humidity.

Peptides from enzymatic hydrolysis, with its fraction of chemical hydrolysate concentrated to 50% acidulated.

Peptides from enzymatic hydrolysis with its fraction of chemical hydrolysate, dry to 6% humidity.

The bags are stored in pallets with 3 height levels.

The air used for drying in a spray dryer and/or band dryer at low temperature with 12 effects, with a recycling system through an automatic sleeve filter, self-cleaning and a condenser to eliminate humidity generated in the dryer, decreasing a 25% the use of exterior air required; the fake air entering the circuit and a fraction of drying air recycled, after the condenser, will pass through a drop collector and a heater, which will re-heat the air to overcome the saturation point, to subsequently being burned in the burner of the vapor generating boiler for the heaters of the production process.

The equipments of the process tricanter, separator and evaporator are subjected to chemical cleaning daily, the products used are neutralized before sending them to the homogenizing tanks of the liquid industrial waste (LIW) from the factory.

The water used in condensers, from both dryers and evaporator, with 5°C more than the temperature at which they were supplied from the spring and/or deep well, are used for irrigation and/or are infiltrated back to earth.

The water used in the plant cleaning and distillates from the boiler and evaporator, are homogenized in the LIW tank and are subjected to a physical separation and filtration process before they are destined to irrigation water and/or infiltration together with the water from condensers.

Claims (14)

1. Patentkrav

   1. Fremgangsmåde til fremstilling af vådopløsninger af peptider, som er koncentreret til 50 %, eller tørre peptider, der skal indtages af mennesker eller dyr, ved at der som råmateriale anvendes sekundære produkter, som fremstilles inden for produktionen af proteinfødevarer til menneskelig indtagelse, hvor fremgangsmåden omfatter de følgende trin:

   a) at formale råmaterialet og pumpe det ind i varmevekslere;

   b) at opvarme råmaterialet til 50 °C;

   c) at centrifugere råmaterialet for at danne et produkt med en lavere fedtprocent end råmaterialet;

   d) at pumpe produktet med en lavere fedtprocent end råmaterialet ind i digestionstanke;

   e) at modificere produktets pH ved tilsætning af syre og/eller baser;

   f) at opvarme digestionstankene og fastholde temperaturen inden for et område fra 47 °C til 53 °C, at tilsætte en blanding af proteolytiske enzymer, som kontrollerer pH'en, for at øge hydrolysens virkningsgrad i blandingen af udvalgte enzymer;

   g) at pumpe produktet, så snart den enzymatiske proces er tilendebragt, ind i en varmeveksler for at øge dets temperatur til 96 °C;

   h) at centrifugere produktet for at ekstrahere den resterende olie og separere de ikke-hydrolyserede faststoffer og væsken med opløselige faststoffer og peptider;

   i) at kemisk hydrolysere de separerede ikke-hydrolyserede faststoffer ved tilsætning af en syre og/eller base,

   j) at neutralisere kemisk hydrolyse af separerede ikkehydrolyserede faststoffer ved en lav temperatur og koncentrere den hydrolyserede væske i en fordamper med descenderende film, en spraytørrer eller en båndtørrer ved lav temperatur.
2. 2. Fremgangsmåde til fremstilling af vådopløsninger af peptider ifølge krav 1, hvor blandingen er kontinuerlig i trin (f).
3. 3. Fremgangsmåde til fremstilling af vådopløsninger af peptider ifølge krav 2, hvor fremgangsmåden endvidere omfatter fremstilling af en syrlig opløsning ved 50 % i en fordamper og/eller tørring af opløsningen i en spraytørrer eller en luftbåndtørrer ved lav temperatur, der formales og opbevares.
4. 4. Fremgangsmåde til fremstilling af vådopløsninger af peptider ifølge et af kravene 1 til 3, hvor den resterende væske med opløselige faststoffer og peptider pumpes ind i en varmeveksler for at genindvinde temperaturen på 96 °C med henblik på et sidste separationstrin med den resterende olie i en vertikal separator.
5. 5. Fremgangsmåde til fremstilling af vådopløsninger ifølge krav 4, hvor væsken med opløselige stoffer koncentreres til 50 % af faststoffer i en fordamper.
6. 6. Fremgangsmåde til fremstilling af vådopløsninger af peptider ifølge krav 5, hvor 50 % koncentratet pumpes alternativt ind i en tromletørrer med indirekte opvarmning ved anvendelse af damp eller varmluftspray eller en varmeveksler.
7. 7. Fremgangsmåde til fremstilling af vådopløsninger af peptider ifølge krav 6, hvor fremgangsmåden omfatter køling af koncentratet til 2 °C for at føde en ekstruder, som muliggør fødningen af en båndtørrer, med luftrecirkulation, hvor de tørre faststoffer formales ved en 6 % fugtighed.
8. 8. Peptid fremstillet ved enzymatisk hydrolyse koncentreret til 50 % syrlig, hvor peptidet tilvejebringes ved fremgangsmåden ifølge et af kravene 1 til 7.
9. 9. Peptid fremstillet ved enzymatisk hydrolyse tørret til 6 % fugtighed, hvor peptidet tilvejebringes ved fremgangsmåden ifølge et af kravene 1 til 7.
10. 10. Kemisk hydrolysat koncentreret til 50 % syrligt, hvor hydrolysatet tilveje5 bringes ved fremgangsmåden ifølge et af kravene 1 til 7.
11. 11. Kemisk hydrolysat, som er tørret til 6 % fugtighed, hvor hydrolysatet tilvejebringes ved fremgangsmåden ifølge et af kravene 1 til 7.

    10
12. 12. Peptid, som er fremstillet ved enzymatisk hydrolyse med en fraktion af kemisk hydrolysat koncentreret til 50 % syrligt, hvor peptidet fremstilles ved fremgangsmåden ifølge et af kravene 1 til 7.
13. 13. Peptid, som er fremstillet ved enzymatisk hydrolyse med en fraktion af
14. 15 kemisk hydrolysat tørret til 6 % fugtighed, hvor peptidet tilvejebringes ved fremgangsmåden ifølge et af kravene 1 til 7.

    öäassa Fäto? Asm Oma

    SEARCH REPORT - PATENT Application No. PA 2011 70176 1. 1 1 Certain claims were found unsearchable (See Box No. I). 2. 1 1 Unity of invention is lacking prior to search (See Box No. II). A. CLASSIFICATION OF SUBJECT MATTER A23J 3/34; A23J 1/02; A23J 1/04; A23J 3/30 (all version 2006.01); A23K 10/20 (version 2016.01); C07K 1/12; C12P 21/06 (both version 2006.01) According to International Patent Classification (IPC) or to both national classification and IPC B. FIELDS SEARCHED Minimum documentation searched (classification system followed by classification symbols) A23J, A23K, C07K, C12P (IPC & CPC) Documentation searched other than minimum documentation to the extent that such documents are included in the fields searched DK, NO, SE, FI: IPC-classes as above. Electronic database consulted during the search (name of database and, where practicable, search terms used) EPODOC, WPI, FULL TEXT: ENGLISH C. DOCUMENTS CONSIDERED TO BE RELEVANT Category* Citation of document, with indication, where appropriate, of the relevant passages Relevant for claim No. X WO 2004/021797 Al (AMI GO AS) 18 March 2004 1-5, 13-18 Y Page 3, lines 13-15; page 18, lines 19-25; claims 1, 8-9; fig. 1 6-12 Y DE 2705671 Al (ROHM GMBH) 17 August 1978 6-12 Claims 1, 4 A WO 88/05633 Al (MCLEAN, W.K. et al.) 11 August 1988 - Further documents are listed in the continuation of Box C. * Special categories of cited documents: P Document published prior to the filing date but later than the A Document defining the general state of the art which is not priority date claimed. considered to be of particular relevance. T Document not in conflict with the application but cited to D Document cited in the application. E Earlier application or patent but published on or after the filing date. understand the principle or theory underlying the invention. X Document of particular relevance; the claimed invention cannot be considered novel or cannot be considered to involve an inventive step when the document is taken alone. Y Document of particular relevance; the claimed invention cannot be considered to involve an inventive step when the document is combined with one or more other such documents, such L Document which may throw doubt on priority claim(s) or which is cited to establish the publication date of another citation or other special reason (as specified). O Document referring to an oral disclosure, use, exhibition or other means. combination being obvious to a person skilled in the art. Document member of the same patent family. Danish Patent and Trademark Office Date of completion of the search report Helgeshøj Allé 81 DK-2630 Taastrun 26 February 2016 Denmark Authorized officer Telephone No. +45 4350 8000 Facsimile No. +45 4350 8001 Peter Eisner Telephone No. +45 4350 8330

    Search Report

    SEARCH REPORT - PATENT Application No. PA 2011 70176 C (Continuation). DOCUMENTS CONSIDERED TO BE RELEVANT Category* Citation of document, with indication, where appropriate, of the relevant passages Relevant for claim No. A US 5053234 A (ANDERSON, P.S. et al.) 1 October 1991 - A FR 2835703 Al (TECHNIAGRO) 15 August 2003 - A WO 2006/096067 Al (WAHL PROCESS SYSTEMS AS) 14 September 2006

    Search Report

    SEARCH REPORT - PATENT Application No. PA 2011 70176 Box No. I Observations where certain claims were found unsearchable This search report has not been established in respect of certain claims for the following reasons: 1. 1 1 Claims Nos.: because they relate to subject matter not required to be searched, namely: 2. 1 1 Claims Nos.: because they relate to parts of the patent application that do not comply with the prescribed requirements to such an extent that no meaningful search can be carried out, specifically: 3. 1 1 Claims Nos.: because of other matters. Box No, 11 Observations where unity of invention is lacking prior to the search The Danish Patent and Trademark Office found multiple inventions in this patent application, as follows:

    Search Report

    SEARCH REPORT - PATENT Application No. PA 2011 70176 SUPPLEMENTAL BOX Continuation of Box [.]

    Search Report