CA2408551C - Protein and lipid sources for use in aquafeeds and animal feeds and a process for their preparation - Google Patents

Protein and lipid sources for use in aquafeeds and animal feeds and a process for their preparation Download PDF

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Publication number
CA2408551C
CA2408551C CA002408551A CA2408551A CA2408551C CA 2408551 C CA2408551 C CA 2408551C CA 002408551 A CA002408551 A CA 002408551A CA 2408551 A CA2408551 A CA 2408551A CA 2408551 C CA2408551 C CA 2408551C
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Prior art keywords
seed
oilseed
protein
oil
lipid
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CA002408551A
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CA2408551A1 (en
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David Higgs
Robert E. Cairns
Ian Shand
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Canada Minister of Fisheries and Oceans
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Canada Minister of Fisheries and Oceans
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Priority claimed from CA002335745A external-priority patent/CA2335745A1/en
Application filed by Canada Minister of Fisheries and Oceans filed Critical Canada Minister of Fisheries and Oceans
Priority to CA002408551A priority Critical patent/CA2408551C/en
Priority to CA002482299A priority patent/CA2482299A1/en
Priority claimed from PCT/CA2001/000663 external-priority patent/WO2001084949A2/en
Publication of CA2408551A1 publication Critical patent/CA2408551A1/en
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    • 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
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A40/00Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
    • Y02A40/80Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in fisheries management
    • Y02A40/81Aquaculture, e.g. of fish
    • Y02A40/818Alternative feeds for fish, e.g. in aquacultures

Abstract

A process for producing cold pressed human food grade plant oils, nutritionally upgraded oilseed meals, highly digestible protein concentrates, animal feed grade lipid sources, and constituents suitable for inclusion in organic fertilizers. The oilseed may be raw cold pressed/dehulled, heat-treated cold pressed/undehulled, heat-treated cold pressed/dehulled or heat-treated/dehulled seed. A source of minced and hydrolyzed animal offal is used and the oilseeds and the animal offal are blended together to form a mixture.
Products produced by the process are also included.

Description

PROTEIN AND LIPID SOURCES FOR USE IN AQUAFEEDS AND
ANIMAL FEEDS AND A PROCESS FOR THEIR PREPARATION
Field of the Invention The present invention relates to a novel process for the production of nutritionally upgraded protein and lipid sources for use in aquafeeds and other animal feeds. More specifically, the present invention relates to a process involving the co-processing of animal offal(s) with oilseed(s); the invention also relates to products produced thereby.

In addition, the invention relates to cold pressed plant oils suitable for organic human'foods, as well as products for use as components in organic fertilizers, both produced by the process of the invention.

Background of the Invention Feed accounts for on average 35-60% of the operating costs of salmon farms and it represents the largest cost in the culture of other carnivorous aquatic species. Moreover, the protein sources presently used account for about 51 % of the total feed cost and this percentage can be higher than this when increased reliance is placed on imported premium quality fish meals. The latter mainly originate from South America through the processing of whole pelagic fish species like sardines and anchovies and they are used to meet most of the dietary protein needs of farmed Canadian salmon. Accordingly, salmon farming profitability is marginal in Canada.

Currently, aquatic feeds contain high levels of fish meal and oil, which are mostly imported, to produce a protein-rich and sometimes lipid-rich (e.g.
salmon diets) aquatic feed. However, as noted hereinabove, such fish meal and oil can be very expensive and this will be especially true in the future due to progressively increasing demands that are being placed on the finite global supplies of fish meal and oil. Hence, alternative economical sources of protein and lipid are required.
2 One known approach is to use less expensive plant protein sources in aquafeed that have been specially processed so that they are in the form of nutritionally upgraded protein meals, concentrates, and isolates. These may be used either singly or in combination with rendered animal protein ingredients such as poultry-by-product meal. To date, each of these protein products, such as canola meal, soybean meal, and poultry-by-product meal have been processed (produced) separately and then these protein sources have been blended together in dried and finely ground form in appropriate ratios for a particular aquatic species at the time of diet formulation and preparation.

U.S. Patent No. 4,418,086 to-Marino et al. discloses the preparation of an animal feed which comprises (a) a proteinaceous matrix, (b) fat or oil, (c) a sulfur source, (d) farinaceous material, (e) a plasticizer and (f) water. The method disclosed involves the blending of the ingredients together, introducing the mixture into an extruder and subjecting it to shear forces, mechanical work, heat and pressure such that the product temperature prior to discharge is at least 280 degrees F. This patent is concerned with the production of an animal feed with a "meat like texture".

U.S. Patent No. 3,952,115 to Damico et al. relates to a feed where an amino acid is utilized as an additive to fortify a proteinaceous feed.

U.S. Patent No. 4,973,490 to Holmes discloses the production of animal feed products utilizing rape seed in combination with another plant species.
U.S. Patent No. 5,773,051 to Kim relates to a process for manufacturing a fish feed which refloats after initially sinking. This document discloses a process including blending conventional fish feed containing fish meal, wheat meal, soybean meal and other substances and compressing the mixture at a constant temperature to produce a molded product.
3 Summary of the Invention In the present invention, there are several different aspects represented by different process aspects, as well as several novel product compositions resulting from different process aspects.

Dealing initially with the process aspects, there is provided a first aspect involving the preparation of nutritionally upgraded oilseed meals, which are protein and lipid-rich and have a reduced fibre content, and plant oils from oilseeds for use in fish or other non-human animal diets or human foods.
This process comprises the steps of:
- providing a source of an oilseed;
- subjecting said oilseed to a non-aqueous heat treatment at a temperature sufficient to reduce the concentration of at least some antinutritional components normally present in said oilseed to obtain a heat-treated seed;
- dehulling the heat-treated seed to produce a meat fraction and a hull fraction or a mixture thereof; and - cold pressing said meat fraction or said mixture to yield said plant oils and said protein and lipid-rich meals with reduced hull content.
According to a second aspect of the present invention, there is provided a process for preparation of nutritionally upgraded oilseed meals, which are protein and lipid-rich and have a reduced fibre content, and plant oils from oilseeds for use in fish or other non-human animal diets or human foods comprising the steps of:
- providing a source of oilseed;
- subjecting said oilseed to heat treatment to substantially reduce the concentration of at least some antinutritional components normally present in said oilseed to obtain heat-treated seed;
- providing a source of unhydrolyzed animal offal;
- blending said heat-treated seed in particulate form with said animal offal to form a mixture thereof;
4 - cooking said mixture under conditions selected to substantially improve protein digestibility, and substantially free cellular water present in said animal offal, as well as to facilitate separation of protein from the lipid in said oilseeds to obtain a cooked mixture; and - separating said cooked mixture into a stickwater fraction, a moisture containing protein-rich fraction, and an animal feed grade oil fraction.

In a third aspect of this invention, the above-described second aspect can be modified as described herein to provide the third process aspect. In particular, in the above second aspect, the modifications involve the further steps of:
- providing a source of an unhydrolyzed animal offal;
- blending said protein and lipid-rich meal with said unhydrolyzed animal offal to form a mixture thereof;
- cooking said mixture under conditions selected to improve protein digestibility, and free cellular water present in said unhydrolyzed animal offal, as well as to facilitate separation of a protein from a lipid to obtain a cooked mixture; and - separating said cooked mixture into a stickwater fraction, a moisture containing protein-rich fraction, and an animal feed grade oil fraction.
A fourth aspect of the process of the present invention involves the preparation of protein concentrates and lipid sources from the co-processing of animal offal with raw oilseeds for use in fish or other non-human animal diets. The fourth process aspect comprises the steps of:
- providing a source of raw oilseed;
- cold pressing said oilseed under conditions to substantially reduce the particle size of said oilseed and obtain pressed raw seeds;
- providing a source of unhydrolyzed animal offal;
- blending said pressed raw seeds with said animal offal to produce a mixture thereof;
- cooking said mixture under conditions to substantially improve protein digestibility, and substantially free cellular water present in said animal offal and facilitate separation of protein from the lipid in said animal offal and said oilseed to obtain a cooked mixture; and - separating said cooked mixture into a stickwater fraction, a moisture containing protein-rich fraction, and an animal feed grade oil fraction.
In a fifth aspect of the. present invention, there is provided a process for preparation of protein concentrates and lipid sources from the co-processing of animal offal with dried and then dehulled oilseeds for use in fish or other non-human animal diets. In this.fifth aspect, the process comprises the steps of:
- providing a source of oilseed;
- drying said oilseed to produce a dried seed;
- dehulling said dried seed to produce a meat fraction and a hull fraction or a mixture thereof;
- cold pressing said meatfraction or mixture under conditions selected to substantially reduce particle size of said meat or mixture to yield a high value human grade oil and protein and lipid-rich meals with reduced fibre content;
- providing a source of unhydrolyzed animal offal;
- blending said protein and lipid-rich meal with said animal offal to form a mixture thereof;
- cooking said mixture under conditions selected to substantially improve protein digestibility, substantially free cellular water present in said animal offal and facilitate separation of protein from the lipid in said animal offal and said oilseeds to obtain a cooked mixture; and - separating said cooked mixture into a stickwater fraction, a moisture containing protein-rich fraction, and an animal feed grade oil fraction.

In a sixth aspect of the present invention, there is provided a process for producing a protein concentrate for use in animal and aquafeeds. As such, the sixth aspect process steps comprise:
- providing a source of oilseed ;
- drying'said oilseed to reduce its moisture content to beiow about 10% to obtain dried seed or subjecting said oilseed to heat treatment under conditions selected to substantially deactivate, destroy or reduce the concentration of at least some of the antinutritional components normally present in the oilseed to produce a heat-treated seed;
- cold pressing or grinding said dried seed or heat-treated seed to reduce the particle size and yield human grade oil;
- providing a source of unhydrolyzed animal offal;
- blending said oilseed and said animal offal in ratios from about 10:90 to about 90:10 form a mixture thereof;
- extracting said mixture with a solvent; and - removing said solvent to obtain a protein concentrate.

In the first aspect of the process, as an optional feature, the process may further include the step of extracting said protein and lipid-rich meals with a solvent. The protein rich fraction of the second to fifth aspects of the process may also be subjected to a solvent extraction to obtain a protein concentrate.
In all of the above process aspects, there may also be included the step of stabilizing said plant oils by adding an antioxidant.

In the sixth process aspect, there may be also included the step of cooking said mixture to obtain a cooked mixture prior to said extracting step. In this embodiment, there may be further included the step of separating said cooked mixture into a stickwater fraction, a moisture containing protein-rich fraction, and an animal feed grade oil. If desired, there also may be provided the step of drying the protein concentrate.

In each of the second to fifth embodiments, one may also include, if desired, the step of drying said protein-rich fraction to reduce its moisture content to below about 10%, preferably 6% to 9%.

In other preferred embodiments, in any of the first, second, third or sixth process aspects, desirably the heat treatment is a rapid heat treatment.
The heat treatment may be carried out in one or more stages - for example, a two stage heat treatment can be employed where temperatures range from about 100 C to 115 C, and for treatment times ranging from 1.5 minutes to 30 minutes or more depending on the specific components being treated.
Particularly suitable for the first four process aspects, as well as the sixth aspect, is where the oilseed is selected from the group consisting of canola, rape seed, soybeans, sunflower seed, flax seed, mustard seed, cotton seed, hemp and mixtures thereof. In either of the first, third, fourth or fifth process aspects, the oilseed may be selected from the group consisting of canolaTM
rape seed, sunflower seed, flax seed, mustard seed, cotton seed and mixtures thereof. In either of the second or sixth process aspects, the oilseed may also be a commercially available processed ground oilseed meal. In this case, the initial steps involving rapid heat-treatment and cold pressing are deleted. In the fifth process aspect, particularly suitable is where the oilseed is sunflower. Particularly suitable for the sixth process aspect is where the oilseed is selected from the group consisting of canolaTM, soybeans, cotton seed, sunflower, hemp and mixtures thereof.

In the second to sixth aspects of the invention, the animal offal may be selected from the group consisting of fish processing waste, whole fish, fish by-catch, squid offal, whole birds, beef offal, lamb offal and mixtures thereof.
Particularly suitable in the sixth aspect is where the animal offal is a fish product or poultry. In preferred embodiments of these second to sixth aspects, squid offal, poultry offal without feet, and whole birds including chickens, turkeys and others without feathers can be used. In more preferred embodiments, the fish offal or whole fish utilized include fish species having low levels of chlorinated hydrocarbons and heavy metals such as mercury.
In all the above-mentioned aspects, preferred animal offal is a minced unhydrolyzed animal offal. Also in these aspects if desired, the process may include the step of dehulling the heat-treated seed and the blending step may include adding hot water to the mixture.

The dehulling step in the first to third, fifth and sixth process aspects may be carried out by a mechanical treatment with a gravity screening or air-classification step or both and may also further include a seed sizing step before subjecting said oilseed source to treatment. Optionally the oilseed can be treated by suitable techniques to remove the outer mucilage layer of the seed coat before the seed is used; the preferred oilseed used in this embodiment includes flax seed. In accordance with another embodiment, especially when producing aquatic feeds, oilseed selected from canolaTM
soybeans, sunflower seed, hemp or delinted cotton seed or mixtures thereof is used, due to their global availability, cost, and/or high quality of protein and/or lipid.

In the second to sixth aspects, the cooking step may be performed at a temperature of from about 90 C to about 93 C and may further include the step of adding an antioxidant and/or a palatability enhancer to the cooked mixture. In preferred embodiments, in these second to sixth process aspects, the antioxidant may be selected from the group consisting of ethoxyquin (santoquinTM), butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT), tertiary butyl hydroquinone, natural antioxidants and mixtures thereof.
One or more of the foregoing antioxidants are also added to the dried protein concentrate, and the animal feed grade lipid fraction. In the case of the former, the amount of antioxidant utilized is from about 200 ppm to about 250 ppm whereas the latter is supplemented with about 250 ppm to about 500 ppm antioxidant(s). In preferred embodiments, combinations of BHA and ethoxyquin or ethyoxquin alone at highest level is used. The palatability enhancer may be,selected from the. group consisting of natural and synthetic products based on krill, euphausiids and derivatives thereof, squid, FinnstimTM and mixtures thereof. In preferred embodiments of the invention, other ingredients such as enzymes, fillers, as well as other sources of lipid of plant or animal origin and other protein sources such as heat-treated field peas or lupins may be added to the composition of the mixture.

The oilseed and the animal offal inAthe second to fifth process aspects are mixed together in a ratio of about 10:90 to about 90:10 by weight. Preferred ratios in these aspects, as well as in the sixth process aspect is from about 25:75 to about 75:25 by weight or from about 60:40 to about 40:60 by weight.
The amount of oilseed present in the mixture depends upon the sources of oilseed and animal offal actually used. This amount also depends on respective attendant concentrations of protein and lipid, as well as costs. In accordance with one embodiment, the oilseed is present in a range of about
5% to about 78% by weight. In preferred embodiments, the oilseed is present in the amount of about 22% to about 78% by weight, and in more preferred embodiments, the range is of about 40% to about 60% by weight.
In accordance with another embodiment, it is important to maintain an .. A
optimal ratio of water (from endogenous and exogenous sources) to the oil-free dry matter content of the oilseed in the initial mixture and usually this is found within the range of about 3-6:1 w/w. Ratios within this range facilitate the removal of water soluble antinutritional factors from the oilseed (in press liquor).

The mixture is further pressed and/or centrifuged using respectively either a screw press equipped with perforated screens, an expeller equipped with flat steel bars set edgewise around the periphery and spaced to allow the fluids to flow between the bars, a decanter centrifuge or any combination of these. In preferred embodiments, depending upon the efficiency of liquid/solid separation the mixture is centrifuged before or after the presscake has passed through the screw press or expeller. This part of the process removes fluids generally comprised of water that contains some soluble 10 protein and water soluble antinutritional factors stemming from the oilseed such as glucosinolates, phenolic compounds and unwanted sugars including oligosaccharides (raffinose and stachyose). Animal feed grade plant oil that is enriched with fatty acids from the animal offal lipid is also removed.

The drying step in the second to sixth process aspects may be performed at a temperature of between about 70 C to about 85 C. As mentioned above, the separation step may be carried out in a$crew press, expeller press or decanter centrifuge, or any combination thereof. As an optional feature, the stickwater fraction obtained after separation may be further condensed to yield condensed solubles. Preferred embodiments in these process aspects further comprise, if desired, the step of stabilizing said condensed solubles with an inorganic acid.

In each of the second to sixth process.aspects, the step of incubating said mixture in the presence of one or more enzymes prior to the cooking step may further be included. Preferred enzymes used in this embodiment include the enzyme phytase.

When a palatability enhancer is utilized, it may be selected from conventional products based on krill, euphausiids, and/or squid or other like palatability enhancers such as FinnstimTM or the like. The palatabiity enhancers may be added to the dried protein concentrates in amounts ranging from about 1%
to about 3% by weight.

The cooking step in the second to sixth process aspects is carried out using a heat exchanger or through direct steam injection coupled with batch processor. In these aspects as well as in the sixth aspect, the process may further comprise, if desired, the initial step of deboning said animal offal to produced deboned animal offal and bones.

The cold pressing step in any of the first, third, fourth, fifth or sixth process aspects should be carried out at a temperature not exceeding 85 C, desirably below about 70 C.

In the second and sixth embodiments of the process of the present invention, the source of the oil seed utilized is most desirably a commercially available particulate processed oil seed meal, which has not been previously subjected to initial rapid heat treatment or cold processing.

The extraction step in the second to sixth process aspects may be carried out at least twice; preferably the solvent used is or includes hexane.

An optional feature of various processes described above which involve processing of oilseed prior to co-processing it with animal offal, can utilize the addition of hot water (from about 37 C to about 55 C) to ground oilseed, followed by adjustment of the pH to a value of from about 5.5 to about 6.0 using an inorganic acid such as sulphuric acid; this treatment being carried out in the presence of an enzyme such as the enzyme phytase.

The various processes of the present invention can be economically and readily carried out using conventional equipment. Such processes will provide cost effective products which can be used in place of or added to other known products in order to achieve additional sources of the desired ingredients for use in fish or other non-human animal diets or human foods.
The use of inexpensive fish wastes and other animal offal in the various processes of the present invention is a positive way to deal with waste streams rather than considering them as a liability.

As described hereinafter, it will be seen that the different processes can be combined into one overall procedure allowing separation of products at various stages of the process.

lo Turning now to the various novel products and compositions according to the invention, the first product aspect relates to a protein source having from about 40% to about 80% protein, desirably from about 55% to about 77%
protein calculated on a(ipid-free dry weight basis, said source being adapted for use in animal and aquafeeds and comprising an admixture of treated oilseed protein and animal offal whereby said admixture is characterized by at least one of the following:
- enriched concentrations of essential amino acids and bioavailable minerals relative to those present in said animal offal or untreated oilseed;
ZO - enriched concentrations of highly unsaturated n-3 fatty acids relative to those present initially in said oilseed if said source of animal offal is fish;
- reduced concentrations of heat-labile and water soluble antinutritional factors in an amount of at least 20% by weight relative to non-treated oilseed protein;
- increased protein digestibility relative to non-treated oilseed protein;
and - a lipid concentration of less than 10% of dry weight of said source.

The first product aspect of the invention may also have a reduced content of heat-labile and antinutritional components of at least 80% calculated on a lipid-free dry weight basis. This product may further comprise if desired, an antioxidant which may be selected from the group consisting of ethoxyquin (santoquin), butylated hydroxyanisole, butylated hydroxytoluene, tertiary butyl hydroxyquinone, natural antioxidants and mixtures thereof. The amount of antioxidant utilized will range depending on the components; generally speaking, this will be from about 200 ppm to about 250 ppm in the protein concentrate, and the animal feed grade lipid fraction resulting from the production of the concentrate may be supplemented with about 250 ppm to ,. .
about 500 ppm"antioxidants.. In preferred embodiments, a combination of BHA and ethoxyquin or ethoxyquin alone at highest levels is used.

The above product invention also comprises enrichment of at least one amino acid selected from the group consisting of arginine, histidine, isoleucine, leucine, lysine, methionine, cystine, phenylalanine, tyrosine, threonine, tryptophan, and valine. Preferred amino acids altered in this product are selected from lysine, methionine or cystine. This product also comprises enrichment of at least one mineral selected from the group consisting of calcium, phosphorus, magnesium, sodium, potassium, copper and zinc. Preferred minerals altered in this product are selected from calcium, phosphorus, sodium, zinc or mixtures thereof.

This first product comprises enrichment of at least one n-3 highly saturated fafty acid; this is preferably at least one fatty acid selected from eicosapentaenoic acid (20:5n-3) and docosahexaenoic acid (22:6n-3) if said source of animal offal is fish.

The heat-labile and water soluble antinutritional components in the first product are most desirably selected from glucosinates, phenolic compounds including sinapine, chlorogenic acid, oligosaccharides, trypsin inhibitor, saponins and isoflavones or mixtures thereof.

The digestibility of the first product of the invention is about at least 89%
for Atlantic salmon in sea water (fecal settling columns or the Guelph System of fecal collection was used). This percentage may vary and is desirabiy as high as possible, e.g., in the order of from about 92% to about 100%.

The oilseed in the first product of the invention is selected from the group consisting of canolaT"", rapeseed, soybeans, sunflower seed, flax seed, mustard seed, cotton seed, hemp and mixtures thereof. In preferred embodiments, as an optional feature, the oilseed may be heat-treated.

The animal offal in the first product is most desirably selected from the group consisting of whole fish, fish by-catch, fish processing waste, squid offal, whole birds, beef offal, lamb offal and mixtures thereof.

The protein and lipid contents of the first product are present in an amount within the range (respectively) of about 50% to about 77% calculated on a lipid-free dry weight basis and less than about 10% by weight if the step involving organic solvent extraction has been employed.

In accordance with a further embodiment, phytate-reduced protein products can be produced. The process involves an additional step consisting of adding hot water (temperature of about 37 C to about 55 C) to the ground oilseed in the presence of the enzyme phytase. It should be mentioned that the moisture content of the ground oilseed should be raised to about 80% or more and the pH should be about 5.5 to about 6.0 by addition of an inorganic acid, such as sulphuric acid. The mixture is then incubated for about 30 minutes and not more than 240 minutes, before being mixed with the animal offal.

The protein source of this first product finds particular use for animal and fish feeds to cost effectively and extensively replace high nutritive value protein sources such as premium quality fish meal, or conventionally processed oilseed meals that have lower nutritional value. The advantage of the above products according to the present invention, is that they may be produced in a very economical manner by co-processing sources of protein that heretofore have been processed separately without the attendant benefits of enhancing the nutritive value of the oilseed protein fraction through protein and mineral complementation from the animal offal and by concurrent 10 reduction of the concentrations of heat-labile and water soluble antinutritional factors as well as phytic acid if the optional initial step of phytase pretreatment of the oilseed is adopted. These protein products provide significant advantages to animal and fish feed manufacturers which in addition to the economic savings, also provide highly desirable and digestible proteins that have excellent amino acid profiles relative to the essential amino acid needs of commercially important animals and fish.

A second aspect of the invention relates to another product which is an edible human food grade oil comprising an oilseed oil, the human food grade oil having been obtained by cold pressing oilseed in which the cold pressing was carried out at temperatures below 85 C, said oil having minimal lipid oxidation products and a peroxide value of less than about 2 milliequivalents per kg.
The oilseed providing the oil of the second product is preferably selected from canolaT'", rape seed, sunflower seed, flax seed, mustard seed, cotton seed and mixtures thereof. In more preferred embodiments, the oilseed is heat-treated.

The edible organic or human food grade oils of this aspect of the present invention provide highly nutritional products which can be used for human consumption. Such oils may be packaged and distributed per se or may be incorporated into various types of foods or food compositions where edible oils are required or utilized.
A further advantage of such organic oils is that they have not been subjected to any organic solvent or other processing steps that would reduce their concentrations of natural antioxidants. Moreover, they are generated under conditions that minimize lipid peroxidation and the products that result from the process. They are highly desired by health conscious people who are concerned with ingesting vegetable oils close to their natural state. Hence, these oils command a premium price in the market place.

A third product aspect relates to an animal feed grade oil for use in animal and aquafeeds comprising an admixture of treated oilseed oil and animal offal, said admixture having an enriched n-3 highly unsaturated fatty acid content (20:5n-3 + 22:6n-3) relative to non-treated oilseed oil if the animal offal used is fish or poultry that have been fed diets comprising adequate concentrations of one or more fish products. The oilseed oil of the third product is desirably oil derived from seeds selected from canolaTMsoybeans, sunflower seed, flax seed, hemp and mixtures thereof. In this third product, the oil utilized may be derived from oilseed that has been heat-treated.
Preferred oilseeds in this embodiment is oil derived from canola seed since the product may further comprise an enriched monounsaturated fatty acid content (18:1 n-9) relative to non-treated oilseed oil.

The feed grade oils of this aspect of the present invention will find utility in animal and fish foods; they have the advantage that they can be produced in a very efficient and economic manner and they provide highly nutritional sources of enriched unsaturated fatty acid contents. The latter lipid sources are highly desirable particularly for use in fish feeds to partially replace premium quality fish oil that may be expensive and difficult to obtain. This is specially true if the plant oil fraction has been enriched with n-3 highly unsaturated fatty acids from the fish offal fraction. These oils can be utilized individually or, if desired, combined with other known and conventional oils at the time of feed manufacture.

A fourth product aspect relates to a constituent for an organic fertilizer comprising at least one of canola, sunflower, soybean, mustard seed, cotton seed and hemp hulls, said hulls being dried hulls and containing protein and lipid. In preferred embodiments of this fourth product aspect, the hulls are heat-treated hulls. As a constituent for organic fertilizers, the fourth product can be used in combination with other conventional fertilizer components such as sawdust. As a result of adding this constituent, fertilizers have the advantage of a readily available source of nitrogen. The hulls will act as soil conditioner and carrier for nutrients, these being delivered to the soil on a sustained basis. In addition, the fourth product of the invention will facilitate soil irrigation and water retention in soils. This feature is particularly important in times of drought.

A fifth product aspect relates to a composition of condensed solubles for use as constituents in organic fertilizers comprising an admixture of treated oilseed and animal offal whereby said admixture has an enriched soluble nitrogen content, water soluble carbohydrate content, water soluble antinutritional component content and mineral content.

In accordance with a preferred aspect of the invention, the original hull fraction may be directed for use in ruminant diets either as is or pretreated with carbohydrases. In accordance with another embodiment, the original hull fraction is used in the production of organic fertilizers where it serves as a carrier medium that is completely broken down enzymatically during aerobic or anaerobic decomposition processes.

The oilseed in the fifth product is selected from canolaTM, rape seed, soybeans, sunflower seed, flax seed, mustard seed, cotton seed, hemp and mixtures thereof. Optionally in this fifth product, the oilseed may be heat-treated.
The animal offal in the fifth product of the invention is selected from fish processing waste, whole fish, fish by-catch, squid offal, whole birds, beef offal, lamb offal and mixtures thereof.

The water soluble antinutritional component in the fifth product is selected from glucosinates, phenolic compounds including sinapine, chlorogenic acid, oligosaccharides, saponins or isoflavones. In this fifth product, the soluble carbohydrate is selected from monosaccharides, disaccharides and ,,.
oligosaccharides.
The mineral in the fifth product is selected from calcium, phosphorus, magnesium, sodium, potassium, copper, iron and zinc.

This fifth product is enriched with soluble nitrogen, phosphorus, potassium, as well as organic nutrients. As a constituent for organic fertilizers this product contributes to upgrade the quality of the fertilizer. It should stimulate plant growth, specially the root structure of plants.

The condensed soluble products of the fifth aspect of the present invention may be utilized with other fertilizer components to provide enhanced fertilizers. As described above with respect to the fourth aspect, also relating to fertilizers, the condensed solubles can be incorporated into known fertilizers or, if desired, could be marketed as additives per se to known fertilizers.

There is also provided a sixth product according to the present invention which relates to a protein and lipid-rich oilseed meal suitable for use in fish and non-human animal diets. This product comprises a heat-treated dehulled oilseed, said oilseed being substantially free of flaxseed, mustard seed, rapeseed and cotton seed, said meal having:
- from about 26% to about 40% protein on a dry weight basis;
- from about 48% to about 64% protein on a lipid-free dry weight-basis;
-from about 2.4% to about 4.6% methionine and cystine calculated as a percent of said protein;
-from about 3.6% to about 6.1 % lysine calculated as a percent of said protein;
- from about 21 % to about 52% lipid on a dry weight basis;
- from about 2% to about 12% crude fibre on a lipid-free dry weight basis;
- from about 0.16% to about 0.45% calcium on a lipid-free dry weight basis; and - less than about 0.01 % sodium on a lipid-free dry weight basis.
The sixth product of the present invention may further comprise at least one of trypsin inhibitor, glucosinolates, sinapine, chlorogenic acid and mixtures thereof. In preferred embodiments of this sixth product aspect, the trypsin inhibitor is in an amount of up to about 8000 units/g on a lipid-free dry weight basis; the glucosinolates are in an amount of up to about 20 moles/g of total glucosinolates on a lipid-free dry weight basis; the sinapine is in an amount of up to about 2.1 % on a lipid-free dry weight basis; and the chlorogenic acid is in an amount of up to about 3 !o on a lipid-free dry weight basis.

The oilseed in this sixth product may be partially or totally dehulled.

The protein and lipid rich meals of the sixth product of the present invention can be produced in a very economical manner and will find utility in fish and animal feeds requiring high_ protein and lipid rich meal with reduced concentrations of fibre and heat-labile antinutritional factors. . Their utility will depend on various factors such as the species of animal or fish and their respective requirements for protein and energy, etc. As described previously with respect to other animal and fish feed sources, the products of this aspect of the invention can be incorporated into the feeds of animal and fish as-replacements for conventionally processed oilseed meals and oils, and fish meals and oils. Due to the protein and lipid rich content of such products, a beneficial result will be obtained in the increased digestible energy content of diets for such animals and fish. The protein concentration can also be increased in the preceding meals through removal of lipid by solvent extraction which increases their utility as components in low energy diets for 10 animals and fish.

In a seventh product aspect of the present invention, there is provided a protein concentrate containing an admixture of a co-processed oilseed and unhydrolyzed animal offal, said concentrate being suitable for use in fish and non-human animal diets, said oilseed comprising a heat-treated dehulled oilseed substantially free of flaxseed, mustard seed, rapeseed and cotton seed, said protein concentrate having:
- from about 38% to about 58% protein on a dry weight basis;
- from about 52% to about 77%, desirably up to about 57% protein on a lipid-free dry weight basis;
20 -from about 2.7% to about 4.6% methionine and cystine calculated as a percent of protein;
-from about 4.3% to about 7.9% lysine calculated as a percent of said protein;
- from about 24% to about 37% lipid on a dry weight basis;
- from about 1.7% to about 10% crude fibre on a lipid-free dry weight basis;
- from about 0.7% to about 3.6% calcium on a lipid-free dry weight basis; and - from about 0.06% to about 0.30% sodium on a lipid-free dry weight basis.

The seventh product may further comprise at least one of trypsin inhibitor, glucosinolates, sinapine, chiorogenic acid and mixtures thereof. In preferred embodiments of this seventh product aspect, the trypsin inhibitor is in ari amount of up to about 2500 units/g on a lipid-free dry weight basis; the glucosinolates are in an amount of up to 4.0 moles/g of total glucosinolates on a lipid-free dry weight basis; sinapine is in an amount of up to about 1.2%
on a lipid-free dry weight basis; and the chlorogenic acid is in an amount of up to about 1.7% on a lipid-free dry weight basis.

The oilseed in this seventh product may be partially or totally dehulled if desired.

The high digestible protein content, moderate content of highly digestibie lipid, reduced fibre content and substantially reduced heat-label and water soluble antinutritional factor content of the seventh product make them suitable as major replacements for fish meal and other conventional sources of protein used in fish and non-human animal diets. Their enriched content of at least some of the essential amino acids and minerals, togetherwith their economical cost of production will make such products highly desirable as feed stuff commodities throughout the world.

In an eighth product aspect of the present invention, there is also provided an animal feed grade oil comprising oil derived from an admixture of a co-processed oilseed and unhydrolyzed animal offal, said oil being substantially free of flaxseed oil, mustard seed oil, rapeseed oil and cotton seed oil, said animal feed grade oil having:
- from about 60% to about 92% of total fatty acids as unsaturated fatty acids;

- from about 8% to about*50% of total fatty acids as (n-6) fatty acids;
- from about 0.5% to about 35% of total fatty acids as (n-3) fatty acids;
- from about 3% to about 25% of total fatty acids as n-3 highly unsaturated fatty acids; and - a peroxide value less than about 8 milliequivalents per kg of oil at the time of production.

The oilseed in this eighth product may be a raw oilseed or a heat-treated oilseed. In preferred embodiments of this eighth product, the animal offal is a fish product and the product further comprises (20:5n-3+22:6n-3).
The eighth product has a generally high content of n-3 highly unsaturated fatty acids compared to the oil from the initial oilseed used if the source of animal offal is fsh and hence it is desirable for use in both fish and animal diets. The additional benefits of this type of product include ease of production, economical attributes, readily available sources of natural products for obtaining the oil, and its adaptability to incorporation into existing animal diets, as well as its utility as a separate dietary component.
A ninth product aspect of the present invention relates to an edible organic oil comprising oil of cold pressed heat-treated oilseed, said oil being substantially free of flaxseed oil, mustard seed oil, rapeseed oil and cotton seed oil, said organic oil comprising:
- from about 86% to about 96% of total fatty acids as unsaturated fatty acids;
-from about 20 to about 80% of total fatty acids as (n-6) fatty acids;
and - a peroxide value of less than about 2 milliequivalents of peroxide per kg oil at the time of production.

The ninth product may further comprise up to about 22% of total fatty acids as (n-3) fatty acids.

The oilseed in the ninth product may be undehulled, partially dehulled or totally dehulled if desired. This ninth product is a very cost-effective organic oil for the increasing organic human food industry. As described above with respect to the second product embodiment of this invention, the oil of this embodiment will find utility in various types of food products or as a separate product in and of itself.

In different embodiments of the products of the present invention, depending on their intended utility, particularly preferred embodiments are those where the animal feed grade oil, is an oil derived from raw oilseed;
likewise, in another embodiment, the edible organic oils may be derived from raw oilseed.

It will be understood that reference to the above described products which are suitable for animal and fish feeds, refers to products which can be used by numerous types of species. For example, depending on the geographic location, fish feeds are used in fish farming operations for salmon, trout, tilapia, carp, catfish, sea bream and many other warm water as well as cold water species of commercial importance. In the case of animal feeds, conventional farmingApractices utilize such feeds for poultry, hogs, swine and cattle.

In further explanation of the various embodiments of both the products and process aspects of the present invention, the solvent used for extracting the mixture obtained from co-processing of oilseed and animal offal includes hexane or other compatible solvents used in the animal feed or human food industry.

In various embodiments of the process and product aspects of the present invention, the ash content in the protein concentrates can be regulated as desired by controlling the concentration of bone in the animal offal. Thus, the ash can be controlled by using a deboning step to obtain offal with the desired bone content. Bones in wet or dry form of different types of offal can be utilized, with varying degrees of bone coarseness. By way of example, the ash content can thus be controlled by controlling the amount of bone added to the mixture of oilseed and animal offal.

In the process and product aspects of the present invention, when referring to animal offal such as birds or chickens, it is to be understood that a most preferred embodiment is the use of offal without bird feathers.

In both the process and product aspects of the present invention, when using dehulled seeds, the term "dehulled" is intended to mean seeds which have substantially all of their hulls removed. However, in many cases, partially dehulled seeds can be employed as otherwise noted herein, and to this end, dehulled seeds are those which have had at least 55% of their hulls removed.

The above described products can be produced by the various processes described herein; specific embodiments of such processes producing the products will be described hereinafter in greater detail.

As used in the specification, the term "unhydrolyzed" in describing the animal offal refers to animal offal which has less than about 20% by weight of hydrolyzed content, desirably less than 5% and most desirably no hydrolysis whatsoever (fresh, unspoiled). In most preferred embodiments, the amount of hydrolyzed content is as close as possible to 0% in order to best achieve the highest nutritive value in the products that are formed.

In this invention, the animal offal is preferably in a particulate form such as that which would be obtained by processing procedures resulting in minced offal. Well known techniques in the offal 'processing art can be employed to obtain such minced offal.

Brief Description of the Drawing Having generally described the invention, reference will be made to the accompanied drawing which illustrates the preferred embodiments only.
Figure 1 is a schematic representation of the process according to the present invention.

Detailed Desci-iption of the Invention 10 The steps involved in the process of the invention are broadly represented in Figure 1. In this Figure, there is illustrated a schematic representation of the co-processing of animal offal(s) with oilseed(s) to yield cold pressed oil indicated as product 1; hulls from dehulled oilseed meats indicated as product 2; nutritionally upgraded oilseed meal produced from heat treated, dehulled and cold pressed oilseed indicated as product 3; animal-feed grade oil indicated as product 4; condensed solubles indicated as product 5; and high nutritive value protein concentrate indicated as product 6. Other products of the invention are obtained by further processing the above-mentioned products as will be described in greater 20 detail hereinafter.

In accordance with certain embodiments of the invention, undehulled oilseed (A) is used in the process. Other embodiments involve dehulled seed (B) and raw seed. Dehulled seed is preferred when it is desired to feed monogastric species such as fish and poultry, and the preferred raw seed used in this embodiment inciudes 'canola, sunflower, or delinted cottonseed.

The following examples are presented to describe embodiments of the invention and are not meant to limit the invention unless otherwise stated.

Examples 1 to 10 outlined below described each step involved in the process of the invention:

EXAMPLE 1: Animal offal A common batch of whole Pacific herring was used as the main source of animal offal for the project. Soon after the herring were caught, they were rapidly block frozen by McMillan J.S. Fisheries Ltd., Vancouver, BC and stored at -40 C for about 9 months.
At this time, about 500 kg of herring were transported to the Department of Fisheries and Oceans, West Vancouver Laboratory where they were held at -20 C until small batches of about 50 kg were partially thawed for each test run. The thawed herring were cold extruded using a Butcher Boy equipped with an auger, cutter knife, and perforated plate having holes with diameter 9.52 mm.

Fresh poultry offal (heads and viscera minus feet) was also used for some trials that involved co-processing the offal with partially dehulled animal feed grade sunflower seed (designated as batch 2 hereinafter). The offal was obtained from West Coast Reduction Ltd., Vancouver, BC and was stored for one night at -20 C under cover before being handled as described above for the herring.

EXAMPLE 2: Oilseeds The four oilseeds that have been tested successfully in this project include Goliath canola seed (CloutierAgra Seeds Inc., Winnipeg, MB), soybeans (infraReady Products Ltd., Saskatoon SK), sunflower (completely dehulled confectionary grade seed obtained from North West Grain, St. Hilaire, MN, USA (batch 1) and undehulled animal feed grade seed obtained from Cargill Incorporated, Wayzata, MN, USA; batch 2), and devitalized hemp seed (Seedtec/Terramax, Qu'Appelle, SK sterilized by lnfraReady Products Ltd., Saskatoon SK). Delinted glandless cottonseed (California Planting Cottonseed Distributor, Bakersfield, CA, USA) and brown flax (InfraReady Products Ltd., Saskatoon, SK) were also tested in the process. The analytical results pertaining to products based on the former are pending. It was concluded that flax seed would be suitable for the process provided that the seed is almost totally dehulled or the outer mucilage layer of the seed coat is removed through an economical process.
EXAMPLE 3: Heat treatment or micr=onization of oilseeds In a preferred embodiment of the invention, specially for canola, soya, flax and hemp, an initial heat treatment was performed. The process involved subjecting the whole seeds to infrared energy so that the seed temperature reached 110-115 C for 90 seconds. Subsequently, the micronized seeds were held for 20-30 min, depending upon the seed source, in an insulated tank where temperatures ranged from 100-(residual cooking conditions). These conditions inactivated enzymes such as myrosinase in canola and trypsin inhibitors in soya as well as peroxidase and cyanogenic glucosides. Further, they ensured devitalization of viable germ tissue in hemp, improved starch digestibility, and destroyed or reduced the concentrations of heat labile antinutritional factors other than those mentioned above.

Sunflower seeds (batches 1 and 2) were not micronized before co-processing with animal offal but the batch 1 seeds were dried to ~ 10% moisture to ensure proper seed storage and facilitate dehulling. Thus, only non-micronized dehulled sunflower seeds were tested in this study.

EXAMPLE 4: Oilseed dehulling Micronized canola, soya, hemp and flax and non-micronized animal feed-grade sunflowerwere dehulled. The process involved seed sizing, impact dehulling (Forsberg model 15-D impact huller), screening and air classification (Forsberg model screener and screen-aire).

EXAMPLE 5: Oilseed cold-pressing In a preferred embodiment of the invention, the oilseeds (micronized or raw), except soya and micronized dehulled hemp were cold-pressed at a temperature not exceeding 85 C, using a Canadian designed and manufactured laboratory scale Gusta cold press (1 HP Model 11, Gusta Cold Press, St. Andrews, Manitoba, Canada). This served to remove some (dehulled seeds) or a significant proportion (undehulled seeds) of the residual oil (organic human food grade oil) and concomitantly reduced the particle size of the oilseed before itwas co-processed with minced animal offal in various proportions (improved the efficiency of the subsequent aqueous extraction of the water soluble antinutritional factors and oligosaccharides present in the oilseed).

In a more preferred embodiment, specially for soya, the particle size was further reduced, using a modified crumbler (model 706S, W.W. Grinder Corp., Wichita, Kansas). This machine was equipped afteir modification with dual motorized corrugated rolls. One of these had a fixed speed whereas the speed of the other could be varied.
For the purpose of this investigation, the variable speed roller was adjusted to rotate much faster than the fixed speed roller to achieve a shearing action.

EXAMPLE 6: Mixing or co-processing step Thawed, ground, whole animal offal (mostly herring, but in two cases.poultry offal minus feet, was used) and oilseeds that had been micronized or dried as described in Example 3 or in raw form and either cold pressed or ground as described in Example 5 were first combined in various proportions. In preferred embodiments, the usual percentages of offal to oilseed were 75:25; 50:50; or 25:75 (w/w). Thereafter, 100 mg of santoquin (antioxidant) per kg of mixture in a rnarine oil carrier (1 g/kg) were added.
Then hot water was added to the mixture in such a way that the ratio of water to oil-free dry matter present in the oilseed was maintained between 3-6:1(w/w), depending upon the source and proportion of oilseed in the mixture. Both the endogenous water originating from the offal and the exogenous water were considered when calculating the aforementioned ratios.

EXAMPLE 7: Cooking step The mixture obtained from co-processing of animal offal and oilseed (Example
6) was cooked for about 27 min at 90-93 C in the steam jacketed cooker section of a pilot-scale fish meal machine (Chemical Research Organization, Esbjerg, Denmark), that was equipped with a heated auger (it is notworthy that the cooking step could have also been performed by using a heat exchanger with a positive displacement pump or through direct steam injection coupled with processor). The cooking step was undertaken to: (1) minimize the loss of soluble protein through protein denaturation, (2) destroy or reduce the concentration of heat labile antinutritional factors present in the oilseed (especially important when processing non-micronized seeds and micronized soya), (3) liberate the bound cellular water and lipid in the offal and the oilseed, and (4) subject the oilseed to aqueous washing to facilitate removal of the water soluble antinutritional factors originating from this source.

EXAMPLE 8: Pressing step Significant but not total removal of the latter as wei( as lipid (animal-feed grade product) was accomplished by passing the cooked mixture through the fish meal machine screw press that was equipped with perforated screens and then a laboratory-scale press (Vincent model CP-4; Vincent Corp.,-Tampa Florida). Constituents in the waterfraction of the press liquids consisted of water soluble carbohydrates such as monosaccharides, disaccharides, or problem sugars like raffinose and stachyose, phenolic compounds, glucosinolates (when canola used), chlorogenic acid (when sunflower used), isoflavones and saponins (when soybeans used) as well as some soluble nitrogen, and water soluble vitamins. In preferred embodiments, the presscake in each case was dried in the steam jacketed drier portion of the above-mentioned fish meal machine at to produce dried protein and lipid-rich *products.

EXAMPLE 9: Drying step In one preferred embodiment, further drying of the protein products was necessary to reduce their moisture content. The drying was performed for about 30 min to reduce their moisture content to less than 10%. This was accomplished using a custom designed vertical stack (stainless steel mesh trays) pellet coolerthat was equipped with two electric base heaters and a top mounted variable speed fan. The temperature of the upward drawn air was maintained between 70 C and 80 C during the process.
All protein and lipid sources stemming from the above process, including the cold-pressed oils were further stabilized with santoquin (ethoxyquin). In a more preferred embodiment, specially in the case of the dried protein products, 100 mg of santoquin were added per kg of product in a marine oil carrier (1 g/kg). Then, each of the products was vacuum packaged in oxygen impermeable bags and stored at -20 C pending chemical analysis or their evaluation in a digestibility trial (see below). In another embodiment, specially in relation to the oils, 500 mg of santoquin were added per kg and then each lipid source was stored at,4-5 C in I L black plastic bottles.
EXAMPLE 10: Separation step In preferred embodiments, the press liquid was separated into water and lipid fractions using an Alpha de Laval batch dairy centrifuge (Centrifuges Unlimited Inc., Calgary, Alberta). Then, the water fraction was condensed to about one third of its original volume using a steam jacketed bowl cooker.

EXAMPLE 11: Preparation of protein concentrates 10 Protein concentrates that are mostly based on protein from canola, soya, sunflower and hemp were prepared by hexane extracting the products that originated from the co-processing of 1:1 combinations of whole herring and each of the preceding oilseeds. In this regard, 200 g of each of the four protein products were extracted four times with hexane (5:1 vlw). During each extraction,-the mixture was held for 30 min (stirred once after 15 min) before being filtered through Whatman No.1 filter paper in a Buchner funnel. Following hexane extraction, each protein product was placed on a tray that was lined with aluminum foil and then it was air-dried overnight. Then, each product was placed in the pellet cooler described in Example 9, where it was dried at about 70-80 C
for 15 min to remove any residual traces of hexane.

?0 EXAMPLE 12: In vivo protein digestibility experiments In a preferred embodiment, the in vivo availability (digestibility) of protein in some of the test protein sources that were prepared by co-processing various proportions of whole herring with canola, soya, sunflower and hemp was determined using Atlantic salmon in seawater as the test animal. Two experiments were conducted and the experimental conditions for each are provided in the table 1 below, wherein the flow rate of the oxygenated, filtered, ambient sea water was 6 - 8 Umin, feeding frequency was twice daily, ration was maximum (fish fed to satiation), and the photoperiod was natural.

Table 1.

Variable Experiment 1 Experiment 2 Fish source NorAm Aquaculture, NorAm Aquaculture, Campbell River, BC Campbell River, BC
Range in initial mean 76.6-85.8 54.2-61.6 weight (g) Number of fish per tank 15 15 Tanks per diet 3 3 Stocking density (kg/m 3) <8.6 <6.2 Water temperature ( C) 8.9-9.1 9.0-9.5 Salinity (g/L) 29-31 28-30 Dissolved oxygen (mg/L) 8.5-9.4 7.5-9.0 Fecal collection period 14 13 da s The design of the digestibility tanks and the fecal collection procedures have been described by Hajen etal. (1993a,b. Aquaculture 112: 321-348). The experimental diets consisted of 29.85% test protein product, 69.65% reference diet, and 0.5%
chromic oxide as the indigestible marker. Table 2 outlined below provides the ingredient and proximate composition of the reference diet used in the digestibility experiments.

Table 2.

Ingredients /k ; air-dry basis) LT Anchovy meal 643.2 Blood flour; spray-dried 41.0 Pregelatinized wheat starch 80.9 Raw wheat starch 26.9 Vitamin supplement 18.9 Mineral supplement 2' 18.9 Menhaden oil; stabilized 3l 122.4 Soybean lecithin 9.46 Choline chloride (60%) 4.73 Vitamin C, monophosphate (42%) 3.38 Permapell 9.46 Finnstim T"' 14.2 DL-methionine 1.51 Chromic oxide 5.00 Level of:
Dry matter 924-926 Protein 452-453 Lipid 184 Ash 118-123 "The vitamin supplement provided the following amounts/kg of diet on an air-dry basis:
vitamin A acetate, 4731 IU; cholecalciferol (D3), 2271 IU; DL-a- tocopheryl acetate (E), 284 IU; menadione, 17.0 mg; D-calcium pantothenate, 159.3 mg; pyridoxine HCI, 46.6 mg; riboflavin, 56.8 mg; niacin, 283.8 mg; folic acid, 14.2 mg; thiamine mononitrate, 53.0 mg; biotin, 1.42 mg; cyanocobalamin (B12), 0.085 mg; inositol, 378.5 mg.

' The mineral supplement provided the following (mg/kg diet on an air-dry basis):
manganese (as MnSO4 = H20), 71.0; zinc (as ZnSO4 = 7H20), 85.2; cobalt (as CoCiZ -6H20), 2.84; copper (as CuSO4 = 5H20), 6.62; iron (as FeSO4 - 7H20), 94.6;
iodine (as K103 and K1,1:1), 9.46; fluorine (as NaF), 4.73; selenium (as NaZSeO3), 0.19;
sodium (as NaCI), 1419; magnesium (as MgSO4 = 7H20), 378; potassium (as K2S04 and K2C03, 1:1), 1419.

31 Stabilized with 0.5 g santoquin/kg oil.

After adjustment of all experimental diet mashes to a moisture content of 9%, they were cold pelleted using a California model CL type 2 pellet mill. Diet particle size was adjusted to suit fish size. The reference and experimental diets that were used in the study were stored at 5 C in air-tight containers until required.

The reference and experimental diets (rriixture of reference and test diet) and lyophilized fecal samples were analyzed for levels o{ moisture, protein and chromic oxide at the DFO, West Vancouver Laboratory (WVL) using the procedures described below.
Subsequently, the digestibility coefficients for protein were determined for each diet according to Cho et al. (1985. Finfish nutrition in Asia: methodological approaches to research and development. IDRC Ottawa, Ont.,154p.). Then, the digestibility coefficients for each of the protein products themselves were calculated according to Forster (1999.
Aquaculture Nutrition 5: 143-145).

The results of chemical analyses of the protein sources used in this study and of the products derived from the co-processing of animal offals (herring or poultry offal) with canola, sunflower, soya and hemp treated as described above are presented in Tables 3-20. The results have been expressed on a dry weight basis and a lipid-free dry weight basis since the mechanical pressing of lipid from the cooked blends of offal and oilseed was variable and not complete. This is a function of the design of the presses and other conventional presses available in industry can be of higher efficiency. -Examples 13 to 16 outlined hereinafter give the results of chemical analyses performed on products obtained in accordance with the process of the invention from:
canola and canola-based products, sunflower and sunflower-based products, soya and soya-based products, as well as hemp and hemp-based products. The chemical analyses were performed according to the following methods:

Concentrations of protein, moisture, and ash in the protein sources and products that were prepared as well as in all test_ diets, and fecal samples were determined at the Department of Fisheries and Oceans, West Vancouver Laboratory (DFO-WVL) using the procedures described by Higgs et al. (1979. In J.E. Halver, and K. Tiews, eds.
Finfish Nutrition and Fishfeed Technology, Vol. 2. Heenemann Verlagsgesellschaft MbH., Berlin, pp. 191-218).

Similarly, the fatty acid compositions of the cold pressed oils and animal feed grade oils stemming from the press liquids were determined at the same laboratory using the procedures of Silver et al. (1993. In S.J. Kaushik and P. Luquet, eds. Fish nutrition in practice. IV' International Symposium on Fish Nutrition and Feeding, INRA, Paris, pp.
459-468).

Moreover, the chromic acid concentrations in diets and lyophilized fecal samples were determined at the DFO-WVL using the methods of Fenton and Fenton (1979. Can.
J.
Anim. Sci., 59: 631-634).

Concentrations of crude fibre (AOCS Official Method Ba 6-84), lipid (Troeng, S. 1955.
J.A.O.C.S. 32:124-126), chlorogenic acid (capillary electrophoresis method developed by M. Marianchuk at the POS Pilot Plant Corp.) and sinapine (capillary electrophoresis method developed by P. Kolodziejczyk et al. at the POS Pilot Plant Corp.) in the oilseeds and test protein products as well as measurements of trypsin inhibitor (AOCS
Official Method Ba 12-75 reapproved 1997) and urease (AOCS Official Method Ba reapproved 1993) activities in soya and sunflower seeds and protein products were determined at the POS Pilot Plant Corp., Saskatoon, SK. according to the methods cited in the parentheses.

peterminations of the amino acid concentrations in the oilseeds and test protein products were conducted by AAA Laboratory, Mercer Island, WA, USA using the general procedures described by Mwachireya etal. (1999. Aquaculture Nutrition 5: 73-82).

Levels of phytic acid in all oilseeds and in the products derived from the co-processing of oilseeds and animal offal were determined by Ralston Analytical Laboratories, Saint Louis, MO using the procedures described by Forster et al. (1999. Aquaculture 179:
109-125).

Mineral concentrations in the oilseeds and the protein products were determined by Norwest Labs, Surrey, BC using plasma spectroscopy (Higgs eta/., 1982.
Aquaculture 29: 1-31).

Concentrations of glucosinolate corrnpounds (total of all the different types of glucosinolates) present in canola and-canola- based products were measured by Dr.
Phil Raney, of Agriculture & Agri-Food Canada, Saskatoon, SK according to the methods of Daun and McGregor (1981. Glucosinolate Analysis of Rapeseed (Canola).
Method of the Canadian Grain Commission Revised Edn. Grain Research Laboratory, Canadian Grain Commission, Winnipeg, Manitoba, Canada).

Measurements of soy isoflavones namely, daidzein, glycitein, genistein, and saponins were conducted by Dr. Chung-Ja C. Jackson, of the Guelph Center for Functional Foods, University of Guelph Laboratory Services and have been reported here as the total for the preceding compounds (the methodology in each case is the subject of a patent application and hence has not been published).

EXAMPLE 13: Results obtained for canola and canola-based products Table 3 outlined below gives the percentages of extensively dehulled and partially dehulled Goliath canola seed and of hulls in relation to seed size after dehulling by Forsberg Incorporated, Thief River Falls, MN.

Table.3.
Seed size/fraction Weight (kg) %
Extensively 35.8 39.4 dehulled; lar e Extensively 10.8 11.8 dehulled; small "
10 Partially dehulled; 20.4 22.4 lareti Partially dehulled; 14.3 15.7 small ti Hulls; small 3.33 3.66 Hulls; large 6.49. 7.13 Total 91.1 100 The extensively dehulled canola as identified visually by the lack of hulls in the material was used in the tests reported below (referred to as dehulled canola) 20 y The partially dehulled canola could be subjected to further dehulling, directed into ruminant diets, and/or mixed at a low proportion with animal offal and then co-processed to create a nutritionally upgraded protein source for monogastrics.

3/ The hulls contained little visible evidence of canola meats and had low density.
Table 4 gives the percentages of presscake, and oil obtained after cold pressing raw, undehulled and micronized, dehulled Goliath canola seed using a laboratory scale Gusta press.

'36 Table 4.

Raw, undehulled Micronized, dehulled Fraction canola seed canola seed Presscake % 68.3 84.0 Oil (%) 31.7 16.0 Total 100 100 Table 5 sets out the initial ratios of water from endogenous and exogenous sources to oilseed lipid-free dry matter content and percentage yields (air-dry product, moisture-free product, and lipid-free dry weight product) from the co-processing of different blends of whole herring (WH) with dehulled, micronized (DC) and undehulled raw Goliath canola seed (URC).

Table 5.

Protein product " Initial ratio of hot Air-dry Moisture- Lipid-free water to oilseed product free product dry product lipid-free dry (%) (%) (%) matter (w/w) WH75DC25 5:1 29.4 27.0 19.4 WH50DC50 5:1 32.7 31.1 20.4 WH37.5DC62.5 5:1 34.8 31.8 20.0 WH75URC25 4.5:1 30.5 27.1 19.0 WH50URC50 5:1 30.9 29.8 21.3 WH25URC75 5:1 29.6 28.6 20.5 " Numbers following WH, DC, and URC refer to initial percentages of these products in the herring/canola seed blends (canola seed was cold pressed to remove a significant portion of the oil and reduce the particle size of the starting material before blending with herring and santoquin; 0.1 g/kg of mixed product before water addition) before their co-processing using cooking temperatures of 90-93 C and drying temperatures of 77-83 C.
In Table 6, the concentrations of proximate constituents including crude fibre (CF) as well as phytic acid (PA), total glucosinolates (TG), and sinapine in whole herring (WH), dehulled micronized cold pressed Goliath canola (DC), undehulled raw cold pressed Goliath canola (URC), and six protein products produced by the co-processing of different proportions of WH with either DC or URC (expressed on a dry weight basis, DWB or lipid-free dry weight basis, LFDWB) are provided. The composition of a seventh protein product that was produced by hexane extraction of WH50DC50 is also shown (WH50DC50-hexane) togetherwitli the apparent protein digestibility coefficients for some of the products (Atlantic salmon in sea water used as the test animal) is also provided.

Table 6. o Parameter WH DC URC WH75 WH50 WH50 WH37.5 WH75 WH50 WH25 DC25 DC50 DC50 DC62.5 URC25 URC5 URC75 (hexane) 0 Dry matter /k 286 954 936 918 952 928 914 890 966 968 Protein (g/kg) -DWB 488 279 348 529 456 693 416 525 414 404 Lipid /k -DWB 439 458 258 280 345 42.5 372 298 284 284 Ash /k -DWB 70.3 48 60.9 81 67.1 97.2 63 77.1 78.8 73.5 -LFDWB 125 88.6 82.1 113 102 102 100 110 110 103 CF /k -DWB -28.3 66.5 21 24.7 38.3 28.9 - 69.2 76.4 N
-LFDWB - 52.2 89.6 29.2 37.7 40 46 - 96.6 107 ~
PA (g/kg) -DWB - 28.2 33.9 15.6 22.9 - 25.5 14.2 26 30.7 -LFDWB - 52 45.6 21.6 35 - 40.6 20.2 36.3 42.9 N
TG (pmoles/g) 10.8 17.8 1.09 1.26 - 0.92 0.44 0.9 1.06 0 DWB
-LFDWB - 19.9 24 1.52 1.92 - 1.47 0.63 1.26 1.49 ~
Sina ine /k -DWB - 11.2 13.1 3.16 4.94 - 5.8 2.92 5.18 5.68 0 -LFDWB - 20.7 17.7 4.39 7.54 - 9.23 4.16 7.23 7.94 In vivo protein - - - 88.9 94.4 - 94.9 - 94.4 96.4 di estibili (%) Not determined Table 7 provides the concentrations of essential amino acids (% of protein) and selected minerals (ug/g of lipid-free dry matter) in whole herring (WH), micronized, dehulled, cold pressed Goliath canola (DC), undehulled, raw cold pressed Goliath canola (URC), and six protein products produced by the co-processing of different propotions of WH with either DC or URC. The amino acid and mineral concentrations in a seventh protein product, produced by hexane extraction of WH50DC50 are also shown (WH50DC50-hexane).

Table 7. o Parameter WH DC URC WH75 WH50 WH50 WH37.5 WH75 WH50 WH25 DC25 DC50 DC50 DC62.5 URC2 URC5 URC75 (hexane) 5 0 A) Essential amino acids Arginine 6.66 7.09 7.23 7.44 7.5 6.93 - - -Histidine 1.97 2.84 - 2.62 2.69 2.69 2.59 - - -Isoleucine 4.56 4.28 - 4.81 4.78 4.71 4.51 - - -Leucine 8.4 7.47 - 8.15 8.22 8.01 7.71 - - -Lysine 5.47 , 3.87 - 4.92 4.85 7.01 4.4 - - - o Methionine + 3.97 4.55 - 4.54 4.63 4.25 4.47 - - -Cystine Ln Phenylalanine + 7.55 7.26 - 8.08 8.14 7.93 7.54 - - - "
Tyrosine o Threonine 4.97 4.62 - 4.83 4.89 4.73 4.61 - - -T to han 1.51 1.72 - 1.69 1.63 0.92 1.69 - - - o Valine 5.51 5.34 - 5.66 5.75 5.23 5.36 - - -B) Minerals Calcium 30303 4061 5183 23905 14594 16202 12195 22088 14458 10244 Phosphorus 19073 18760 17278 23299 21971 23746 20384 21127 20675 20777 Magnesium 1961 7929 7631 4388 5934 6921 6098 4161 6289 8599 Sodium 5704 <100 <100 3026 1443 1598 1220 2081 772 495 Potassium 14260 18566 18142 12104 12348 14293~ 12544 10244 11234 12019 Copper 5.2 3.09 <1.00 15.4 6.09 12.0 8.36 11.4 10.7 9.81 Zinc 101 70.8 66.7 116 101 106 79.6 96.2 74.6 71.1 " Not determined.

Table 8 sets out the percentages of selected fatty acids and of saturated, unsaturated, (n-6), (n-3) and n-3 highly unsaturated fatf'y acids (n-3 HUFA; 20:5 (n-3) +
22:6 (n-3)) in whole herring (WH), undehulled raw cold pressed Goliath canola (URC), and the press lipids resulting from th e co-processing of different proportions of WH with DC or URC.

Table 8.

Lipid source WH URC WH75 WH50 WH37.5 WH75 WH50 WH25 Fatty acid DC25 DC50 DC62.5 URC25 URC50 URC75 18:1(n-9) 18.9 62.7 35.7 49.9 55.0 22 25.7 18:2(n-6) 0.74 21.4 7.34 15.0 17.5 -. 10.3 17 18:3(n-3) 0.12 8.79 3.28 0.34 7.40 - 2.67 4.28 20:5(n-3) 9.66 0.00 15.4 3.75 2.71 - 4.21 5.83 22:6(n-3) 8.96 0.00 7.00 4.11 1.38 - 6.69 0 Total Saturated 22.2 4.32 20.3 12.4 9.88 - 22.1 20.3 0 Total Unsaturated 77.8 95.7 79.7 87.6 90.1 - 77.9 79.7 Total (n-6) } 4.82 21.7 8.56 15.5 ' 17.9 - 14.1 20 Total (n-3) 31.3 9.96 28.0 14.7 11.8 - 21.7 15.3 0 Total n-3 N
HUFA 18.6 0 22.4 7.86 4.09 - 10.09 5.813 0 Not determined EXAMPLE 14: Results obtained for sunflower and sunflower-based products In Table 9, initial ratios of water from endogenous and exogenous sources to oilseed lipid-free dry matter and percentage yields (air-dry product, moisture-free product, and lipid-free dry weight product) from the co-processing of different blends of whole herring (WH) or poultry offal (PO) with dehulled, raw, sunflower seed, batch 1(DRSF,) or batch 2 (DRSF2) are provided.

- Table 9.

Protein product Initial ratio of hot Air-dry Moisture- Lipid-free water to oilseed product free dry product lipid-free dry matter (%) product (%) (w/w) %
WH75DRSF 25 5:1 30.4 28.2 19.7 ) WH501DRSF 50 3:1 31.6 29.0 19.4 WH25DRSF 75 3:1 31.7 31.1 19.9 P050DRSF 50 6:1 46.9 43.0 31.3 Numbers following WH, DRSF and PO refer to initial percentages of these products in the herring/sunflower seed and poultry/sunflower seed blends (sunflower seed was cold pressed to remove a significant portion of the oil and reduce the particle size of the starting material before blending with herring or poultry and santoquin; 0.1 g/kg of mixed product before water addition) before their co-processing using cooking temperatures of 90-93 C and drying temperatures of 77-83 C.

Table 10 gives the concentrations of proximate constituents including crude fibre (CF), ) phytic acid (PA), trypsin inhibitor activity (TI), urease activity (UA) and chlorogenic acid (CA) content in whole herring (WH), poultry-offal (PO), dehulled, raw cold pressed sunflower, batch 1(DRSF,), and five protein products produced by the co-processing of different proportions of WH or PO with either DRSF, or dehulled, raw cold pressed sunflower, batch 2(DRSFZ) (expressed on a dry weight basis, DWB or lipid-free dry weight basis, LFDWB). The composition of a sixth protein product that was produced by hexane extraction of WH50DRSF,50 is also shown (WH50DRSF,50-hexane) together with the apparent protein digestibility coefficients for some of the products (Atlantic salmon in sea water used as the test animal).

Table 10.

Parameter WH PO DRSF, WH75 WH50 WH50 WH25 P05b DRSF125 DRSF150 DRSF150 DRSF175 DRSF250y (hexane) Dry matter /k 286 328 938 928 919 930 981 918 Protein (g/kg ) 488 370 351 535 479 695 441 382 -DWB

Lipid g/kg -DWB 439 451 409 302 330 32.2 360 271 Ash (g/kg -DWB 70.3 104 50.7 126 118 95.8 115 58.9 -LFDWB 125 189 85.8 181 176 99 180 80.8 CF /k -DWB - '~ - 34 19.2 32.4 37.5 27.2 124 -LFDWB - - 57.5 27.5 48.4 38.8 42.5 170 4- PA /k -DWB - - 31.4 14.2 23.3 -30.7 25.9 -LFDWB - - 53.2 20.4 34.8 - 47.9 35.6 ~
TI (TIA units/g) - - - 1603 1766 1730 - 1268 0 LFDWB
UA A H - - 0.06 0.03 0.02 - 0.01 CA /k -DWB - - 14.9 2.6 5.65 - 8.58 6.22 -LFDWB - - 27.7 3.72 8.43 13.4 8.53 In vivo protein digestibility - - - 97.6 - 97.1 -(%) '/ Not determined ti DRSF2 co-processed with PO was pressed, partially dehulled (58%) animal feed grade with a DM, protein, lipid, ash and crude fibre content (g/kg expressed on a dry weight basis except DM) of 918, 379, 211, 59.4, and 123, respectively.

Table 11 gives the concentrations of essential amino acids (% of protein) and selected minerals (pg/g of lipid-free dry matter) in whole herring (WH), poultry offal (PO), dehulled, raw, cold pressed sunflower, batch 1(DRSF,), and four protein products produced by the co-processing of different proportions of WH or PO with either DRSF, or DRSF2. The concentrations in a fifth protein product, produced by hexane extraction of WH50DRSF,50, is also shown (WH50DRSF,50-hexane).

Table 11 Parameter WH PO DRSF12J WH75 WH50 WH50 WH25 P050 (hexane) A) Essential amino acids Arginine 6.66 8.11 10.6 7.66 8.58 8.64 9.16 8.52 Histidine 1.97 1.91 2.59 2.34 2.42 2.40 2.41 2.56 Isoleucine 4.56 3.19 4.45 4.28 4.45 4.52 4.38 4.56 Leucine 8.40 5.88 6.32 7.16 6.96 7.11 6.57 6.95 Lysine 5.47 5.28 3.67 6.88 5.57 5.57 4.30 4.59 Methionine + Cystine 3.97 3.16 3.61 3.71 3.41 3.61 3.42 3.25 Phenylalanine + 0 Tyrosine 7.55* 5.45 7.66 7.46 7.65 7.82 7.55 7.72 0 CD
Threonine 4.97 3.67 4.15 4.40> 4.17 4.10 4.06 ~ 3.99 61 T to han . 1.51 0.75 1.28 1.27 0.78 1.27 1.03 1.40 Valine 5.51 4.03 5.19 5.09 - 5.29 4.86 5.08 4.81 N
~
B) Minerals Calcium 30303 -' 1930 33810 15055 14999 10226 12420 Phosphorus 19073 - 22188 29950 25011 23221 23573 15843 Magnesium 1961 - 10805 4493 7503 7544 9987 4992 Sodium 5704 - 19.8 2223 1454 1378 836 852 Potassium 14260 - 23090 11085 14406 15110 15036 9894 Copper 5.20 - 39.1 21.6 36.5 28.9 37.0 39.9 Zinc 101 - 124 99.0 118 124 123 - 93.0 "Not determined.
ti Values for essential amino acids were derived from unpressed DRSF,.
31 DRSF2 co-processed with PO was partially dehulled (58%) animal feed grade with a DM, protein, lipid, ash and crude fibre composition (g/kg expressed on a dry weight basis except DM) of 918, 379, 211, 59.4, and 123, respectively.

In Table 12, percentages of selected fatty acids and of saturated, unsaturated, (n-6), (n-3) and n-3 highly unsaturated fatty acids (n-3 HUFA; 20:5 (n-3) + 22:6 (n-3)) in whole herring (WH), poultry offal (PO), dehulled, raw, cold pressed sunflower, batch 1(DRSFA
and the press lipids resulting from the co-processing of different proportions of WH or PO with DRSF, or dehulled, raw, cold pressed sunflower, batch 2(DRSF2).

Table 12 0 Lipid source Fatty acid WH PO DRSF, WH75 WH50 WH25 P050 DRSF 25 DRSF 50 DRSF 75 DRSF 50v 18:1(n-9) 18.9 39.9 9.39 21.6 18.2 " 17.9 18:2(n-6) 0.74 17.6 76.6 22.4 25.3 - 38.7 18:3(n-3) 0.12 2.56 0.11 4.28 0.42 - 0.80 20:5(n-3) 9.66 0.00 0.00 3.15 3.67 - 0.00 22:6(n-3) 8.96 0.00 0.00 6.04 7.87 - 0.00 Total Saturated 22.2 33.9 12.1 16.9 14.5 - 37.7 0 Total -Unsaturated 77.8 66.17 87.9 83.1 85.5 62.3 o Total (n-6) 4.82 17.8 76.6 29.5 36.3 - 38.7 Total (n-3) 31.3 2.56 0.12 19.2 17.7. - Ø80 0 Total n-3 H U FA 18.6 0.00 0.00 9.19 11.5 - 0.00 0 "Not determined.

ti DRSFZ co-processed with PO was partially dehulled (58%) animal feed grade with a DM, crude protein,lipid; ash and crude fibre content (g/kg expressed on a dry weight basis except DM) of 918, 379, 211, 59.4, and 'f 23, respectively.

EXAMPLE 15: Results obtained for soya and soya-based products In Table 13, the initial ratios of water from endogenous and exogenous sources to oilseed, lipid-free dry matter and percentage yields (air-dry product, moisture-free product, and lipid-free dry weight product) from the co-processing of different blends of whole herring (WH) with dehulled, micronized (DSY) and undehulled raw soya seed (URSY).

Table 13.

Protein productInitial ratio of hot Air-dry Moisture- Lipid-free water to oilseed product free product dry product lipid-free dry (%) (%) (%) matter (w/w) WH75DSY25 5:1 14.2 13.6 10.3 0 WH50DSY50 5:1 36.7 34.9 26.4 WH25DSY75 4:1 48.3 43.8 32.7 WH75URSY25 5:1 20.7 19.1 15.0 WH50URSY50 5:1 29.9 27.4 21.1 WH25URSY75 4:1 43.8 38.4 33.7 Numbers following WH, DSY and URSY refer to initial percentages of these products in the herring/soya blends (soya seed was ground to reduce the particle size of the starting material before blending with herring and santoquin; 0.1 g/kg of mixed product before water addition) prior to their co-processing using cooking temperatures of 90-93 C and drying temperatures of 77-83 C.

:0 Table 14 shows the concentrations of proximate constituents including crude fibre (CF) as well as phytic acid (PA), total saponins, total isoflavones (TIF), urease activity (UA), and trypsin inhibitor activity (TI) in whole herring (WH), dehulled, micronized, , soya (DSY), undehulled, raw soya (URSY), and six protein products produced by the co-processing of different proportions of WH with either DSY or URSY (expressed on a dry weight basis, DWB or lipid-free dry weight basis, LFDWB). The composition of a seventh protein product that was produced by hexAne extraction of WH50DSY50 is also shown (WH50DSY50-hexane) together with the apparent protein digestibility coefficients for some of the products (Atlantic salmon in sea water used as the test animal).

Table 14 0 Parameter WH DSY URSY WH75 WH50 WH50 WH25 WH75 WH50 WH25 (hexane) 0 Dry matter /k 286 921 897 956 950 936 907 921 916 878 Protein (g/kg ) - 488 396 334 526 531 647 507 497 429 388 DWB

Lipid (g/kg ) - 439 242 230 244 '242 30.1 254 215 230 232 DWB
Ash (g/kg ) - 70.3 50.3 57.1 77.2 59.4 71.2 52.2 85.8 66.4 56.8 DWB N
-LFDWB 125 66.4 74.2 102 78.4 73.4 70.0 109 86.2 74.0 0 CF (g/kg) -16.2 44.6 16.0 1643 18.7 19.3 46.6 67.5 82.2 ~
DWB
N
-LFDWB - 21.3 57.9 21.2 21.5 19.3 25.9 59.3 87.6 107 0 PA (g/kg ) - - 14.9 20.0 9.87 11.9 - 12.9 12.5 15.9 17.2 DWB
-LFDWB - 19.6 25.9 13.1 15.7 - 17.3 15.9 20.7 22.4 0 Saponins (mg/g ) - 1.60 - 0.71 1.02 - 1.18 - - --DWB
-LFDWB - 2.11 - 0.94 1.35 - 1.58 - - -TIF( g/g ) - - 2305 - 899 1402 - 1622 - - -DWB

UA(ApH) - 0.01 2.48 0.02 0.01 - 0.02 0.09 0.28 0.35 TI (TIA units/g) - - 7813 101563 871 1017 - 553 1902 8296 11138 LFDWB
In vivo protein - - - - 96.2 - 94.2 - 93.5 88.2 di estibili (%) Not determined Table 15 provides concentrations of essential amino acids (% of protein) and selected minerals (pg/g of lipid-free dry matter) in whole herring (WH), dehulled, micronized, soya (DSY), and three protein products produced by the co-processing of different proportions of WH with DSY. The concentrations in a fourth protein product, produced by hexane extraction of WH50DSY50, is also shown (WH50DSY50-hexane).

Table 15 0 ~
Parameter WH DSY WH75 WH50 WH50 WH25 hexane A) Essential amino acids Arginine 6.66 7.57 7.39 7.17 7.64 7.38 Histidine 1.97 2.48 2,45 2.42 2.49 2.47 Isoleucine 4.56 4.65 4.67 4.60 4.83 4.57 Leucine 8.40 7.53 7.66 7.48 8.00 7.58 Lysine 5.47 6.14 7.13 6.70 6.72 6.52 N
Methionine + Cystine 3.97 2.46 3.30 2.70 3.20 2.97 U, Phenylalanine +
Tyrosine 7.55 8.56 8.21 8.27 8.78 8.47 N
Threonine 4.97 4.21 4.57 4.37 4.44 4.30 N
T to han 1.51 1.45 1.38 1.31 1.20 1.35 Valine 5.51 4.54 5.26 5.04 4.79 4.99 0 B) Minerals Calcium 30303 2637 22138 14304 9958 8646 Phosphorus 19073 9339 19648 14998 11897 12385 Magnesium 1961 3638 2684 2597 2324 2971 Sodium 5704 <5.00 2228 1290 1157 668 Potassium 14260 27646 17157 16942 13769 17587 Copper 5.20 21.6 36.7 .26.7 23.6 27.2 Zinc 101 57.3 75.3 65.5 65.6 67.8 Table 16 provides the percentages of selected fatty acids and of saturated, unsaturated, (n-6), (n-3) and n-3 highly unsaturated fatty acids (n-3 HUFA; 20:5 (n-3) +
22:6 (n-3)) in whole herring (WH), micronized, dehulled, soya (DSY), undehulled, raw soya (URSY), and the press Iipids resulting from the co-processing of different proportions of WH with DSY or URSY.

Table 16. o Lipid source Fatty acid WH DSY URSY WH75 WH50 WH25 WH75 WH50 WH25 18:1(n-9) 18.9 17.8 17.4 17.9 18.86 15.8 18.4 14.5 13.1 18:2(n-6) 0.74 57.5 57.2 6.39 10.1 22.8 8.24 13.0 25.2 18:3(n-3) 0.12 9.79 10.2 2.67 2.19 4.38 2.99 2.79 4.60 20:5(n-3) 9.66 0.00 0.00 11.2 6.92 5.58 10.4 7.85 5.17 22:6(n-3) 8.96 0.00 0.00 8.55 8.11 6.77 9.10 8.33 6.29 N
Total Ln Saturated 22.2 13.4 13.3 22.1 25.7 22.8 21.0 26.4 26.8 Total Unsaturated 77.8 86.6 86.7 77.9 74.3 77.2 79.0 73.6 73.2 0 Total (n-6) 4.82 57.9 57.8 9.26 10.1 22.8 8.24 13.0 25.2 Total (n-3) 31.3 10.0 10.4 29.3 25.6 24.5 32.7 27.5 22.1 Total n-3 HUFA 18.6 0.00 0.00 19.7 15.0 12.3 19.5 16.2 11.5 Example 16: Results obtained for hemp and hemp-based products.
In Table .17, the initial ratios of water from endogenous and exogenous sources to oilseed lipid-free dry matter and percentage yields (air-dry product, moisture-free product, and lipid-free dry weight product) from the co-processing of different blends of whole herring (WH) with dehulled, sterilized (DHP) and undehulled sterilized hemp seed (UHP).
Table 17.

Protein product 11 Initial ratio of hot Air-dry Moisture- Lipid-free dry water to oilseed lipid- product free product product (%) free dry matter (wlw) (%) %
WH75DHP25 5:1 3.04 2.93 2.80 WH50DHP50 4:1 20.4 19.9 ,.15.1 WH25DHP75 3:1 37.3 32.6 23.2 WH75UHP25 5:1 15.0 14.7 11.9 WH50UHP50 5:1 36.9 36.4 31.4 WH25UHP75 4:1 40.3 39.7 34.2 "Numbers following WH, DHP and UHP refer to initial percentages of these products in the herring/hemp blends (UHP seed was cold pressed to remove a significant portion of the oil and to reduce the particle size of the starting material before blending with herring and santoquin; 0.1 g/kg of mixed product before water addition) prior to their co-processing using cooking temperatures of 90-93 C and drying temperatures of 77-83 C.

Table 18 gives the concentrations of proximate constituents including crude fibre (CF) as well as phytic acid (PA) in whole herring (WH), dehulled, sterilized hemp (DHP), cold pressed undehulled, sterilized hemp (UHP), and six protein products produced by the co-processing of different proportions of WH with either DHP or UHP (expressed on a dry weight basis, DWB or lipid-free .dry weight basis, LFDWB). The composition of a seventh protein productthatwas produced by hexane extraction of WH50DHP50 is also shown (WH50DHP50-hexane) togetherwith the apparent protein digestibility coefficients for some of the products (Atlantic salmon in sea water used as the test animal).

Table 18.
Parameter WH DHP UHP WH75 WH50 WH50 WH25 WH75 WH50 WH25 DHP25 DHP50 DHP50 DHP75 UHP25. UHP50 UHP75 (hexane) Dry matter /k 286 963 952 976 975 969 874 983 986 986 Protein (g/kg ) 488 313 311 579 575 721 533 504 429 448 -DWB

Lipid (g/kg) - 439 505 221 243 240 33.4 289 193 138 138 DWB
Ash /k -DWB 70.3 59.2 63.6 99.2 88.7 118 87.6 77.4 116 117 -LFDWB 125 120 81.6 131 117 122 123 95.9 135 136 CF /k -DWB -44.1 251 14.7 39.1 51.9 52.5 153 237 239 Ul -LFDWB - 89.2 322 19.4 51.4 53.7 73.9 , 189 275 277 Ln PA (g/kg) -DWB - 37.5 33.7 12.5 35.2 - 47.7 15.3 25.3 24.6 -LFDWB - 75.7 43.3 16.5 46.3 - 67.1 18.9 29.3 28.6 N
In vivo protein digestibility - - - - 96.1 - 99.9 - - -o/a Not determined ,57 Table 19 shows the concentrations of essential amino acids (% of protein) and selected minerals ( g/g of lipid-free dry matter) in whole herring (WH), dehulled, sterilized hemp (DHP), and three protein products produced bythe co-processing of different proportions of WH with DHP. or UHP. The concentrations in a fourth protein product, produced by hexane extraction of WH50DHP50, are also shown (WH50DHP50-hexane).

Table 19 Parameter WH DHP WH75 WH50 WH50 WH25 (hexane) A) Essential amino acids Arginine 6.66 14.0 8.48 10.4 10.6 11.7 Histidine 1.97 2.81 2.53 2.58 2.62 2.71 Isoleucine 4.56 4.24 4.97 4.72 4.79 4.54 Leucine 8.40 6.72 8.32 7.70 7.90 7.31 Lysine 5.47 3.81 7.93 6.45 6.39 5.35 Methionine,+ Cystine 3.97 4.11 4.11 4.08 4.02 3.91 10 Phenylalanine + ~

Tyrosine 7.55 8.41 8.62 8.48 8.68 8.52 Ln Threonine 4.97 3.71 4.80 4.37 4.36 4.06 0 T to han 1.51 0.40 0.41 0.75 1.39 0.75 N
Valine 5.51 4.97 5.58 5.37 5.19 5.20 B) Minerals Calcium 30303 1792 35867 16734 17616 7789 Phosphorus 19073 31048 29641 28340 27652 31219 Magnesium 1961 14202 3668 8772 8531 1-2375 Sodium 5704 37.8 2558 1646 1708 1162 20 Potassium 14260 18880 10882 11876 13559 14419 Copper 5.20 30.8 18.7 22.5 26.5 25.4 Zinc 101 169 101 125 141 154 Table 20 sets out the percentages of selected fatty acids and of saturated, unsaturated, (n-6), (n-3) and n-3 highly unsaturated fatty acids (n-3 HUFA; 20:5 (n-3) +
22:6 (n-3)) in whole herring (WH), dehulled, sterilized hemp (DHP), undehulled, sterilized hemp (UHP), and the press lipids resulting from the co-processing of different proportions of WH with DHP or UHP.

Table 20 Lipid source Fatty acid DHP25 DHP50 DHP75 UHP25 UHP50 UHP75 18:1(n-9) 18.9 5.48 7.72 8.30 8.63 6.51 15.5 17.1 14.2 18:2(n-6) 0.74 57.7 56.4 30.9 42.7 49.8 18.7 18.9 33.6 18:3(n-3) 0.12 19.8 19.0 10.9 15.0 16.8 7.12 7.32 11.5 20:5(n-3) 9.66 0.16 0.02 4.30 2.72 1.55 4.63 3.46 0.05 22:6(n-3) 8.96 0.00 0.00 3.94 2.68 1.91 7.05 5.94 3.00 N

Total CD
Saturated 22.2 12.5 10.0 24.0 16.4 14.6 20.8 21.4 16.7 y =4 Total Unsaturated 77:8 87.5 90.0 76.0 83.6 85.4 79.2 78.6 83.3 N
Total (n-6) 4.82 57.7 60.6 31.6 42.8 49.9 21.8 20.9 36.5 Total (n-3) 31.3 20.3 19.1 23.4 24.2 22.1 25.9 22.6 18.3 0 Total n-3 HUFA
18.6 0.16 0.02 8.25 5.39 3.46 11.7 9.40 3.05 i61 The co-processing of animal offal with the foregoing oilseeds pretreated using the methods according to the present invention resulted in nutritionally upgraded protein sources suitable for use.

The yields of these protein sources were good for all canola and sunflower-based products and this was also true for the soya and hemp-based products when higher concentrations (> 50% in initial mixture) of these treated oilseeds were used.
All of the yields were likely underestimated of true values owing to the difficulty in quantitatively collecting all of the material from the drier portion of the fish meal machine.

The oilseed-based protein products contained high concentrations of prbtein that was highly bioavailable to salmon (generally 89% to 100% of the protein was noted to be digestible in Atlantic salmon held- in s@a water depending upon the source and percentage of the oilseed in the initial mixture of offal and oilseed and the pretreatment of the latter and the offal before their co-processing). Moreover, these protein products had significantly reduced concentrations of all heat labile and water soluble antinutritional factors except phytic acid relative to their respective initial levels in the oilseeds. Phytic acid was concentrated during the co-processing of offal with oi(seed and the extent depended upon its initiaf concentration in the oilseed used in the process.
The fatty acid compositions of the animal feed grade lipid sources produced by the process largely reflected the fatty acid compositions and lipid levels contributed by the different proportions of the animal offal and oilseed used initially in the process. This provides considerable scope to produce specially designed lipid sources that are tailored to meet the fatty acid needs of various animal species.

The cold-pressing of oilseeds before they are blended with animal offal yielded high quality economically valuable human food grade oils whose fatty acid compositions can be varied, depending upon market requirements and the selection of the oilseed or combination of oilseeds that are used in cold pressing. The high value of the cold pressed oils which can be generated in greater quantities wen undehulled seeds rather than dehulled seeds are cold pressed will contribute to the overall economic viability of the co-processing of animal offais with oilseeds.

The hulls resulted from the dehulling of the oilseeds used in this study and the condensed solubles produced by co-processing animal offal(s) with oilseed(s) likely will be excellent organic fertilizer constituents. This is because they collectively contain soluble protein, some lipid and minerals and other components that can be degraded by aerobic or anaerobic bacterial processes into value-added fertilizer products making the overall process described herein economically viable.

The rapid heat treatment of oilseeds to inactivate enzymes like the protease inhibitors in soya and destruct heat labile antinutritional components coupled with the dehulling of oilseeds yield protein and lipid-rich products that potential can be used directly in high energy feeds such as those destined for aquatic species like salmon (salmon grower diets frequently contain 25-35% lipid on an air-dry basis and they are produced by extrusion processing technology).

Claims (44)

WE CLAIM:
1. A process for preparation of nutritionally upgraded oilseed meals, which are protein and lipid-rich and have a reduced fibre content and thermal labile active anti-nutritional content, comprising the steps of:
- providing a source of an oilseed, - subjecting said oilseed to a non-aqueous heat treatment at a temperature sufficient to reduce the concentration of at least some antinutritional components normally present in said oilseed to obtain a heat-treated seed;
- dehulling said heat-treated seed under non-aqueous conditions to produce a meat fraction, a hull fraction or a mixture thereof; and - cold pressing said meat fraction or said mixture to yield said protein and lipid-rich meals with reduced hull content.
2. The process according to claim 1, wherein the product obtained is a protein product having greater than 40% protein on a moisture lipid-free basis.
3. The process according to claim 1 or 2, further including the step of stabilizing said plant oils by adding an antioxidant.
4. The process according to claim 1, 2 or 3, wherein said heat treatment is a rapid heat treatment.
5. The process according to any one of claims 1 to 4, wherein said oilseed is selected from the group consisting of canola.TM., rape seed, soybeans, sunflower seed, flax seed, mustard seed, cotton seed, hemp seed and mixtures thereof.
6. The process according to any one of claims 1 to 5, wherein said oilseed is selected from the group consisting of canola.TM., rape seed, sunflower seed, flax seed, mustard seed, cotton seed and mixtures thereof.
7. The process according to any one of claims 1 to 6, wherein said dehulling is carried out by a mechanical treatment with at least one of a gravity screening and an air-classification step.
8. The process according to any one of claims 1 to 7, wherein said process further includes a seed sizing step before subjecting said oilseed source to said treatment.
9. The process according to any one of claims 1 to 8, further including the step of adding said antioxidant, wherein said antioxidant is selected from the group consisting of ethoxyquin (santoquin.TM.), butylated hydroxyanisole, butylated hydroxytoluene, tertiary butyl hydroquinone, natural antioxidants and mixtures thereof.
10. The process according to any one of claims 1 to 9, wherein said cold pressing step is carried out at a temperature not exceeding 85°C.
11. An edible human food grade oil comprising an oilseed oil, said human food grade oil having been obtained by cold pressing oilseed in which the cold pressing was carried out at temperatures below 85°C, said oil having minimal lipid oxidation products and a peroxide value of less than about 2 milliequivalents per kg.
12. The human food grade oil according to claim 11, wherein said oilseed is heat-treated.
13. The human food grade oil according to claim 11 or 12, wherein said oilseed is selected from canola.TM., rape seed, sunflower seed, flax seed, mustard seed, cotton seed, hemp seed and mixtures thereof.
14. A composition of matter for an organic fertilizer comprising the product obtained by co-processing of animal offal with pretreated oilseeds or hulls wherein the pretreated oilseed is at least one of canola.TM., sunflower, soybean, mustard seed and cotton seed and hemp seed wherein the composition of matter is comprised of dried hulls and contain protein and lipid mixed with a condensed soluble fraction derived from said co-processing of animal offal with pretreated oilseeds.
15. The composition of matter for an organic fertilizer according to claim 14, wherein said hulls are heat-treated hulls.
16. A protein and lipid-rich oilseed meal suitable for use in fish and non-human animal diets comprising a heat-treated at least partially dehulled oilseed, said oilseed being substantially free of flaxseed, mustard seed, rapeseed and cotton seed, said meal having - from about 26% to about 40% protein on a dry weight basis, - from about 48% to about 64% protein on a lipid-free dry weight basis, - from about 24% to about 46% methionine and cystine calculated as a percent of said protein, - from about 36% to about 61% lysine calculated as a percent of said protein, - from about 21 % to about 52% lipid on a dry weight basis, - from about 2% to about 12% crude fibre on a lipid-free dry weight basis, - from about 0.16% to about 0.45% calcium on a lipid-free dry weight basis, and - less than about 0.01 % sodium on a lipid-free dry weight basis.
17. The meal according to claim 16, further comprising at least one of trypsin inhibitor, glucosinolates, sinapine, chlorogenic acid and mixtures thereof.
18. The meal according to claim 16, wherein said trypsin inhibitor is in an amount of up to about 8000 units/g on a lipid-free dry weight basis
19. The meal according to claim 17, wherein said glucosinolates are in an amount of up to about 20 µmoles/g of total glucosinolates on a lipid-free dry weight basis.
20. The meal according to claim 17, wherein said sinapine is in an amount of up to about 21% on a lipid-free dry weight basis.
21. The meal according to claim 17, wherein said chlorogenic acid is in an amount of up to about 3% on a lipid-free dry weight basis.
22. The meal according to any one of claims 16 to 21, wherein said dehulled oilseed is greater than about 55% dehulled.
23. An edible human food grade oil comprised of cold pressed heat-treated oilseed, said oil being substantially free of flaxseed oil, mustard seed oil, rapeseed oil and cotton seed oil, said human food grade oil comprising - from about 86% to about 96% of total fatty acids as unsaturated fatty acids, - from about 20% to about 80% of total fatty acids as (n-6) fatty acids;
and, - a peroxide value of less than about 2 milliequivalents of peroxide per kg oil at the time of production.
24. The human food grade oil according to claim 23, further comprising up to about 22% of total fatty acids as (n-3) fatty acids.
25. The human food grade oil according to claim 23 or 24, wherein said oilseed is greater than about 55% dehulled.
26. The human food grade oil according to claim 23, wherein said oilseed is undehulled.
27. The human food grade oil according to claim 23, wherein said oilseed is a raw oilseed.
28. In a process for producing a phytate or phytic acid-reduced protein product from a protein and lipid rich oil seed source having water soluble antinutritional factors wherein the process includes the steps of providing a source of dehulled oilseed and mixing the oil seed with an acidified aqueous solution consisting essentially of water to extract protein therefrom, the improvement wherein the oil seed has a high oil content greater than 18%
and is dehulled, and in which the dehulled oilseed is treated with at least one enzyme in said acidified aqueous solution to provide a dephosphorolated or phytic acid reduced oil seed.
29. The process as defined in claim 28, wherein said enzyme is phytase.
30. The process as defined in claim 28 or 29, wherein the product is a phytic acid reduced oilseed protein product.
31. The process as defined in claim 28 or 29, wherein the product is a protein product having greater than 40% protein on a moisture lipid-free basis.
32. The process as defined in any one of claims 28 to 31, wherein the oil seed comprises an at least partially defatted oil seed.
33. The process as defined in any one of claims 28 to 32 which comprises the further step of heating the mixture containing the oil seed and the enzyme.
34. The process as defined in claim 33, wherein the mixture is incubated for at least thirty minutes and up to two hundred and forty minutes.
35. The process as defined in any one of claims 28 to 34, wherein the oil seed is an oil seed selected from canola.TM. seed, rape seed, sunflower seed, flax seed, cotton seed, hemp seed and mixtures thereof.
36. The process as defined in claim 35, wherein the oil seed is rape seed or canola.TM. seed.
37. The process as defined in any one of claims 28 to 36, wherein the aqueous solution is at a temperature from about 37°C to 55°C.
38. The process as defined in any one of claims 28 to 37, which comprises a first step of separating the mixture into a liquid phase and a solid phase.
39. The process as defined in any one of claims 28 to 38, wherein the moisture content of the mixture containing the oil seed is at least 80%.
40. The process as defined in any one of claims 28 to 39, wherein the pH of the solution is below about 60.
41. As a new composition of matter, a protein product having reduced amounts of water soluble components comprising at least a partially defatted oil seed and having a reduced phytate content.
42. The composition as defined in claim 41, wherein the oil seed is an oil seed selected from canola.TM. seed, rape seed, sunflower seed, flax seed and cotton seed and hemp seed.
43. The composition as defined in claim 41, wherein the oil seed is rape seed or canola.TM. seed.
44. A process according to claim 1 or 28, said process comprising the further steps of:
- providing a source of an unhydrolyzed animal offal, - blending said protein and lipid-rich meal with said unhydrolzyed animal offal to form a blended mixture thereof, - cooking said blended mixture under conditions selected to improve protein digestibility, and free cellular water present in said unhydrolyzed animal offal, as well as to facilitate separation of a protein from a lipid to obtain a cooked - separating said cooked mixture into a stickwater fraction, a moisture containing protein-rich fraction, and an animal feed grade oil fraction.
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PCT/CA2001/000663 WO2001084949A2 (en) 2000-05-09 2001-05-08 Protein and lipid sources for use in aquafeeds and animal feeds and a process for their preparation
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