CA1087451A - Process for the treatment of comminuted oats - Google Patents
Process for the treatment of comminuted oatsInfo
- Publication number
- CA1087451A CA1087451A CA254,864A CA254864A CA1087451A CA 1087451 A CA1087451 A CA 1087451A CA 254864 A CA254864 A CA 254864A CA 1087451 A CA1087451 A CA 1087451A
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- CA
- Canada
- Prior art keywords
- gum
- bran
- oats
- flour
- solvent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
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- A—HUMAN NECESSITIES
- A21—BAKING; EDIBLE DOUGHS
- A21D—TREATMENT, e.g. PRESERVATION, OF FLOUR OR DOUGH, e.g. BY ADDITION OF MATERIALS; BAKING; BAKERY PRODUCTS; PRESERVATION THEREOF
- A21D2/00—Treatment of flour or dough by adding materials thereto before or during baking
- A21D2/08—Treatment of flour or dough by adding materials thereto before or during baking by adding organic substances
- A21D2/36—Vegetable material
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23J—PROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
- A23J1/00—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites
- A23J1/12—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites from cereals, wheat, bran, or molasses
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K10/00—Animal feeding-stuffs
- A23K10/30—Animal feeding-stuffs from material of plant origin, e.g. roots, seeds or hay; from material of fungal origin, e.g. mushrooms
- A23K10/37—Animal feeding-stuffs from material of plant origin, e.g. roots, seeds or hay; from material of fungal origin, e.g. mushrooms from waste material
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L7/00—Cereal-derived products; Malt products; Preparation or treatment thereof
- A23L7/10—Cereal-derived products
- A23L7/198—Dry unshaped finely divided cereal products, not provided for in groups A23L7/117 - A23L7/196 and A23L29/00, e.g. meal, flour, powder, dried cereal creams or extracts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
- Y02P60/80—Food processing, e.g. use of renewable energies or variable speed drives in handling, conveying or stacking
- Y02P60/87—Re-use of by-products of food processing for fodder production
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Polymers & Plastics (AREA)
- Food Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Wood Science & Technology (AREA)
- Physiology (AREA)
- Nutrition Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Molecular Biology (AREA)
- Mycology (AREA)
- Organic Chemistry (AREA)
- Animal Husbandry (AREA)
- Zoology (AREA)
- Biochemistry (AREA)
- Cereal-Derived Products (AREA)
- Fats And Perfumes (AREA)
- Peptides Or Proteins (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
Abstract of the Disclosure A process for the separation of substantially gum-free flour from oats is disclosed. The process comprises admixing comminuted oats with a solvent for oil in the oats and separating substantially gum-free flour from the admixture.
In an embodiment the admixture of oats and solvent is separated into two fractions, one being substantially gum-free flour and the other being a bran fraction. Gum is extractable from the bran fraction. Oat oil is recoverable from the solvent.
The separation of fractions of varying protein content, in-cluding acid-soluble protein, is also disclosed. Examples of suitable solvents are pentane, hexane, heptane, cyclohexane and alcohol of 1-4 carbon atoms. The products have a variety of uses in the food industry.
In an embodiment the admixture of oats and solvent is separated into two fractions, one being substantially gum-free flour and the other being a bran fraction. Gum is extractable from the bran fraction. Oat oil is recoverable from the solvent.
The separation of fractions of varying protein content, in-cluding acid-soluble protein, is also disclosed. Examples of suitable solvents are pentane, hexane, heptane, cyclohexane and alcohol of 1-4 carbon atoms. The products have a variety of uses in the food industry.
Description
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The present invention rela~es to a process for the treatment of comminuted oa-ts so as to effect the separation of ~he comminuted oats into frac~ions of di~fering composition. In particular, the present invention relates to the treatment of comminuted oa~s so as to separate the comminuted oats into a so-called "flour" fraction, a so~called "bran" fraction and an oil, and into products derived therefrom, in which the flour is substantially free of gum.
As used herein the expression "groat" refers to the kernel oE the oat, the expression "flour" refers to the endosperm of the oat and the expression "bran" refers to the bran of the oat, such bran may have endosperm attached thereto as is exempli-fied hereinafter. The expression "gum" refers in particular to water-soluble gum.
Oats are a potential source of a wide variety of useful product~. Examples o~ such products are flour, starch, protein isolate, protein-rich flour, bran, gum and oil. Traditional techniques used in the cereal grain processing industry are ~re-quently difficult to use with oats. For example, milling tech-niques are difficult to use with oats because of process problemsrelating to the presence of oil in the oats. Moreover, unless ~he oats are de-oiled prior to milling, such milling techniques would result in the formation of flours and brans containing oil which may result in rancidity problems on storage of the flour and bran.
Gum, together with some pro~ein and starch, may be removed in part by treatment of oats with water, the resultant dilute aqueous solution of gum, then requiring treatment prior to ; disposal or or recovery of the gum. Protein may be extracted from comminuted oats with aqueous solutions, especially alkaline solutions. However any gum present in the oats may also be ' "
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extracted into solution and the resultant solutions may be viscous and cause process problems, especially in the separation of solids from the aquoeus solutions.
The composition and properties of water-soluble gums obtained from cereal grains are discussed by B. L. D'Appolonia in a paper presented at the symposium on "Industrial Uses of Cereals" held in conjunction with the 58th Annual Meeting of the Rmerican Association of Cereal Chemists, ~ovember 1973.
A process for the separation o~ acid-soluble protein from comminuted oats, and techniques for the recovery of starch, gum, and the like in related processes, is described in Canadian Application No. 245,163 of of A. Bell, J. R. B. Boocock and R. W. Oughton, filed February 4, 1976. Techniques for the separ-ation of oil from comminuted oats are known such techniques are discussed in the aforementioned application of A. Bell et al. A
process for isolating protein from a pulverized oil seed using liquid fluorocarbons is disclosed in U. ~. Patent 3,869,438 of J. W. Finley et al, which issued March 4, 1975.
Processes for the solvent-extractive milling of maize or corn, wheat, rye and the sorghum grains to remove the bran coat from whole ~ernels of such grains ~ollowed by comminution of ; the whole milled kernels and for separation of fibrous, protein-aceous, endosperm and/or starch fractions derived from such grains are disclosed by T. B. Wayne in Canadian Patents ~364,538, which issued February 23, 1971, and 905,909 and 905,910, both of which issued July 25, 1972.
A need exists ~or the discovery of a process ~or the treatment of comminuted oats, especially for the production of flour and/or protein, that is less susceptible to process problems relating to the presence of oil and gum in the oats.
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A process for the separation of a flour ~raction a bran fraction and oil from comminuted oats -7n ~rhic~ gum does not cause signi~icant process problems and in which the ~lour is essentially ~ree o~ gum has now been found.
Accordingly, the present invention provides a process ~or the separation o~ a substantially gum~free flour from oats, said process comprising:
(a) adm~xing comminuted oats with an organic solvent, said solvent being capable of extracting oat oil from said oats, and (b) separating substantially gum-free flour ~rom the a~xture of comminuted oats and solvent, the amount o~ -~lour separated from the admixture being at least 20~ by weight of the comminuted oats.
In a prePerred embodiment of the process of the present invention the oats are comminuted dehulled oats.
In another embodiment ~he comminu~ed oats and solvent are admixed under controlled conditions, said controlled conditions being adapted to cause non-uni~orm distribution o~
the com~inuted oats in the solvent.
In ye~ another embod-7ment o~ the controlled conditions ~nclude the cessation o~ mixing immediately prior to separating the first ~raction from the second ~raction~
In a further embodiment the solvent and co~minuted oats are miLxed continuously and under the controllea conditions.
In a still further embodiment solvent is continuously added to ~he comminu~ed oats and the gum-~ree flour is con-tinuously separated ~rom the admixture o~ comm-7nuted oats and solvent.
The comminuted oats used in the process o~ the pre-sent invention are preferably dehulled oats~ Techniques ~or dehulling oats are kno~m in ~he art~ ~ne dehulled oats~
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herein fre~uently re~erred to as groat, are comminuted in order to facilikate extraction of oil and to facilitate separation of the comminuted groat so obtained into a flour fraction and a bran fraction. Convention comminuting techniques, for example , pin-milling, hammer milling, corrugated rollers and other shearing techniques, would appear to produce an acceptable comminuted groat. Suitable sizes are exemplified in the examples hereinafter.
The comminuted groat is added to a solvent for the oil in the oats. The solvents used should be acceptable for use with food, e.g., be non-toxic at the levels remaining in the products produced, not cause the formation of toxic materials in the prod-uct and not have a significant deleterious effect on the nutri-tional value of the produc~, and must be capable of causing sepa-ration of the ~lour and bran fractions. ~he amount and type of solvent remaining in products offered for sale must be acceptable to the appropriate health authorities, as will be understood by those skilled in the art. Examples of solvents are pentane, hex-ane, heptane, cyclohexane and alcohols of 1-4 carbon atoms, and mixtures thereof, as used herein the sol~ents hexane and heptane include those solvents referred to in the food industry as hexane and heptane. The preferred solvent is hexane. The present invention will generally be described hereinafter with reference to hexane as the solvent and to the separation of substantially gum-free flour from comminuted groat.
Before separating the comminuted groat into flour and bran fractions it may be desirable to thoroughly mix the solvent, hexane, and comminuted groat for a period of time so as to facilitate extraction of the oil from the comminuted groat, -i.e. to de-oil the comminuted groat. Such mixing is preferably ., - . ' ' .
c-~-carried out with agitation, e.g., by forming a slurry of the comminuted groat and hexane.
According to the present invention there are a number of techniques for separating the flour fraction from the bran fraction. In an embodiment of a so-called batch process the comminuted groat and hexane are thoroughly mixed for a period of time so as to extract oil from the comminuted groat. The mixing may then be adjusted to efEect separation of the mixture of com-minuted groat and hexane into a flour fraction and a bran frac-tion, as is discussed in more detail hereinafter, or the mixingmay be discontinued. If mixing is discontinued, the bran frac-tion tends to settle relatively rapidly, thereby allowing the flour fraction to be separated from the bran fraction of the admixture. The flour fraction should be separated as soon as practical after cessation of mixing as the flour in the flour fraction also tends to settle thereby making separation from the bran fraction less efficient and/or more difficult. In the ernbodiment of the process involving the cessation of mixing it is preferable to repeat the above sequence of steps one or more times e.g., by adding hexane each time and re-mixing, in order to effect a high degree of separation of the comminuted groat into flour and bran. Alternatively the admixture of comminuted groat and hexane may be separated into fractions by sieving the admix-ture. The mesh size of the sieve selected will depend primarily on the degree of separation desired. Preferahly a sieve having a fine mesh e.g., 300 or finer, is used, the use of a 325 mesh TYLER* sieve being exemp~ified herein-after. The bran fraction, which as exemplified is retained . .
on the sieve, may be used as such or subjected to further ` 30 comminution as described hereinafter. Preferably the * denotes trade mark `, '`', ~'':
':
mesh size o~ the sieve is suc'n that the solid component of ~he ~lour fraction, which passes through the sieve, is ~rhite and essentially ~ree o~ bran.
In another embodiment, ln particular when the pro-cess is operated as a so-called continuous process, separation of the admixture o~ commlnuted groat and hexane may be e~ected by care~ul control of the mixing o~ the comminuted groat and hexane, especially immediately prior to and during sep-aration o~ the flour and bran fractions. Such control of the mixing is essential to cause a non-uni~orm distribution of comminuted ~roat in the hexane and separation o~ the comminuted groat into ~ractions. I~ the mixing is too ef~icient a "uniform" mixtur~ of comminuted groat and hexane will be obtained -and separation of the comminuted groat into the flour and ~ran ~ractions will not occur in situ. Separation ma~, howeverJ be e!~fected b~ removing a portion of the mixture of comminuted groat and hexane, separating e.g. by using a sieve, the flour ~raction and recycling the bran ~raction. I~ the mix-ing is insufficien~ the distribution o~ comminuted gro2t in the hexane will be non-uni~orm and the comminuted groat tends not to separate in~o ~ractions unless periods of insufficient mlxing ara interspersed with periods in which there is a higher degree o~ mixing.
Intermediate between the sta~es o~ uniform mixing and of insuf~icient mixing described above, the mixing is capable of being controlled so as to produce continuously a non-uniform distribution o~ comminuted groat in the hexane and in particular ~o produce two ~ractions of com~inuted groat in the hexane.
The first ~raction, usually the upper fraction, is comprised of flour as the major solid component. The second fraction, usually the lower fxaction, is comprised of bran as a ma~or ~, ~
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component. As exemplified hereinafter the mixing may be controlled so that the two fractions are distinc-t, except near the interface between the two fractions, in terms of colour and general appearance. The two fractions are capable of being sepa-rated from each other. One separation technique relies on par-tial separation of the flour fraction, followed by addition of hexane to the fractions remaining and to subsequently eEfect fur-ther separation of a flour fraction from the bran fraction, as described hereinabove with reference to the embodiment involving 10 the discontinuation of mixing. A preferred separation technique -comprises continuously adding hexane to the mixture of hexane and comminuted groat and at the same time removing hexane and part of, in particular, the flour fraction. Using the latter separa- ~ `
tion technique any flour suspended in the bran fraction is cap-able of being separated. It may be desirable to sieve the flour fraction as it is being separated from the bran fraction, or thereafter, and to return any oversize particles to the bran fraction for further treatment. The bran fraction may also be separated. The bran fraction separated in the process of the ~ -~
pr~sent invention may be comprised of bran particles having endo-sperm adhered there~o. The bran fraction, after separation from any hsxane, may be subjected to further comminution and either ~ ;
returned to the admixture of comminuted oats and hexane for fur-ther separation into flour and bran fractions or separate~ly admixed with hexane and separated into further flour and bran fractions. Bran fractions of varying endosperm content are obtainable.
The flour may be separated from the flour fraction by known techniques for separating a solid from a solution. For example, the flour may be separated from the flour fraction by centrifuging techniques. As the hexane contains dissolved oil, -~
it may be desirable to wash the flour after separation so ~ 7 ~
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as to remove any oil adsorbed Qn the flour. me oil may be recovered ~rom the oil-containing hexane solution b~J re-moval of the hexane. Similarly, bran may be recovered from the bran fraction by removal o~ any hexane in ~he fraction.
In these operations the hexane is preferably recovered and re-used in the separation of the flour and bran fractions from the comminuted groat. Al~ernatively, the oil-containing hexane solu~ion may at least in part be used in the separation of the flour and bran ~ractions from the comminuted groa~. ;
While the separation of the flour and bran ~rac~ions has been generally described above as a one step process~ the process may be opera~ed, possibly more efficiently, as a multi-step process, e.g., the flour and bran may be sepærated in a - series of process operations. Such a method may result ln the separation of flour frac~ions containing flour of varying pro-tein conten~s and of bran fractions having varying properties.
Such may be adv~ntageous for some end;uses.
~ ne oil obtained in the process o, the present in-vention m~y be turbid and it may be desirable to clàrify the oil. me oil may be clarified by techniques known in the art or by mixing with isopropanol especially isopropanol containing hydrogen peroxide, agit~ting and then remo~ing any solid ; material, e.g., by centrifuging~ As is exemplifie~ hereinafter a clear brown oil is obtainable. me solids removed on centri-fuging are believed to contain signi~icant amounts of phos-pholipids and may be suitable for use, for example, as emulsi~iers.
~ne flour that is separated by the process o~ the `~ present inventi~n is essentially free of gum. In addition the flour is essentially free o~ oil. The gum and oil content of the flour is exemplifi.ed hereinafter. The water-soluble gums, ~hich are in the bran ~raction, are recoverable. The products of the process o~ the presen~ invention are believed .
--S--to be useful in the food industry either as such or as a source of other products.
The major components of the Elour are starch and pro-tein. The flour is capable of being separated into fractions of varying starch and protein contents using air classification techniques. Protein and starch concentrates may be obtained from the flour by extracting the flour with aqueous acidic or alkaline solu-tions. As is exemplified hereina~ter a high proportion of the protein in the flour may be extracted by forming a slurry of the flour in such aqueous solutions. The pH of the aqueous solu-tion is preferably at least 9.0 and especially about 11.0 if the solution is alkaline and about 2.0 if the solution is acidic.
Examples of suitable alkalisfor the adjustment oE pH are sodium hydroxide and potassium hydroxide. Examples of suitable acids are phosphoric acid, hydrochloric acid and citric acid. As dis-cussed and exemplified herein gums especially water-soluble gums in the oat are separated in the bran fraction in the process described above and the flour obtained is essentially free of gum. Thus processes for the extraction of protein from the flour of the process of the present invention may be operated at low solution viscosities, which is most advantageous from a proces- -sing and especially a product separation point of view. The solid material in the protein extraction solution may be sepa-rated Erom the solution using, for example, centrifuging tech-niques. It may be desirable to wash or re-slurry the solids with water to separate adsorbed solubilized protein and to re-separate the solids. The solid material is comprised primarily of starch. -~ -If the starch contains a minor amount of bran or the like it may be desirable to subject it to, for example, sieving, washing or air classification to purify the starch.
The solubilized protein may be recovered by, for :
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example, isoelectric precipitation. The pH of the solubilized protein solution is adjusted to about 3.5--4.5 with alkali, e.g., sodium hydroxide, or acidr e.g., phosphoric acid, as required.
The precipitate of protein obtained may be separated by, for example, centrifuging the solution. Protein may also be obtained by freeze drying the solution of solubilized protein. This may be especially useful for recovery of acid-soluble protein espe-cially from solutions at the pH a~ which it is de~ired that the protein be soluble. The properties of the protein, including the colour of the protein may depend on the technique of extracting and separating the protein. Protein obtained by alkali or acid extraction is believed to be stable in hot aqueous acidic solu-tions. Acid-soluble protein obtainable from flour, as described herein, may be preferable to that obtainable directly from de-oiled groat. If the protein is to be blended with another substance, e.g., flour, it may be preferable to extract the pro-tein from the flour with an acidic solution and freeze dry the protein as the protein so obtained may be whiter than that obtained by isoelectric precipitation.
Protein may also be extracted from the Elour using aqueous solutions of substantially neutral pH. Such protein is capable of being precipitated in hot water.
The products obtainea in the process described herein are believed to be commercially viable products. The bran frac-tion, with or without added protein~ may be used, for example, in breakfast cereals or as a iller for meat products or pet foods.
The flour is capable of being used as such or when enriched with protein, for example, in breakfast cereals, baby foods and cake ~ i flour. The gum is capable of being extracted from the bran with, for example, hot water and recovered for use as a binder or thickener in the food industry. The oil is capable of being used as, for example, a vegetable oil.
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The present invention is illustrated by the following examples:
EXAMPLE I
Dehulled Hinoat oats, obtained from Agriculture Canada, Ottawa, Ontario, were ground (comminuted) in a CASELLA* grain mill having a 2.5 mm diameter circular hole sieve. 250 g of the resultant ground groat were placed in a vertical cylinder having a diameter of 6.3 cm and a height of 40.6 cm. 600 ml of hexane were added to the cylinder and the resultant mixture was main-tained as a slurry, using an agitator, for 20 minutes at ambienttemperature. Agitation was then stopped and the upper bran-free layer was siphoned off. The procedure was repeated four times with 500 ml of hexane being added each time. The bran layer was then centri~uged to separate hexane and the bran fraction was dried under vacuum at room temperature and weighed.
The hexane fractions were passed through a 325 TYLER
mesh sieve and oversi~e particles were added to the bran frac-tion. Flour was then centrifuged from the hexane solution. Oil was obtained from the resultant hexane solution by evaporating the hexane.
The centrifuged flour was admixed, as a slurry, with hexane to remove any adsorbed oil and re-centrifuged. The flour was then dried under vacuum~ The white flour obtained was very bland to taste.
The bran obtained above was reground in the CASELLA
grain mill using a 0.5 mm diameter circular sieve. 112 g of the reground bran were treated three times with hexane using the procedure described above for ground groat. The bran and flour fractions so obtained were dried. A 5~ g sample o~ this bran : :
fraction was wet ground in hexane in a puck mill and re-treated with hexane. The resultant bran and flour fractions * denotes trade mark :
11 -- . ~
~,: . :, . : '-, , . . . . . . ,,.. . - ~, - . -, ...... ., - .
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were dried.
The results were as Po]lows: (all percentages by weight).
Weight Product Protein Moisture Sample (g) Extracted (~** Content (%~* Content (%) Ground groat 20.5 9.84 First Separation (250 g of ground groat treated) Flour 89.6 35.8 20.5 9.38 Oil 12.3 4.9 Bran 149.5 59.8 22.3 8.46 Second Separation (112 g of reground bran treated) Flour 28.7 25.6 19.6 12.29 Bran 82.9 74.0 7.31 Third Separation (55 g of pucX milled bran treated) Flour 5.1 9.3 29.9 14~84 Bran 49.6 90.2 * based on Kjelda~l analysis for nitrogen times 6.25 ** percentages are based on weight o material treated This example shows that the protein content of the flour is capable of being varied.
EXAMPLE II
A sample of dehulled Hinoat oat was pinmilled using an Alpine CONTRAPLEX*** 250 CW pinmill. It is believed, based on data from the pinmilling of wheat, that 90% of the re3ultant comminuted groat would pass through a 325 mesh TYLER sieve.
200 g of the comminuted groat were placed in a column that was 38.1 cm high, 6.3 cm in diameter and adapted so that hexane could be fed to the bottom of the column and removed, by means of an overflow, near the top of the columnO The column was equipped with a stirrer, the blades of which were near the `' '' ' '.. ' *** denotes trade mark . - - -37~
bottom of the column. Over a period of about two hours 2000 ml of hexane was passed through the column. During this period the stirrer was adjusted so that a separation of the comminuted groat/hexane mixture into a flour fraction and a bran fraction occurred approximately 7.7 cm below the overflow.
The bran was separated from the hexane in the column and dried under vacuum. The flour, which passed with the hexane through the overflow, was centrifuged from the hexane and dried.
Oil was separated from the hexane.
The results were as follows:
Weight Product Extracted Protein Content Sample (g) (~
.. ..
Comminuted Groat 200 23.9 Flour 128.0 64.0 28.75 Bran 62.7 31.4 20.65 Oil 12.8 6~
EXAMPLE III
A sample of dehulled ~inoat oat was ground in a CASELLA
grain mill using a 2.5 mm diameter circular hole sieve. The resultant ground groat was placed in the cylinder of Example II
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and slurried with 600 ml of cyclohexane for 30 minutes at ambient temperature. The stirrer was then stopped and the bran-free upper layer was siphoned o~ This procedure was repeated three times with 500 ml of cyclohexane being added each time. ~-The flour fraction, from the bran-free upper layer, was poured through a 325 mesh TYLER sieve; oversize particles were added to the bran fraction. Bran, flour and oil were separated and dried using the procedures described above.
The results were as follows:
Weight Product Protein Mcisture ~ (g) Extracted (~) Content (~) Content (~) __ , Ground groat 250 20~5 9.8 Flour 73.429~4 17.4 5.2 Bran 145.758.3 23.9 6.5 Oil 14.5 5.8 -; - 13 -. .~ ,., . -.
' ;: . ' : . '. ' ~ . ' ' ' , ;, . ' , :', ' . ' ':
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EXAMPLE_IV
The procedure of Example I]:I was repeated using methanol, instead of cyclohexane, as solvent. The results were as follows:
Weight Product Protein Moisture Sample(g) Extracted (g) Content (g ? Content (g) Ground Groat 250 20.5 9.8 Flour74.5 29.8 19.0 9.4 Bran145.1 58.1 25.6 4.1 Oil11.1 4.4 The flour obtained was very white, odour-free and bland to taste.
EXAMPLE V
A sample of dehulled Hinoat oat was ground in a CASELLA
grain mill using a 2.5 mm diameter circular hole sieve. 500 g of the ground groat were admixed with 1000 ml of hexane in a 2000 ml ; beaker. The resultant mixture was admixed, using a mechanical s1:irrer, as a slurry for 30 minutes at ambient temperature. The stirrer speed was decreased so as to cause separation of the mix-ture into a flour fraction and a bran fraction, and the flour fraction was siphoned off through a 325 mesh TYLER sieve; over-si~e matter was returned to the beaker. The procedure was repeated four times with 100 ml of hexane being added each time.
The 1Our was separated rom the siphoned-off solution using a j centrifuge and dried. 118.1 g of white flour containing 20.3 protein and bland to taste was obtained.
; 20 g samples of the flour were admixed as a slurry, for 30 minutes with 100 ml of distilled water. The pH of the water was adjusted to 11.0, 9.0, 2.6 or 1.5 using either sodium hydrox-ide or phosphoric acid, as appropriateO The slurry was then centrifuged. The supernatant liquid was removed and the solid material admixed as a slurry for 30 minutes with 100 ml of water ~ ~ ' ` ; . ' ' - ~-~7~L5~
to separate adsorbed protein and re-centrifuged. The solids (mainly starch) were dried. The supernatant liquid was combined with that obtained previously and the pH of the resultant solu-tion was adjusted to 4.5 with either sodium hydroxide or phos-phoric acid. The protein, which precipita~ed, was centrifuged from the solution and dried under vacuum.
The results were as follows:
Solution Starch Protein in Protein Protein Content of ~H (g) Starch (%) Fraction (g) Protein Fraction (%) 1011.0 15.60 0.93 4.10 89.5 9.0 15.67 7.4 2.74 88.4
The present invention rela~es to a process for the treatment of comminuted oa-ts so as to effect the separation of ~he comminuted oats into frac~ions of di~fering composition. In particular, the present invention relates to the treatment of comminuted oa~s so as to separate the comminuted oats into a so-called "flour" fraction, a so~called "bran" fraction and an oil, and into products derived therefrom, in which the flour is substantially free of gum.
As used herein the expression "groat" refers to the kernel oE the oat, the expression "flour" refers to the endosperm of the oat and the expression "bran" refers to the bran of the oat, such bran may have endosperm attached thereto as is exempli-fied hereinafter. The expression "gum" refers in particular to water-soluble gum.
Oats are a potential source of a wide variety of useful product~. Examples o~ such products are flour, starch, protein isolate, protein-rich flour, bran, gum and oil. Traditional techniques used in the cereal grain processing industry are ~re-quently difficult to use with oats. For example, milling tech-niques are difficult to use with oats because of process problemsrelating to the presence of oil in the oats. Moreover, unless ~he oats are de-oiled prior to milling, such milling techniques would result in the formation of flours and brans containing oil which may result in rancidity problems on storage of the flour and bran.
Gum, together with some pro~ein and starch, may be removed in part by treatment of oats with water, the resultant dilute aqueous solution of gum, then requiring treatment prior to ; disposal or or recovery of the gum. Protein may be extracted from comminuted oats with aqueous solutions, especially alkaline solutions. However any gum present in the oats may also be ' "
~.:
,, ~ ,.
~87~
extracted into solution and the resultant solutions may be viscous and cause process problems, especially in the separation of solids from the aquoeus solutions.
The composition and properties of water-soluble gums obtained from cereal grains are discussed by B. L. D'Appolonia in a paper presented at the symposium on "Industrial Uses of Cereals" held in conjunction with the 58th Annual Meeting of the Rmerican Association of Cereal Chemists, ~ovember 1973.
A process for the separation o~ acid-soluble protein from comminuted oats, and techniques for the recovery of starch, gum, and the like in related processes, is described in Canadian Application No. 245,163 of of A. Bell, J. R. B. Boocock and R. W. Oughton, filed February 4, 1976. Techniques for the separ-ation of oil from comminuted oats are known such techniques are discussed in the aforementioned application of A. Bell et al. A
process for isolating protein from a pulverized oil seed using liquid fluorocarbons is disclosed in U. ~. Patent 3,869,438 of J. W. Finley et al, which issued March 4, 1975.
Processes for the solvent-extractive milling of maize or corn, wheat, rye and the sorghum grains to remove the bran coat from whole ~ernels of such grains ~ollowed by comminution of ; the whole milled kernels and for separation of fibrous, protein-aceous, endosperm and/or starch fractions derived from such grains are disclosed by T. B. Wayne in Canadian Patents ~364,538, which issued February 23, 1971, and 905,909 and 905,910, both of which issued July 25, 1972.
A need exists ~or the discovery of a process ~or the treatment of comminuted oats, especially for the production of flour and/or protein, that is less susceptible to process problems relating to the presence of oil and gum in the oats.
.
,.
.. . . .
~ 7 ~ 5~
A process for the separation of a flour ~raction a bran fraction and oil from comminuted oats -7n ~rhic~ gum does not cause signi~icant process problems and in which the ~lour is essentially ~ree o~ gum has now been found.
Accordingly, the present invention provides a process ~or the separation o~ a substantially gum~free flour from oats, said process comprising:
(a) adm~xing comminuted oats with an organic solvent, said solvent being capable of extracting oat oil from said oats, and (b) separating substantially gum-free flour ~rom the a~xture of comminuted oats and solvent, the amount o~ -~lour separated from the admixture being at least 20~ by weight of the comminuted oats.
In a prePerred embodiment of the process of the present invention the oats are comminuted dehulled oats.
In another embodiment ~he comminu~ed oats and solvent are admixed under controlled conditions, said controlled conditions being adapted to cause non-uni~orm distribution o~
the com~inuted oats in the solvent.
In ye~ another embod-7ment o~ the controlled conditions ~nclude the cessation o~ mixing immediately prior to separating the first ~raction from the second ~raction~
In a further embodiment the solvent and co~minuted oats are miLxed continuously and under the controllea conditions.
In a still further embodiment solvent is continuously added to ~he comminu~ed oats and the gum-~ree flour is con-tinuously separated ~rom the admixture o~ comm-7nuted oats and solvent.
The comminuted oats used in the process o~ the pre-sent invention are preferably dehulled oats~ Techniques ~or dehulling oats are kno~m in ~he art~ ~ne dehulled oats~
''' ~
herein fre~uently re~erred to as groat, are comminuted in order to facilikate extraction of oil and to facilitate separation of the comminuted groat so obtained into a flour fraction and a bran fraction. Convention comminuting techniques, for example , pin-milling, hammer milling, corrugated rollers and other shearing techniques, would appear to produce an acceptable comminuted groat. Suitable sizes are exemplified in the examples hereinafter.
The comminuted groat is added to a solvent for the oil in the oats. The solvents used should be acceptable for use with food, e.g., be non-toxic at the levels remaining in the products produced, not cause the formation of toxic materials in the prod-uct and not have a significant deleterious effect on the nutri-tional value of the produc~, and must be capable of causing sepa-ration of the ~lour and bran fractions. ~he amount and type of solvent remaining in products offered for sale must be acceptable to the appropriate health authorities, as will be understood by those skilled in the art. Examples of solvents are pentane, hex-ane, heptane, cyclohexane and alcohols of 1-4 carbon atoms, and mixtures thereof, as used herein the sol~ents hexane and heptane include those solvents referred to in the food industry as hexane and heptane. The preferred solvent is hexane. The present invention will generally be described hereinafter with reference to hexane as the solvent and to the separation of substantially gum-free flour from comminuted groat.
Before separating the comminuted groat into flour and bran fractions it may be desirable to thoroughly mix the solvent, hexane, and comminuted groat for a period of time so as to facilitate extraction of the oil from the comminuted groat, -i.e. to de-oil the comminuted groat. Such mixing is preferably ., - . ' ' .
c-~-carried out with agitation, e.g., by forming a slurry of the comminuted groat and hexane.
According to the present invention there are a number of techniques for separating the flour fraction from the bran fraction. In an embodiment of a so-called batch process the comminuted groat and hexane are thoroughly mixed for a period of time so as to extract oil from the comminuted groat. The mixing may then be adjusted to efEect separation of the mixture of com-minuted groat and hexane into a flour fraction and a bran frac-tion, as is discussed in more detail hereinafter, or the mixingmay be discontinued. If mixing is discontinued, the bran frac-tion tends to settle relatively rapidly, thereby allowing the flour fraction to be separated from the bran fraction of the admixture. The flour fraction should be separated as soon as practical after cessation of mixing as the flour in the flour fraction also tends to settle thereby making separation from the bran fraction less efficient and/or more difficult. In the ernbodiment of the process involving the cessation of mixing it is preferable to repeat the above sequence of steps one or more times e.g., by adding hexane each time and re-mixing, in order to effect a high degree of separation of the comminuted groat into flour and bran. Alternatively the admixture of comminuted groat and hexane may be separated into fractions by sieving the admix-ture. The mesh size of the sieve selected will depend primarily on the degree of separation desired. Preferahly a sieve having a fine mesh e.g., 300 or finer, is used, the use of a 325 mesh TYLER* sieve being exemp~ified herein-after. The bran fraction, which as exemplified is retained . .
on the sieve, may be used as such or subjected to further ` 30 comminution as described hereinafter. Preferably the * denotes trade mark `, '`', ~'':
':
mesh size o~ the sieve is suc'n that the solid component of ~he ~lour fraction, which passes through the sieve, is ~rhite and essentially ~ree o~ bran.
In another embodiment, ln particular when the pro-cess is operated as a so-called continuous process, separation of the admixture o~ commlnuted groat and hexane may be e~ected by care~ul control of the mixing o~ the comminuted groat and hexane, especially immediately prior to and during sep-aration o~ the flour and bran fractions. Such control of the mixing is essential to cause a non-uni~orm distribution of comminuted ~roat in the hexane and separation o~ the comminuted groat into ~ractions. I~ the mixing is too ef~icient a "uniform" mixtur~ of comminuted groat and hexane will be obtained -and separation of the comminuted groat into the flour and ~ran ~ractions will not occur in situ. Separation ma~, howeverJ be e!~fected b~ removing a portion of the mixture of comminuted groat and hexane, separating e.g. by using a sieve, the flour ~raction and recycling the bran ~raction. I~ the mix-ing is insufficien~ the distribution o~ comminuted gro2t in the hexane will be non-uni~orm and the comminuted groat tends not to separate in~o ~ractions unless periods of insufficient mlxing ara interspersed with periods in which there is a higher degree o~ mixing.
Intermediate between the sta~es o~ uniform mixing and of insuf~icient mixing described above, the mixing is capable of being controlled so as to produce continuously a non-uniform distribution o~ comminuted groat in the hexane and in particular ~o produce two ~ractions of com~inuted groat in the hexane.
The first ~raction, usually the upper fraction, is comprised of flour as the major solid component. The second fraction, usually the lower fxaction, is comprised of bran as a ma~or ~, ~
.
. .
component. As exemplified hereinafter the mixing may be controlled so that the two fractions are distinc-t, except near the interface between the two fractions, in terms of colour and general appearance. The two fractions are capable of being sepa-rated from each other. One separation technique relies on par-tial separation of the flour fraction, followed by addition of hexane to the fractions remaining and to subsequently eEfect fur-ther separation of a flour fraction from the bran fraction, as described hereinabove with reference to the embodiment involving 10 the discontinuation of mixing. A preferred separation technique -comprises continuously adding hexane to the mixture of hexane and comminuted groat and at the same time removing hexane and part of, in particular, the flour fraction. Using the latter separa- ~ `
tion technique any flour suspended in the bran fraction is cap-able of being separated. It may be desirable to sieve the flour fraction as it is being separated from the bran fraction, or thereafter, and to return any oversize particles to the bran fraction for further treatment. The bran fraction may also be separated. The bran fraction separated in the process of the ~ -~
pr~sent invention may be comprised of bran particles having endo-sperm adhered there~o. The bran fraction, after separation from any hsxane, may be subjected to further comminution and either ~ ;
returned to the admixture of comminuted oats and hexane for fur-ther separation into flour and bran fractions or separate~ly admixed with hexane and separated into further flour and bran fractions. Bran fractions of varying endosperm content are obtainable.
The flour may be separated from the flour fraction by known techniques for separating a solid from a solution. For example, the flour may be separated from the flour fraction by centrifuging techniques. As the hexane contains dissolved oil, -~
it may be desirable to wash the flour after separation so ~ 7 ~
7~
as to remove any oil adsorbed Qn the flour. me oil may be recovered ~rom the oil-containing hexane solution b~J re-moval of the hexane. Similarly, bran may be recovered from the bran fraction by removal o~ any hexane in ~he fraction.
In these operations the hexane is preferably recovered and re-used in the separation of the flour and bran fractions from the comminuted groat. Al~ernatively, the oil-containing hexane solu~ion may at least in part be used in the separation of the flour and bran ~ractions from the comminuted groa~. ;
While the separation of the flour and bran ~rac~ions has been generally described above as a one step process~ the process may be opera~ed, possibly more efficiently, as a multi-step process, e.g., the flour and bran may be sepærated in a - series of process operations. Such a method may result ln the separation of flour frac~ions containing flour of varying pro-tein conten~s and of bran fractions having varying properties.
Such may be adv~ntageous for some end;uses.
~ ne oil obtained in the process o, the present in-vention m~y be turbid and it may be desirable to clàrify the oil. me oil may be clarified by techniques known in the art or by mixing with isopropanol especially isopropanol containing hydrogen peroxide, agit~ting and then remo~ing any solid ; material, e.g., by centrifuging~ As is exemplifie~ hereinafter a clear brown oil is obtainable. me solids removed on centri-fuging are believed to contain signi~icant amounts of phos-pholipids and may be suitable for use, for example, as emulsi~iers.
~ne flour that is separated by the process o~ the `~ present inventi~n is essentially free of gum. In addition the flour is essentially free o~ oil. The gum and oil content of the flour is exemplifi.ed hereinafter. The water-soluble gums, ~hich are in the bran ~raction, are recoverable. The products of the process o~ the presen~ invention are believed .
--S--to be useful in the food industry either as such or as a source of other products.
The major components of the Elour are starch and pro-tein. The flour is capable of being separated into fractions of varying starch and protein contents using air classification techniques. Protein and starch concentrates may be obtained from the flour by extracting the flour with aqueous acidic or alkaline solu-tions. As is exemplified hereina~ter a high proportion of the protein in the flour may be extracted by forming a slurry of the flour in such aqueous solutions. The pH of the aqueous solu-tion is preferably at least 9.0 and especially about 11.0 if the solution is alkaline and about 2.0 if the solution is acidic.
Examples of suitable alkalisfor the adjustment oE pH are sodium hydroxide and potassium hydroxide. Examples of suitable acids are phosphoric acid, hydrochloric acid and citric acid. As dis-cussed and exemplified herein gums especially water-soluble gums in the oat are separated in the bran fraction in the process described above and the flour obtained is essentially free of gum. Thus processes for the extraction of protein from the flour of the process of the present invention may be operated at low solution viscosities, which is most advantageous from a proces- -sing and especially a product separation point of view. The solid material in the protein extraction solution may be sepa-rated Erom the solution using, for example, centrifuging tech-niques. It may be desirable to wash or re-slurry the solids with water to separate adsorbed solubilized protein and to re-separate the solids. The solid material is comprised primarily of starch. -~ -If the starch contains a minor amount of bran or the like it may be desirable to subject it to, for example, sieving, washing or air classification to purify the starch.
The solubilized protein may be recovered by, for :
_ 9 _ ~
., , 7~5~
example, isoelectric precipitation. The pH of the solubilized protein solution is adjusted to about 3.5--4.5 with alkali, e.g., sodium hydroxide, or acidr e.g., phosphoric acid, as required.
The precipitate of protein obtained may be separated by, for example, centrifuging the solution. Protein may also be obtained by freeze drying the solution of solubilized protein. This may be especially useful for recovery of acid-soluble protein espe-cially from solutions at the pH a~ which it is de~ired that the protein be soluble. The properties of the protein, including the colour of the protein may depend on the technique of extracting and separating the protein. Protein obtained by alkali or acid extraction is believed to be stable in hot aqueous acidic solu-tions. Acid-soluble protein obtainable from flour, as described herein, may be preferable to that obtainable directly from de-oiled groat. If the protein is to be blended with another substance, e.g., flour, it may be preferable to extract the pro-tein from the flour with an acidic solution and freeze dry the protein as the protein so obtained may be whiter than that obtained by isoelectric precipitation.
Protein may also be extracted from the Elour using aqueous solutions of substantially neutral pH. Such protein is capable of being precipitated in hot water.
The products obtainea in the process described herein are believed to be commercially viable products. The bran frac-tion, with or without added protein~ may be used, for example, in breakfast cereals or as a iller for meat products or pet foods.
The flour is capable of being used as such or when enriched with protein, for example, in breakfast cereals, baby foods and cake ~ i flour. The gum is capable of being extracted from the bran with, for example, hot water and recovered for use as a binder or thickener in the food industry. The oil is capable of being used as, for example, a vegetable oil.
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The present invention is illustrated by the following examples:
EXAMPLE I
Dehulled Hinoat oats, obtained from Agriculture Canada, Ottawa, Ontario, were ground (comminuted) in a CASELLA* grain mill having a 2.5 mm diameter circular hole sieve. 250 g of the resultant ground groat were placed in a vertical cylinder having a diameter of 6.3 cm and a height of 40.6 cm. 600 ml of hexane were added to the cylinder and the resultant mixture was main-tained as a slurry, using an agitator, for 20 minutes at ambienttemperature. Agitation was then stopped and the upper bran-free layer was siphoned off. The procedure was repeated four times with 500 ml of hexane being added each time. The bran layer was then centri~uged to separate hexane and the bran fraction was dried under vacuum at room temperature and weighed.
The hexane fractions were passed through a 325 TYLER
mesh sieve and oversi~e particles were added to the bran frac-tion. Flour was then centrifuged from the hexane solution. Oil was obtained from the resultant hexane solution by evaporating the hexane.
The centrifuged flour was admixed, as a slurry, with hexane to remove any adsorbed oil and re-centrifuged. The flour was then dried under vacuum~ The white flour obtained was very bland to taste.
The bran obtained above was reground in the CASELLA
grain mill using a 0.5 mm diameter circular sieve. 112 g of the reground bran were treated three times with hexane using the procedure described above for ground groat. The bran and flour fractions so obtained were dried. A 5~ g sample o~ this bran : :
fraction was wet ground in hexane in a puck mill and re-treated with hexane. The resultant bran and flour fractions * denotes trade mark :
11 -- . ~
~,: . :, . : '-, , . . . . . . ,,.. . - ~, - . -, ...... ., - .
7~5~
were dried.
The results were as Po]lows: (all percentages by weight).
Weight Product Protein Moisture Sample (g) Extracted (~** Content (%~* Content (%) Ground groat 20.5 9.84 First Separation (250 g of ground groat treated) Flour 89.6 35.8 20.5 9.38 Oil 12.3 4.9 Bran 149.5 59.8 22.3 8.46 Second Separation (112 g of reground bran treated) Flour 28.7 25.6 19.6 12.29 Bran 82.9 74.0 7.31 Third Separation (55 g of pucX milled bran treated) Flour 5.1 9.3 29.9 14~84 Bran 49.6 90.2 * based on Kjelda~l analysis for nitrogen times 6.25 ** percentages are based on weight o material treated This example shows that the protein content of the flour is capable of being varied.
EXAMPLE II
A sample of dehulled Hinoat oat was pinmilled using an Alpine CONTRAPLEX*** 250 CW pinmill. It is believed, based on data from the pinmilling of wheat, that 90% of the re3ultant comminuted groat would pass through a 325 mesh TYLER sieve.
200 g of the comminuted groat were placed in a column that was 38.1 cm high, 6.3 cm in diameter and adapted so that hexane could be fed to the bottom of the column and removed, by means of an overflow, near the top of the columnO The column was equipped with a stirrer, the blades of which were near the `' '' ' '.. ' *** denotes trade mark . - - -37~
bottom of the column. Over a period of about two hours 2000 ml of hexane was passed through the column. During this period the stirrer was adjusted so that a separation of the comminuted groat/hexane mixture into a flour fraction and a bran fraction occurred approximately 7.7 cm below the overflow.
The bran was separated from the hexane in the column and dried under vacuum. The flour, which passed with the hexane through the overflow, was centrifuged from the hexane and dried.
Oil was separated from the hexane.
The results were as follows:
Weight Product Extracted Protein Content Sample (g) (~
.. ..
Comminuted Groat 200 23.9 Flour 128.0 64.0 28.75 Bran 62.7 31.4 20.65 Oil 12.8 6~
EXAMPLE III
A sample of dehulled ~inoat oat was ground in a CASELLA
grain mill using a 2.5 mm diameter circular hole sieve. The resultant ground groat was placed in the cylinder of Example II
, .
and slurried with 600 ml of cyclohexane for 30 minutes at ambient temperature. The stirrer was then stopped and the bran-free upper layer was siphoned o~ This procedure was repeated three times with 500 ml of cyclohexane being added each time. ~-The flour fraction, from the bran-free upper layer, was poured through a 325 mesh TYLER sieve; oversize particles were added to the bran fraction. Bran, flour and oil were separated and dried using the procedures described above.
The results were as follows:
Weight Product Protein Mcisture ~ (g) Extracted (~) Content (~) Content (~) __ , Ground groat 250 20~5 9.8 Flour 73.429~4 17.4 5.2 Bran 145.758.3 23.9 6.5 Oil 14.5 5.8 -; - 13 -. .~ ,., . -.
' ;: . ' : . '. ' ~ . ' ' ' , ;, . ' , :', ' . ' ':
~17~5~
EXAMPLE_IV
The procedure of Example I]:I was repeated using methanol, instead of cyclohexane, as solvent. The results were as follows:
Weight Product Protein Moisture Sample(g) Extracted (g) Content (g ? Content (g) Ground Groat 250 20.5 9.8 Flour74.5 29.8 19.0 9.4 Bran145.1 58.1 25.6 4.1 Oil11.1 4.4 The flour obtained was very white, odour-free and bland to taste.
EXAMPLE V
A sample of dehulled Hinoat oat was ground in a CASELLA
grain mill using a 2.5 mm diameter circular hole sieve. 500 g of the ground groat were admixed with 1000 ml of hexane in a 2000 ml ; beaker. The resultant mixture was admixed, using a mechanical s1:irrer, as a slurry for 30 minutes at ambient temperature. The stirrer speed was decreased so as to cause separation of the mix-ture into a flour fraction and a bran fraction, and the flour fraction was siphoned off through a 325 mesh TYLER sieve; over-si~e matter was returned to the beaker. The procedure was repeated four times with 100 ml of hexane being added each time.
The 1Our was separated rom the siphoned-off solution using a j centrifuge and dried. 118.1 g of white flour containing 20.3 protein and bland to taste was obtained.
; 20 g samples of the flour were admixed as a slurry, for 30 minutes with 100 ml of distilled water. The pH of the water was adjusted to 11.0, 9.0, 2.6 or 1.5 using either sodium hydrox-ide or phosphoric acid, as appropriateO The slurry was then centrifuged. The supernatant liquid was removed and the solid material admixed as a slurry for 30 minutes with 100 ml of water ~ ~ ' ` ; . ' ' - ~-~7~L5~
to separate adsorbed protein and re-centrifuged. The solids (mainly starch) were dried. The supernatant liquid was combined with that obtained previously and the pH of the resultant solu-tion was adjusted to 4.5 with either sodium hydroxide or phos-phoric acid. The protein, which precipita~ed, was centrifuged from the solution and dried under vacuum.
The results were as follows:
Solution Starch Protein in Protein Protein Content of ~H (g) Starch (%) Fraction (g) Protein Fraction (%) 1011.0 15.60 0.93 4.10 89.5 9.0 15.67 7.4 2.74 88.4
2.6 1~.48 3.2 3.30 90.8 1.5 14.60 1.7 4.16 83.'7 All protein fractions were white but that extracted with the acid solution was whiter than that obtained using the alkali solution.
EXAMPLE VI
The dried bran fraction of Example V was milled in an e~perimental wheat mill equipped with breaker and reduction rolls and sifters and designed to simulate a commercial wheat milling operation. Four fractions viz bran, coarse shorts, fine shorts and flour were obtained. ~o process problems were observed in the milling~ The flour obtained was whi-te and bland to taste.
The results, reported on a dry matter basis, were as follows:
Fraction Protein Oil Crude Ash Sample o~ Bran (%) (~) _ (%) Fiber (~ (%) Bran 19.4 30.2 1.60 3.32 3.92 Coarse Shorts30.6 31.1 3.01 2.85 4.15 Fine Shorts9.5 24.6 2.28 2.44 3.02 .. . ... . - 15 - ~;
.:
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37~LS~L
continued from Page 15 Fraction Protein Oil Crude Ash Sample of Bran (%) (%) (%) Fiber (%? (%) Flour 19.8 15.4 1.07 0.70 1.23 Flour* - 24.5 0.~8 0.43 1.12 * for comparison, the results are for the flour of Example V.
EXAMPLE VII
174.3 g of oil, which was turbid and green, obtained by the extraction of Hinoat oat with hexane was mixed with 500 ml of 2-propanol for 15 minutes. The resultant solution was centri-fuged and the clear brown upper layer was decanted. The 2-propanol was removed using a rotary evaporator. The oil (125.5 g) obtained was clear and brown.
EXAMPLE VIII
To show the distribution of water-soluble gums in the products of Example II, 20 g of each of ground groat, flour and bran were admixed, as a slurry, with 80 ml of distilled water at 25C. The viscosity of the solution was then determined using a BROOKFIELD* model LVF #1 spindle at 60 rpm.
The resul-ts were as follows:
Sample Viscosity (cps)****
Ground Groat 400 Flour 8 Bran **
Water*** 2.5 ** could not be determined, solution was like paste *** referen~e, water only **** as indicated on viscometer EXAMPLE IX
~,:
Dehulled oats were ground in a CASELLA grain mill ~
: :
having a 2.5 mm diameter circular hole sieve and then reground in the mill using a 1 mm sieve. 250 g of the resultant ground ~-~:, ': ' * denotes trade mark '' groat were placed in a vertical cylinder having a diameter of 6.3 cm and a height o~ 40.6 cm. 600 ml of hexane were added to the cylinder and the resultant mixture was admixed, as a slurry, using an agitator, for 30 minutes at ambient temperature. The speed o~ the agitator was then adjusted so as to cause separation of the slurry into a flour ~raction and a bran fraction. The flour fraction was siphoned off. The extraction procedure was repeated four times, 500 ml of hexane being added each time.
Bran was recovered from the bran fraction and dried. -Flour was centrifuged ~rom the flour fractions, re-admixed, as a slurry with 500 ml of hexane, separated from the hexane solution by centrifuging and dried. Oil was recovered from the hexane solutions.
T~e oil contents of the ground groat, flour and bran were determined by soxhlet extraction using hot hexane.
The results were as follows:
Product Oil Content SampleExtracted (%) _(%) Ground Groat - 5.6 Flour 43.0 0.08 Oil 6.1 Bran 47.4 o.~g EXAMPLE X
Dehulled Hinoat oats (groat) were comminuted in a commercial hammer mill. 200 g o~ the comminuted oats were admixed in the form o~ a slurry for 30 minutes with 400 g of n-heptane (b.p. 97-98C) and then sieved using a 325 mesh TYLER
sieve. m e oversize material i.e. that retained on the sieve, was re-admixed with 400 g of n-heptane in the form of a slurry for 30 minutes and then re-sieved. Once again the oversize -material obtained was admixed, as a slurry, with 400 g _ ~7 ~
,' "
-' of n-heptane for 30 minutes and re-sieved. The oversized material thus obtained, referred to below as bran, was dried overnight in a vacuum oven. The bran was buff coloured~
The undersized material, i.e. that passing through the sieve, from each of the sievings was combined and then centri-fuged. The solution of n-heptane and oil was decanted off. The solid material f~om the centrifuge was admixed with 200 g of n~heptane in the form of a slurry so as to remove any adsorbed oil and re-centrifuged, the n-heptane solution again being decanted off. The oil was separated ~rom the n-heptane from the combined n-heptane/oil solutions using a rotary evaporator and dried overnight in a vacuum oven. The oil was green and turbid.
The solid material from the centrifuge, referred to below as ~lour, was dried overnight in a vacuum oven. The flour was white in colour.
The protein content was measured as in Example I.
The results were as follows:
Weight Protein Content (g?Percentage of Groat (%?
20 Groat 200 19.4 Oil 15.1 7.6 Flour 102.2 51.1 18.6 Bran 68.8 34.4 23.2 Recovery 93.1 EXAMPLE XI
Dehulled Hinoat oats (groat) were comminuted using a BEUHLER* laboratory scale corrugated roller mill. The fractions obtained from the mill were combined and were shown to have the following particle size distribution. -~
* denotes trade mark .
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.... _~ . . . . . . . .
~: , , ~ . : .
Particle Size Percentage b~J I~Jeight (TYLER mesh) _ -+10 5.0 - +12 7.2 +1~ 18.0 +20 16~1 ~2~ 10O2 --25 ~3-5 242.4 g of the above commlnuted ~roat were admixed with 484.o ~ of hexane, in the form of a slurry, for 30 minutes. The slurr~y was then sieved through a 325 mesh TYLER
sieve. The oversiæed material i.e. that re~ained on the sieve, was re-admixed with a ~urther 484.~ g of hexane, as a slurry, for 30 ~inutes and re-sieved. The resultant over sized material was once aga~n re-admixed with 484.8 g Of he~ane, in the ~orm o~ a slurry, for 30 minutes and re-sieved.
me oversized material thus obtained, referred to hereinbelow as bran5 Nas washed with 200 ml of hex~ne and then dried ove-r-~., , night in a vacuum oven. me bran so ob~ained was bu~f coloured.
The undersized materialJ i.e. that passing through the sieve, from all of the above sievings ~as combined and centrifugedO The solid material from the centri~uge, referred to below as flour, was admixed with 200 ml of hexane, in the form of a slurr~, so as to remove an~ adsor~ed oil, and centri-.
fugedO The ~lour was dried overnight in a vacuum oven. ~ne - flour was very white in colour.
The oil was recovered from the solutions of hexane and oil decanted ~rom the above centrifuged solutions using a rctary evaporation. The oil was maintained under vacuum overnight in a vacuum oven. The oil was green in colour and tur~id.
The residual oil in the flour ~nd bran fractions was ' ' . -. -19- '.
7~
determined using a hot Soxhlet e~traction with hexane as th~
solvent.
e results were as ~ollows:
Welght P~rcentages of Residual Oil Protein I~ _ Commlnuted ~ro t ~ (%? .
Comminuted Groat 242.l~ 18.3 Flour 119.7 49.4 0.01 15.1 Bran 107.9 44.5 1.66 24.2 looil 14.7 6.1 * ~ meaæured by total nitrogen x 6.2~ on a KJel - Foss*~ automatlc analyzer.
EXAMEI~ XII
A 25 g sample o~ the bran fraction obtained in -~ -Example XI was extracted wlth water at 50C for 40 minutes.
. . .
The 501utlon obtained was then centrifuged. The aqueous solu- : .
!
tion wa~ decanted from the sollds ~nd co~blned with twice its volume o~ methanol. The preclpitate Or crude gu~ so obtained ~as centrl~uged ~rom th~ l~qu~d and dried overnight in a 20 vacuum oven. me dried crude gum obt,~ined was 9~5$~ b~ weight o~ the bran.
~ hen the procedure was repeated usin~3 the ~lour ~r~ctîon o* Example XI, the dried crude gum obtained wa~ 0.5%
by weight of the ~lour. mus in the procedure o~ 13xam~ XII
~or s~parating commirluted oats into bran ~lour and oil ~ractions ~ . .
the gum primarlly remains with the bran, the flour belng sub~
stantially ~ree o~ ~um.
E~AUPIE XIII .
~n order to show that additional flour ma~ be sep ~ -30 ar~ted ~rom the bran fraction o~ Example XIIg the bran was .
re-~round using a CA~ELLA ~11 having a 0.5 mm circular ~ie~e.
50 g o~ the re-gro~nd material ~a~ admixed with 200 g o~
hexane, in the ~orm of a ~lurry, ~or 15 minutes. The resultant *~ denote~ trade ~rk `. :
~i, :;
. , - . . , . ~ , . - . .
~ ~P~4~
slurry was sieved through a 325 mesh TYLER sieve. ~he over~
size material retained on the sieve was admixed, as a slurry, with a ~urther 200 g o~ hexane J for 15 minutes ~nd re-sieved.
Tkeoversized ~aterial (bran) was dried overnight in a vacuum oven. ~ne undersized material in the hexane was centrifuged ~ and the solids (flour) separated and dried overnignt in a ; vacuum oven. The flour obtained was white and the bran was buff coloured.
The results were as follows:
WeightPercentage of Protein (g)~ran Fract~on ~) Bran Fraction50.0 24.2 Flour 10.0 20.0 16~3 Bran 35.6 71.2 27.3 EXA~LE XIV
A 20 g sample o~ a ~lour containing 11~3~ protein was admixed, as a slurry, with 80 ml of distilled wa~er. me pH of the slurry was adjusted to 2.0 using dilute hydrochloric acid. The slurr~ was maintained at ambient temperature for 30 minutes and then centrifuged. The supernat~nt liquid was dec~ted off and the solids wers re-adm~Lxed, as a slurr~, witn 80 ml of distilled water, the pH o~ which ~as then adjus~ed to 2Ø After 30 minutes the slurry was centrifuged and the supernatant li~uid ~s combined "ith that previously ob-tained. Tne pH o~ the resultant solution ~las then adjusted to 4.5 using dilute sodium hYdroxide. The precipit2te of acid-soluble protein ~ras separated and freeze dried. The solids, re~erred to below as starch, separated from the first two centri~ugations was dried in a vacuum oven.
me above procedure was repeated using ~n aqueous hydrochloric acid solution at a temperature of 50C and using phosphoric acid solutions, instead of the h~Jdrochloric acid ~ .
4~i~
solutions, ~t ambient te~perature and at 50C.
~he results were as follows:
Run 1 Run 2 ~un 3 Run 4 Acid Hydrochloric ~ydrochloric Phosphoric Phosphoric Temperatureambient 50C ambien~ 50C
Weight OL
Flour (g) 20.0 20.0 20.0 20.0 Acid-Soluble : Protein : 10 Weight (g) 1.3 1.4 1.8 1.8 Protein Content~99.4 99.4 93.3 94.9 Starch Neight (g) 16.8 16.8 16.7 16.9 Protein Ccntent(~) 1.6 1.6 1.2 2.2 ` .
Recovery o~ :
Starting ~laterial (flour)($) 91 91 93 94 Both the acid-soluble protein obtained ~nd the starch o~tained were ~ery white in appearance~
To illustrate the solubili-ty of the acld-soluble pro-tein~ one gram o~ the protein from Run 3 was ~dded ~o 99 g o~ ~:
water, the p~ o~ which ~s then adJusted to 2.6. Af~er s~irring ~or 30 mlnutes the solution was cent~i~uged to remove any undissolved solids. The supernatant liquid was sep~ra~ed and analyzed ~or proteinO Ihe solution contained 0.93~ protein indicating that 99.7~ of the protein in the acid-soluble pro-tein had gone into solution.
EX~LE XV
40 g of dehulled Hinoat oats that has been comminuted in a commercial-scale ham~er mill were a~itated, in the ~orm o~
a slurr~, with 160 g o~ 2-propanol ~or 15 minutes. The resultant admuLxture ~las s~eved using ~ 325 mesh TYLER sieve. ~he o~er~
size material i.e. that retained on the sieve, W&S re-admiYed, in the form ol a slurry3 ~Jith a further 160 g of 2-propanol for ,'.' ~',:
~ ~7 ~ ~
15 ~inutes and re-sieved. ~he oversiæed material obtained was once again ad~i~ed with 1~0 g of 2-propanol for 15 minutes and re-sievedO The oversized material thus obtained, referred to below as bran, w~s dried in a vacuum oven overnight. ~ne under-size material~ i e. that passing through the sieve, ~rom all sievings was combined and cen~rifuged. The solvent was decanted of~ and the solid material (flour) was dried overnight in a vacuum oven. Oat oil was recovered from the decanted solvent using a rotary evaporator and dried overnight in a vacuum oven.
The ~lour and bran were ~nalyzed ~or protein using a ~el - Foss Automatic Protein Analyzer.
The results were as ~ollows:
Product WeightPercentage of Protein Colour ~Starting Material ~) ~ _ . . .
F~our 21~85 54.6 13-5 white Bran 11~66 29.2 21.0 buf~
Oil 3.40 8.5 yellow EXAMPLE XVI
The procedure o~ Example VIII was repeated using ~o the bran and flour obtained by the procedure of Example XV
; except th~t a ~2 spindle ~as used in the viscometer.
me results were as follo~s: -Sam~le Viscosity (c~s~
Flour 15 Bran *
Water** 6.5 *too viscous to measure `~ **reference, water only.
The above procedure was also repeated using the flour and br~n obtained by the procedure of Example X.
The results were as follows:
. ~ ~
-23- ~
. .
~:
.
~ 5 Sample Viscosi_y Flour 27.5 Bran *
*too viscous to measure.
EXAMPLE XVII
~, . .
Dehulled Scott oats, which contained 17.~ by weight o~ protein, were ground in a CASEL~A grain mill havi~g a l.O mm circular hole sieve. 50 g of the resultant groat were admixed, as a slurry, with 150 g of hexane for 15 minutes at ambient temperature and then sieved using a 325 me~h TYLER sieve.- The oversized material, i.e. that retained on the sieve, was re-admix~d with 150 g o~ hexa~e, in the ~orm of a slurry, ~or 15 minutes and then re-sieved. Once again the oversized materiaI
obtained was re-adml~ed with 150 g of hexane for 15 minutes and re-sieved. me buf~ coloured oversize material thus obtained, which is re~erred to below as bran, ~as dried overnight in a vacuum oven.
The undersized material i.e~ that passing through the sieve, ~rom each o~ the sievings was combined and centrifuged.
~0 The solution o~ hexane and oil was d~cænted of~. The solid material ~rom the centrifuge was admixed with 150 g of hexane in the ~orm of a slurry so as to remove adsorbed oil and re-centrifuged, the hexane solution again being dec~nted o~ The oil was separated from the hexane from the combined hex~ne oil solutions using a rotary evaporator and dried overnight in a vacuum oven. me oil was green ~nd turbid.
The solid material from the centrifuge, re~erxed to below as ~lour, was dried overnigh~ in a vacuum oven. The ~lour was white in colour.
me ~lour and bran were analyzed for protein using a Kjel - Foss protein analyzerO The results were as ~ollows: -.. .. .
.- . :, ~ -. ,, . " . . : . : - :
~i7~
Weight Protein .. . , ~$) ' ~
Bran 17,4 25.1 Flour 25.1 17.1 Oil 2.7
EXAMPLE VI
The dried bran fraction of Example V was milled in an e~perimental wheat mill equipped with breaker and reduction rolls and sifters and designed to simulate a commercial wheat milling operation. Four fractions viz bran, coarse shorts, fine shorts and flour were obtained. ~o process problems were observed in the milling~ The flour obtained was whi-te and bland to taste.
The results, reported on a dry matter basis, were as follows:
Fraction Protein Oil Crude Ash Sample o~ Bran (%) (~) _ (%) Fiber (~ (%) Bran 19.4 30.2 1.60 3.32 3.92 Coarse Shorts30.6 31.1 3.01 2.85 4.15 Fine Shorts9.5 24.6 2.28 2.44 3.02 .. . ... . - 15 - ~;
.:
. :
.
37~LS~L
continued from Page 15 Fraction Protein Oil Crude Ash Sample of Bran (%) (%) (%) Fiber (%? (%) Flour 19.8 15.4 1.07 0.70 1.23 Flour* - 24.5 0.~8 0.43 1.12 * for comparison, the results are for the flour of Example V.
EXAMPLE VII
174.3 g of oil, which was turbid and green, obtained by the extraction of Hinoat oat with hexane was mixed with 500 ml of 2-propanol for 15 minutes. The resultant solution was centri-fuged and the clear brown upper layer was decanted. The 2-propanol was removed using a rotary evaporator. The oil (125.5 g) obtained was clear and brown.
EXAMPLE VIII
To show the distribution of water-soluble gums in the products of Example II, 20 g of each of ground groat, flour and bran were admixed, as a slurry, with 80 ml of distilled water at 25C. The viscosity of the solution was then determined using a BROOKFIELD* model LVF #1 spindle at 60 rpm.
The resul-ts were as follows:
Sample Viscosity (cps)****
Ground Groat 400 Flour 8 Bran **
Water*** 2.5 ** could not be determined, solution was like paste *** referen~e, water only **** as indicated on viscometer EXAMPLE IX
~,:
Dehulled oats were ground in a CASELLA grain mill ~
: :
having a 2.5 mm diameter circular hole sieve and then reground in the mill using a 1 mm sieve. 250 g of the resultant ground ~-~:, ': ' * denotes trade mark '' groat were placed in a vertical cylinder having a diameter of 6.3 cm and a height o~ 40.6 cm. 600 ml of hexane were added to the cylinder and the resultant mixture was admixed, as a slurry, using an agitator, for 30 minutes at ambient temperature. The speed o~ the agitator was then adjusted so as to cause separation of the slurry into a flour ~raction and a bran fraction. The flour fraction was siphoned off. The extraction procedure was repeated four times, 500 ml of hexane being added each time.
Bran was recovered from the bran fraction and dried. -Flour was centrifuged ~rom the flour fractions, re-admixed, as a slurry with 500 ml of hexane, separated from the hexane solution by centrifuging and dried. Oil was recovered from the hexane solutions.
T~e oil contents of the ground groat, flour and bran were determined by soxhlet extraction using hot hexane.
The results were as follows:
Product Oil Content SampleExtracted (%) _(%) Ground Groat - 5.6 Flour 43.0 0.08 Oil 6.1 Bran 47.4 o.~g EXAMPLE X
Dehulled Hinoat oats (groat) were comminuted in a commercial hammer mill. 200 g o~ the comminuted oats were admixed in the form o~ a slurry for 30 minutes with 400 g of n-heptane (b.p. 97-98C) and then sieved using a 325 mesh TYLER
sieve. m e oversize material i.e. that retained on the sieve, was re-admixed with 400 g of n-heptane in the form of a slurry for 30 minutes and then re-sieved. Once again the oversize -material obtained was admixed, as a slurry, with 400 g _ ~7 ~
,' "
-' of n-heptane for 30 minutes and re-sieved. The oversized material thus obtained, referred to below as bran, was dried overnight in a vacuum oven. The bran was buff coloured~
The undersized material, i.e. that passing through the sieve, from each of the sievings was combined and then centri-fuged. The solution of n-heptane and oil was decanted off. The solid material f~om the centrifuge was admixed with 200 g of n~heptane in the form of a slurry so as to remove any adsorbed oil and re-centrifuged, the n-heptane solution again being decanted off. The oil was separated ~rom the n-heptane from the combined n-heptane/oil solutions using a rotary evaporator and dried overnight in a vacuum oven. The oil was green and turbid.
The solid material from the centrifuge, referred to below as ~lour, was dried overnight in a vacuum oven. The flour was white in colour.
The protein content was measured as in Example I.
The results were as follows:
Weight Protein Content (g?Percentage of Groat (%?
20 Groat 200 19.4 Oil 15.1 7.6 Flour 102.2 51.1 18.6 Bran 68.8 34.4 23.2 Recovery 93.1 EXAMPLE XI
Dehulled Hinoat oats (groat) were comminuted using a BEUHLER* laboratory scale corrugated roller mill. The fractions obtained from the mill were combined and were shown to have the following particle size distribution. -~
* denotes trade mark .
' ' .
. .
.... _~ . . . . . . . .
~: , , ~ . : .
Particle Size Percentage b~J I~Jeight (TYLER mesh) _ -+10 5.0 - +12 7.2 +1~ 18.0 +20 16~1 ~2~ 10O2 --25 ~3-5 242.4 g of the above commlnuted ~roat were admixed with 484.o ~ of hexane, in the form of a slurry, for 30 minutes. The slurr~y was then sieved through a 325 mesh TYLER
sieve. The oversiæed material i.e. that re~ained on the sieve, was re-admixed with a ~urther 484.~ g of hexane, as a slurry, for 30 ~inutes and re-sieved. The resultant over sized material was once aga~n re-admixed with 484.8 g Of he~ane, in the ~orm o~ a slurry, for 30 minutes and re-sieved.
me oversized material thus obtained, referred to hereinbelow as bran5 Nas washed with 200 ml of hex~ne and then dried ove-r-~., , night in a vacuum oven. me bran so ob~ained was bu~f coloured.
The undersized materialJ i.e. that passing through the sieve, from all of the above sievings ~as combined and centrifugedO The solid material from the centri~uge, referred to below as flour, was admixed with 200 ml of hexane, in the form of a slurr~, so as to remove an~ adsor~ed oil, and centri-.
fugedO The ~lour was dried overnight in a vacuum oven. ~ne - flour was very white in colour.
The oil was recovered from the solutions of hexane and oil decanted ~rom the above centrifuged solutions using a rctary evaporation. The oil was maintained under vacuum overnight in a vacuum oven. The oil was green in colour and tur~id.
The residual oil in the flour ~nd bran fractions was ' ' . -. -19- '.
7~
determined using a hot Soxhlet e~traction with hexane as th~
solvent.
e results were as ~ollows:
Welght P~rcentages of Residual Oil Protein I~ _ Commlnuted ~ro t ~ (%? .
Comminuted Groat 242.l~ 18.3 Flour 119.7 49.4 0.01 15.1 Bran 107.9 44.5 1.66 24.2 looil 14.7 6.1 * ~ meaæured by total nitrogen x 6.2~ on a KJel - Foss*~ automatlc analyzer.
EXAMEI~ XII
A 25 g sample o~ the bran fraction obtained in -~ -Example XI was extracted wlth water at 50C for 40 minutes.
. . .
The 501utlon obtained was then centrifuged. The aqueous solu- : .
!
tion wa~ decanted from the sollds ~nd co~blned with twice its volume o~ methanol. The preclpitate Or crude gu~ so obtained ~as centrl~uged ~rom th~ l~qu~d and dried overnight in a 20 vacuum oven. me dried crude gum obt,~ined was 9~5$~ b~ weight o~ the bran.
~ hen the procedure was repeated usin~3 the ~lour ~r~ctîon o* Example XI, the dried crude gum obtained wa~ 0.5%
by weight of the ~lour. mus in the procedure o~ 13xam~ XII
~or s~parating commirluted oats into bran ~lour and oil ~ractions ~ . .
the gum primarlly remains with the bran, the flour belng sub~
stantially ~ree o~ ~um.
E~AUPIE XIII .
~n order to show that additional flour ma~ be sep ~ -30 ar~ted ~rom the bran fraction o~ Example XIIg the bran was .
re-~round using a CA~ELLA ~11 having a 0.5 mm circular ~ie~e.
50 g o~ the re-gro~nd material ~a~ admixed with 200 g o~
hexane, in the ~orm of a ~lurry, ~or 15 minutes. The resultant *~ denote~ trade ~rk `. :
~i, :;
. , - . . , . ~ , . - . .
~ ~P~4~
slurry was sieved through a 325 mesh TYLER sieve. ~he over~
size material retained on the sieve was admixed, as a slurry, with a ~urther 200 g o~ hexane J for 15 minutes ~nd re-sieved.
Tkeoversized ~aterial (bran) was dried overnight in a vacuum oven. ~ne undersized material in the hexane was centrifuged ~ and the solids (flour) separated and dried overnignt in a ; vacuum oven. The flour obtained was white and the bran was buff coloured.
The results were as follows:
WeightPercentage of Protein (g)~ran Fract~on ~) Bran Fraction50.0 24.2 Flour 10.0 20.0 16~3 Bran 35.6 71.2 27.3 EXA~LE XIV
A 20 g sample o~ a ~lour containing 11~3~ protein was admixed, as a slurry, with 80 ml of distilled wa~er. me pH of the slurry was adjusted to 2.0 using dilute hydrochloric acid. The slurr~ was maintained at ambient temperature for 30 minutes and then centrifuged. The supernat~nt liquid was dec~ted off and the solids wers re-adm~Lxed, as a slurr~, witn 80 ml of distilled water, the pH o~ which ~as then adjus~ed to 2Ø After 30 minutes the slurry was centrifuged and the supernatant li~uid ~s combined "ith that previously ob-tained. Tne pH o~ the resultant solution ~las then adjusted to 4.5 using dilute sodium hYdroxide. The precipit2te of acid-soluble protein ~ras separated and freeze dried. The solids, re~erred to below as starch, separated from the first two centri~ugations was dried in a vacuum oven.
me above procedure was repeated using ~n aqueous hydrochloric acid solution at a temperature of 50C and using phosphoric acid solutions, instead of the h~Jdrochloric acid ~ .
4~i~
solutions, ~t ambient te~perature and at 50C.
~he results were as follows:
Run 1 Run 2 ~un 3 Run 4 Acid Hydrochloric ~ydrochloric Phosphoric Phosphoric Temperatureambient 50C ambien~ 50C
Weight OL
Flour (g) 20.0 20.0 20.0 20.0 Acid-Soluble : Protein : 10 Weight (g) 1.3 1.4 1.8 1.8 Protein Content~99.4 99.4 93.3 94.9 Starch Neight (g) 16.8 16.8 16.7 16.9 Protein Ccntent(~) 1.6 1.6 1.2 2.2 ` .
Recovery o~ :
Starting ~laterial (flour)($) 91 91 93 94 Both the acid-soluble protein obtained ~nd the starch o~tained were ~ery white in appearance~
To illustrate the solubili-ty of the acld-soluble pro-tein~ one gram o~ the protein from Run 3 was ~dded ~o 99 g o~ ~:
water, the p~ o~ which ~s then adJusted to 2.6. Af~er s~irring ~or 30 mlnutes the solution was cent~i~uged to remove any undissolved solids. The supernatant liquid was sep~ra~ed and analyzed ~or proteinO Ihe solution contained 0.93~ protein indicating that 99.7~ of the protein in the acid-soluble pro-tein had gone into solution.
EX~LE XV
40 g of dehulled Hinoat oats that has been comminuted in a commercial-scale ham~er mill were a~itated, in the ~orm o~
a slurr~, with 160 g o~ 2-propanol ~or 15 minutes. The resultant admuLxture ~las s~eved using ~ 325 mesh TYLER sieve. ~he o~er~
size material i.e. that retained on the sieve, W&S re-admiYed, in the form ol a slurry3 ~Jith a further 160 g of 2-propanol for ,'.' ~',:
~ ~7 ~ ~
15 ~inutes and re-sieved. ~he oversiæed material obtained was once again ad~i~ed with 1~0 g of 2-propanol for 15 minutes and re-sievedO The oversized material thus obtained, referred to below as bran, w~s dried in a vacuum oven overnight. ~ne under-size material~ i e. that passing through the sieve, ~rom all sievings was combined and cen~rifuged. The solvent was decanted of~ and the solid material (flour) was dried overnight in a vacuum oven. Oat oil was recovered from the decanted solvent using a rotary evaporator and dried overnight in a vacuum oven.
The ~lour and bran were ~nalyzed ~or protein using a ~el - Foss Automatic Protein Analyzer.
The results were as ~ollows:
Product WeightPercentage of Protein Colour ~Starting Material ~) ~ _ . . .
F~our 21~85 54.6 13-5 white Bran 11~66 29.2 21.0 buf~
Oil 3.40 8.5 yellow EXAMPLE XVI
The procedure o~ Example VIII was repeated using ~o the bran and flour obtained by the procedure of Example XV
; except th~t a ~2 spindle ~as used in the viscometer.
me results were as follo~s: -Sam~le Viscosity (c~s~
Flour 15 Bran *
Water** 6.5 *too viscous to measure `~ **reference, water only.
The above procedure was also repeated using the flour and br~n obtained by the procedure of Example X.
The results were as follows:
. ~ ~
-23- ~
. .
~:
.
~ 5 Sample Viscosi_y Flour 27.5 Bran *
*too viscous to measure.
EXAMPLE XVII
~, . .
Dehulled Scott oats, which contained 17.~ by weight o~ protein, were ground in a CASEL~A grain mill havi~g a l.O mm circular hole sieve. 50 g of the resultant groat were admixed, as a slurry, with 150 g of hexane for 15 minutes at ambient temperature and then sieved using a 325 me~h TYLER sieve.- The oversized material, i.e. that retained on the sieve, was re-admix~d with 150 g o~ hexa~e, in the ~orm of a slurry, ~or 15 minutes and then re-sieved. Once again the oversized materiaI
obtained was re-adml~ed with 150 g of hexane for 15 minutes and re-sieved. me buf~ coloured oversize material thus obtained, which is re~erred to below as bran, ~as dried overnight in a vacuum oven.
The undersized material i.e~ that passing through the sieve, ~rom each o~ the sievings was combined and centrifuged.
~0 The solution o~ hexane and oil was d~cænted of~. The solid material ~rom the centrifuge was admixed with 150 g of hexane in the ~orm of a slurry so as to remove adsorbed oil and re-centrifuged, the hexane solution again being dec~nted o~ The oil was separated from the hexane from the combined hex~ne oil solutions using a rotary evaporator and dried overnight in a vacuum oven. me oil was green ~nd turbid.
The solid material from the centrifuge, re~erxed to below as ~lour, was dried overnigh~ in a vacuum oven. The ~lour was white in colour.
me ~lour and bran were analyzed for protein using a Kjel - Foss protein analyzerO The results were as ~ollows: -.. .. .
.- . :, ~ -. ,, . " . . : . : - :
~i7~
Weight Protein .. . , ~$) ' ~
Bran 17,4 25.1 Flour 25.1 17.1 Oil 2.7
Claims (49)
1. A process for the separation of a substantially gum-fre e flour from oats, said process comprising:
(a) admixing comminuted oats with an organic solvent, said solvent being selected from the group consisting of pentane, hexane, heptane, cyclohexane and alcohols of 1-4 carbon atoms, and mixtures thereof, and (b) separating substantially gum-free flour from the admixture of comminuted oats and solvent, the amount of flour separated from the admixture being at least 20% by weight of the comminuted oats.
(a) admixing comminuted oats with an organic solvent, said solvent being selected from the group consisting of pentane, hexane, heptane, cyclohexane and alcohols of 1-4 carbon atoms, and mixtures thereof, and (b) separating substantially gum-free flour from the admixture of comminuted oats and solvent, the amount of flour separated from the admixture being at least 20% by weight of the comminuted oats.
2. The process of Claim 1 in which the oats are de-oiled in step (a) prior to separation of substantially gum-free flour.
3. The process of Claim 2 in which the comminuted oats are comminuted dehulled oats.
4. The process of Claim 3 in which the separation of the gum-free flour from the admixture is carried out as a batch operation.
5. The process of Claim 3 in which the separation of the gum-free flour from the admixture is carried out as a contin-uous operation.
6. me process of any one of Claim 1, Claim 3 and Claim 5 in which the solvent is selected from the group consisting of pentane, hexane, heptane and cyclohexane, and mixtures thereof.
7. The process of Claim 5 in which the gum-free fb ur is essentially free of bran.
8. A process for the separation of a substantially gum-free flour from oats, said process comprising:
(a) admixing comminuted oats with an organic solvent, said solvent being selected from the group consisting of pentane, hexane, heptane, cyclohexane and alcohols of 1-4 carbon atoms, and mixtures thereof, and (b) separating the admixture of comminuted oats and solvent into at least two fractions, one fraction having bran as a substantial part of the solid component and a second fraction having substantially gum-free flour as the major solid component, the amount of flour separated from the admixture being at least 20% by weight of the comminuted oats.
(a) admixing comminuted oats with an organic solvent, said solvent being selected from the group consisting of pentane, hexane, heptane, cyclohexane and alcohols of 1-4 carbon atoms, and mixtures thereof, and (b) separating the admixture of comminuted oats and solvent into at least two fractions, one fraction having bran as a substantial part of the solid component and a second fraction having substantially gum-free flour as the major solid component, the amount of flour separated from the admixture being at least 20% by weight of the comminuted oats.
9. me process of Claim 8 in which the comminuted oats are comminuted dehulled oats.
10. The process of Claim 9 in which the oats are de-oiled in step (a) prior to separating the admixture.
11. The process of Claim 10 in which the solvent is selected from the group consisting of pentane, hexane, heptane, and cyclohexane, and mixtures thereof.
12. The process of Claim 11 in which the second frac-tion is substantially free of bran.
13. The process of Claim 12 in which one or more of bran, gum-free flour and oat oil are separately recovered in an essentially solvent-free form.
14. The process of Claim 13 in which bran is recovered and in which the bran is subjected to further comminution, re-admixed with solvent and a further separation into fractions hav-ing a bran as a substantial solid component and having gum-free flour as the major solid component is carried out.
15. The process of Claim 8 in which the admixture of comminuted oats and solvent is separated into at least two frac-tions and such separation is accomplished by sieving the admixture through a sieve capable of retaining substantially all of the bran on the mesh of the sieve and capable of passing solvent con-taining said gum-free flour.
16. The process of Claim 15 in which the comminuted oats are comminuted dehulled oats and the oats are de-oiled in step (a) prior to separation of the admixture into at least two fractions.
17. The process of Claim 16 in which the solvent is selected from the group consisting of pentane, hexane, heptane and cyclohexane, and mixtures thereof.
18. The process of Claim 17 in which the bran is sub jected to further comminution, re-admixed with solvent and a fur-ther separation into fractions having a bran as a substantial solid component and having gum-free flour as the major solid com-ponent is carried out.
19. The process of Claim 17 in which one or more of bran, gum-free flour and oat oil are separately recovered in an essentially solvent-free form.
20. The process of Claim 10 in which the comminuted oats and solvent are admixed under controlled conditions, said controlled conditions being adapted to cause a non-uniform dis-tribution of the comminuted oats in the solvent.
21. The process of Claim 20 in which the solvent is selected from the group consisting of pentane, hexane, heptane, and cyclohexane, and mixtures thereof.
22. The process of Claim 21 in which the controlled conditions include cessation of mixing immediately prior to separation of the fractions.
23. The process of Claim 22 in which, immediately after cessation of mixing, additional solvent is added to the admixture so as to facilitate separation of the fractions.
24. The process of Claim 21 in which additional solvent is continuously added to the admixture and the gum-free flour is continuously separated form the admixture.
25. The process of Claim 21 in which the bran is separated from the solvent, subjected to further comminution, re-admixed with solvent and separated into a fraction having substantially gum-free flour as the major solid component and another fraction.
26. The process of any one of Claim 1, Claim 8 and Claim 15 in which the comminuted oats are obtained from de-hulled oats using a pin-mill.
27. The process of any one of Claim 1, Claim 8 and Claim 15 in which the comminuted oats are obtained from de-hulled oats using a hammer-mill.
28. The process of any one of Claim 1, Claim 8 and Claim 15 in which the comminuted oats are obtained from de-hulled oats using corrugated rollers.
29. The process of any one of Claim 1, Claim 8 and Claim 15 in which the solvent is hexane.
30. The process of Claim 1 followed by an additional step comprising separating a protein-rich fraction from the gum-free flour.
31. The process of Claim 11 followed by an additional step comprising separating a protein-rich fraction from the gum-free flour.
32. The process of Claim 14 followed by an additional step comprising separating a protein-rich fraction from the gum-free flour.
33. The process of Claim 17 followed by an additional step comprising separating a protein-rich fraction from the gum-free flour.
34. The process of Claim 24 followed by an additional step comprising separating a protein-rich fraction from the gum-free flour.
35. The process of Claim 1 followed by an additional step comprising separating an acid-soluble protein fraction from the gum-free flour.
36. The process of Claim 11 followed by an additional step comprising separating an acid-soluble protein fraction from the gum-free flour.
37. The process of Claim 17 followed by an additional step comprising separating an acid-soluble protein fraction from the gum-free flour.
38. The process of Claim 21 followed by an additional step comprising separating an acid-soluble protein fraction from the gum-free flour.
39. The process of Claim 11 followed by an additional step comprising separating a starch fraction from the gum-free flour.
40. The process of Claim 11 followed by an additional step comprising separating gum from the bran fraction.
41. The process of Claim 14 followed by an additional step comprising separating gum from the bran.
42. me process of Claim 17 followed by an additional step comprising separating gum from the bran fraction.
43. me process of Claim 21 followed by an additional step comprising separating gum from the bran fraction.
44. The process of Claim 38 in which said separation of an acid-soluble protein fraction comprises admixing the gum-free flour with an aqueous acidic solution, separating undissolved solid matter from said aqueous solution and re-covering soluble protein from the solution.
45. The process of Claim 44 in which the protein is recovered from said solution by freeze drying the solution.
46. The process of Claim 44 in which the protein is recovered from said solution by isoelectric precipitation of the protein.
47. The process of Claim 45 in which the aqueous acidic solution is a dilute solution of an acid selected from the group consisting of hydrochloric acid and phosphoric acid.
48. The process of Claim 46 in which the aqueous acidic solution is a dilute solution of an acid selected from the group consisting of hydrochloric acid and phosphoric acid.
49. me process of Claim 41 in which the gum is separated from the bran by admixing said bran with water, separating the bran from the water and recovering gum from the water.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB25804/75 | 1975-06-17 | ||
| GB25804/75A GB1527101A (en) | 1975-06-17 | 1975-06-17 | Process for the treatment of comminuted oats |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1087451A true CA1087451A (en) | 1980-10-14 |
Family
ID=10233586
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA254,864A Expired CA1087451A (en) | 1975-06-17 | 1976-06-15 | Process for the treatment of comminuted oats |
Country Status (7)
| Country | Link |
|---|---|
| JP (1) | JPS521048A (en) |
| AU (1) | AU496745B2 (en) |
| CA (1) | CA1087451A (en) |
| DE (1) | DE2627137A1 (en) |
| FR (1) | FR2314672A1 (en) |
| GB (1) | GB1527101A (en) |
| SE (1) | SE7606863L (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1552012A (en) * | 1975-12-16 | 1979-09-05 | Du Pont Canada | Process for the treatment of comminuted oats |
| US4464402A (en) * | 1978-04-24 | 1984-08-07 | F.I.N.D. Research Corporation | Process for manufacturing a high protein food material |
| JPS60184756A (en) * | 1984-02-29 | 1985-09-20 | Suzuki Motor Co Ltd | V-belt type automatic transmission |
| US5026548A (en) * | 1987-04-28 | 1991-06-25 | Cadbury Schweppes Plc | Surfactant |
| GB8710041D0 (en) * | 1987-04-28 | 1987-06-03 | Cadbury Schweppes Plc | Viscosity reducing agent |
| US6113908A (en) * | 1999-03-22 | 2000-09-05 | Her Majesty The Queen In Right Of Canada, As Represented By The Minister Of Agriculture | Methods for processing oat groats and products thereof |
| JP4868646B2 (en) | 1999-05-06 | 2012-02-01 | シープロ・インコーポレイテッド | Oat extract: purification, composition and method of use |
| WO2002015843A2 (en) * | 2000-08-23 | 2002-02-28 | Sergey Petrovich Semenov | Agent for regulating lipidic metabolism and method for producing said agent |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3519431A (en) * | 1966-06-13 | 1970-07-07 | Truman B Wayne | Milling of cereal grains and processing of products derived therefrom |
| US3615655A (en) * | 1967-07-19 | 1971-10-26 | Cpc International Inc | Method for preparing high protein cereal grain product |
-
1975
- 1975-06-17 GB GB25804/75A patent/GB1527101A/en not_active Expired
-
1976
- 1976-06-11 AU AU14812/76A patent/AU496745B2/en not_active Expired
- 1976-06-15 CA CA254,864A patent/CA1087451A/en not_active Expired
- 1976-06-16 SE SE7606863A patent/SE7606863L/en not_active Application Discontinuation
- 1976-06-16 FR FR7618237A patent/FR2314672A1/en active Granted
- 1976-06-16 DE DE19762627137 patent/DE2627137A1/en not_active Withdrawn
- 1976-06-17 JP JP51070454A patent/JPS521048A/en active Pending
Also Published As
| Publication number | Publication date |
|---|---|
| FR2314672B1 (en) | 1981-08-07 |
| GB1527101A (en) | 1978-10-04 |
| AU496745B2 (en) | 1978-10-26 |
| AU1481276A (en) | 1977-12-15 |
| SE7606863L (en) | 1976-12-18 |
| FR2314672A1 (en) | 1977-01-14 |
| JPS521048A (en) | 1977-01-06 |
| DE2627137A1 (en) | 1976-12-30 |
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| Date | Code | Title | Description |
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| MKEX | Expiry |