Note: Descriptions are shown in the official language in which they were submitted.
~9~97
; The present invention relates to a process for the
treatment of proteinaceous material so as to effect separation
of the comminuted proteinaceous material into fractions differing
in composition. In particular, the present invention relates
to the treatment of comminuted proteinaceous material so as to
separate fractions differing in protein content and/or to separate
the comminuted proteinaceous material into an endosperm fraction,
and "outer coat" fraction and an oil.
As used herein proteinaceous material is defined as
wheat, rye, barley, triticale, peas, beans and buckwheat. Theouter coat of the cereal grains viz. wheat, rye, barley and tri-
ticale is also known as bran, such bran may have endosperm
attached thereto, whereas the outer coat of peas, beans and buck-
wheat is also known as the seed coat. The endosperm of peas and
beans is also known as the cotyledon. For the cereal grains and
buckwheat the endosperm may include the germ. The expression
"gum" used herein refers in particular to water-soluble gums, if
present in the particular proteinaceous material.
The proteinaceous materials are a potential source
of a wide variety of useful products. Examples of such products
are flour, starch, protein-enriched and protein-depleted prod-
ucts, bran, gum and oil, depending on the particular protein-
aceous material. Traditional techniques used in the food pro-
cessing industry if available, for the treatment of proteinaceous
material so as to effect the separation of the proteinaceous
material into fractions of differing composition are capable of
improvement, for example with respect to energy requirements,
potential pollution problems and the taste and/or colour of
products. In other instances techniques may not be available
for the conversion of the proteinaceous material into commer-
cially viable products for example products of increased protein
content.
--1--
109S897
Processes for the separation of a variety of products
from comminuted oats are disclosed in Canadian Application No.
; 245,163 of A. Bell, J.R.B. Boocock and R.W. Oughton, filed
February 4, 1976 and in Canadian Application No. 254,864 of
R.W. Oughton, filed June 15, 1976. A process for isolating
protein from a pulverized oil seed using liquid fluorocarbons is
disclosed in U.S. Patent 3,869,438 of J.W. Finley et al, which
issued March 4, 1975. The density separation of protein and car-
bohydrates from wheat flour, soybeans, green peas and dried
acid whey using a non-aqueous solvent system is described by
J.W. Finley in Journal of Food Science, 41, 882-885 (1976).
Processes for the solvent-extractive milling of maize or corn,
wheat, rye and the sorghum grains to remove the bran coat from
whole kernels of such grains followed by comminution of the
whole milled kernels and for the separation of so-called fibrous,
proteinaceous, endosperm and/or starch fractions derived from
such grains are disclosed by T.B. Wayne in Canadian Patents
864,538, which issued February 23, 1971, and 905,909 and 905,910,
both of which issued July 25, 1972.
A need exists for a process for the treatment of
comminuted proteinaceous materials, so as to effect the sep-
aration of fractions of differing composition.
A process for the separation of fractions differing in
composition from proteinaceous materials has now been found.
Accordingly the present invention provides a process
for the separation of proteinaceous material into at least two
fractions, the proteinaceous material being selected from the
group consisting of wheat, rye, barley, triticale, peas, beans
and buckwheat, said process comprising:
: ~095~j?
..
(a) admixing comminuted proteinaceous material 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 protein-
aceous material and solvent into at least two fractions, one
. fraction having outer coat of the proteinaceous material as a
substantial part of the solid component and a second fraction
having endosperm as the major solid component, the amount of
endosperm separated being at least 5~ of the comminuted protein-
aceous material.
The present invention also provides a process for the
separation of comminuted proteinaceous material into frac~ions
differing in composition, the proteinaceous material being
selected from the group consisting of wheat, rye, barley, tri-
ticale, peas, beans and buckwheat, said process comprising:
(a) admixing comminuted proteinaceous material 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;
(b) forming a slurry of said admixture of comminuted
: proteinaceous material and solvent; and
(c) subjecting the slurry to the influence of cen-
trifugal force and thereby separating the comminuted protein-
! aceous material in said slurry into at least two ~ractions, said
fractions differing in composition~
In addition the present invention provides a processfor the separation of comminuted proteinaceous material into
fractions differing in composition, the prot~inac20us material
being selected from the group consisting of wheat, rye, barley,
triticale, peas, beans and buckwheat, said process comprising:
l~gS897
ta) admixing a proteinaceous fraction, derived from
said comminuted proteinaceous material, 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;
(b) forming a slurry of said admixture of proteinaceous
fraction and organic solvent; and
(c) subjecting the slurry to the influence of cen-
trifugal force and thereby separating said proteinaceous fraction
into at least two fractions, said fractions differing in protein
content.
Furthermore the present invention provides a process
for the separation of comminuted proteinaceous material into
fractions differing in composition, the proteinaceous material
being selected from the group consisting of wheat, rye, barley,
triticale, peas, beans and buckwheat, said process comprising:
(a) admixing a proteinaceous fraction, d~rived from
said comminuted proteinaceous material, 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;
(b) subjecting said admixture to the influence of
centrifugal force in a centrifuge and thereby forming a centri-
fuge cake of said proteinaceous fraction, and
(c) separating said cake in the substantial absence of
said solvent into at least two layers, the protein content of
at least one of said layers being different from the protein
content of at least one of said other layers.
In the process of the present invention the protein-
aceous materials that are cereal grains or buckwheat are prefer-
ably dehulled, if necessary, prior to comminution. Techniques
109589'7
for dehulling cereal grains and buckwheat are known. In
addition peas and beans should be separated from their pods.
The proteinaceous materials are comminuted in order to facili-
tate extraction of any oil and to facilitate separation of a
subsequently formed admixture of comminuted proteinaceous
material and solvent into fractions differing in composition.
The particle size of the comminuted proteinaceous material will
depend in particular on the technique to be used to separate the
comminuted proteinaceous material in the admixture into fractions
and may affect the segregation of protein in the material. For
example, if a hydrocyclone is used to separate the proteinaceous
material into fractions, the particle size of the comminuted
proteinaceous material must be sufficiently small to allow the
hydrocyclone to operate smoothly and efficiently and without
plugging of the hydrocyclone. Conventional techniques, for
example, pinmilling, hammer milling and other shearing techniques
would appear to produce an acceptable comminuted proteinaceous
material, the preferred techniques depending in particular on
the actual separation techniques to be used.
In the process of the present invention the comminuted
proteinaceous material is admixed with an organic solvent,
especially an organic solvent for any oil that may be in the
proteinaceous material. Such admixing facilitates extraction of
oil, if present, in the proteinaceous material. The solvents
used must be acceptable for use with foodstuffs, e.g. be non-
toxic at the levels remaining in the products subsequently pro-
duced, not cause the formation of toxic materials in the product
and not have a significant deleterious effect on the nutritional
value of the product, and must be capable of permitting separa-
tion of the fractions. The amount and type of solvent remaining
in products offered for sale must be acceptable to the appropriate
l~g5~9~
health authorities, as will be understood by those skilled in
- the art. Examples of solvents are pentane, hexane, heptane,
cyclohexane and alcohols of 1-4 carbon atoms, and mixtures
thereof; as used herein the solvents 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.
In the process of the present invention the comminuted
proteinaceous material is admixed with the organic solvent e.g.
hexane. Such admixing is preferably carried out with agitation
e.g. stirring and may be so as to form a slurry. If oil is
present in the proteinaceous material the total period of time
during which the comminuted proteinaceous material and hexane
are admixed should be such that the desired degree of extraction
of any oil from the comminuted proteinaceous material is
achieved, the period of time being dependent in part on the
actual technique of extraction. Generally a slurry of com-
minuted proteinaceous material and hexane will be used.
The separation of the fractions of proteinaceous
" material may be carried out by one or more embodiments of the
process of the present invention. The preferred embodiment will
depend in particular on the particular proteinaceous material
and on the desired products.
In one embodiment the admixture of comminuted protein-
aceous material and hexane is thoroughly mixed using for
example a stirrer. The admixing may then be adjusted to effect
separation of fractions of the proteinaceous material. For
example if mixing is discontinued one fraction, which contains
the outer coat i.e. bran if the proteinaceous material is a
cereal grain or buckwheat, tends to settle significantly faster
than a second fraction comprised of endosperm. Separation may
i~95~g~
be effected by for example decantation. ~hen such a separation
is used it is preferable to repeat the separation one or more
times, optionally subjecting the outer coat fraction to
further comminution to aid in the separation of any endosperm
adhered to the outer coat. Alternatively a separation may be
effected by sieving the admixture. The mesh size of the sieve
will depend primarily on the degree of separation desired.
Preferably a sieve having a fine mesh e.g. 200 or finer, is
used. The outer coat fraction will tend to be retained on
the sieve and may be used as such or, especially if the outer
coat is bran, subjected to further comminution and subsequent
further separation into fractions. The endosperm fraction
tends to pass through the sieve.
In another embodiment the stirring of the admixture
of comminuted proteinaceous material and hexane is controlled
so that the separation of the co~minuted proteinaceous material
into fractions occurs _ situ i.e., a non-uniform distribution
of the proteinaceous material occurs in the admixture.
Separation of one fraction from the admixture may be effected
by adding additional solvent, preferably in a continuous manner,
and removing, preferably simultaneously removing, a fraction
of the comminution proteinaceous material in hexane. The
fraction separated is preferably a fraction comprised of
endosperm. It may be desirable to sieve the fraction being
separated so as to remove any oversize particles therefrom.
The fraction not separated from the admixture and~or any
oversize particles removed from the fractions being separated
may be subjected to further comminution and subsequently further
separation.
In a fuxther embodiment the admixture of comminuted
proteinaceous material and hexane is admixed in the form of a
9~
slurry and then subjected to the influence of centrifugal force.
The means used to subject the slurry to centrifugal force is
a centrifugal separator, preferably a centrifugal separator
capable of being operated on a continuous or semi-continuous
basis. Examples of centrifugal separators are continuous
centrifuges, including semi-continuous centrifuges, ana hydro-
cyclones.
In order to effect separation of a slurry of comminuted
proteinaceous material and hexane into fractions in a hydro-
cyclone, the slurry is fed to the hydrocyclone whereupon theslurry is subjected to centrifugal force and fractionation of
the comminuted proteinaceous material in the slurry tends to
occur. The operation of a hydrocyclone so as to obtain a
desired fractionation of the comminuted proteinaceous material
in the slurry will depend on a number of process variables,
as will be understood by those skilled in the art. Examples
of such variables are degree of comminution of the proteinaceous
material, the amount of solid material in the slurry, the
pressure drop across the hydrocyclone, the ratio of the flows
through the so-called "underflow" and "overflow" outlets, the
solvent and the like. The operation of the hydrocyclone is
adjusted so that a desired fractionation is obtained.
While the present invention has been described herein-
before with particular reference to the separation of comminuted
proteinaceous material into fractions thereof, the present in-
vention is not limited thereto. In a preferred embodiment,
particularly with respect to the use of centrifugal force,
the material which is subjected to separation is a proteinaceous
fraction derived from proteinaceous material by means described
herein or by other means known in the art. In particular
the material subjected to the influence of centrifuga3 force
is a proteinaceous fraction that has been obtained by classi-
109~i89~
fying an admixture of comminuted proteinaceous material andhexane e.g. by sieving, decanting and the like as described
hereinabove.
In general in the embodiments of the present invention,
the fractions obtained will comprise at least 5%, and preferably
at least 20%, of the comminuted proteinaceous material or of
the proteinaceous fraction derived therefrom.
The use of the influence of centrifugal force on
proteinaceous fractions derived from comminuted proteinaceous
material, rather than on the comminuted material per se, may be
advantageGus in that process problems associated with large
particles e.g. the clogging of hydrocyclones, may be reduced
or avoided. In particular endosperm fractions may be subjected
to the influence of centrifugal force in a continuous centrifuge
or hydrocyclone. Proteinaceous fractions, especially endosperm
fractions, may be subjected to single or multiple treatments
under the influence of centrifugal forces to produce a variety
of products, especially products of varying pxotein content.
In a particular embodiment of the process of the
present invention, an endosperm fraction is subjected to the
influence of centrifugal force in a centrifuge. After
separation of the solvent, e.g. hexane, the cake of solid
material obtained may be selectively split into fractions of
differing protein content. Techniques for the selective
splitting of a centrifuge cake into fractions are known. For
example a basket centrifuge may be used as the centrifuge and
the fractions may be split out of the basket using a knife
blade, as is known for basket centrifuges.
In the process of the present invention it is pre-
ferred that water not be added to the admixtures of comminuted
proteinaceous material, or fractions derived therefrom, and
solvent. As exemplified hereinafter, the addition of water
_g_
1~9S897
may actually adversely affect the separation of the fractions~
Although water is preferably not added to the admixtures, it
is not necessary to remove water naturally present in the
proteinaceous material.
The proteinaceous material in the fractions separated
according to the present invention may be separated from the
solvent miscella by known techniques e.g. by the use of a cen-
trifuge. Any oil in the solvent may also be recovered.
In a preferred embodiment of the process of the
present invention the cereal grains, especially wheat, rye and
triticale, have a hardness of less than 50. Hardness is defined
as the time in seconds to pass 20 g of material through a 28
mesh TYLER screen in a WILEY mill. The measurement of hard-
ness is discussed in greater detail in "Wheat Quality Evaluation
Part I Accuracy and Precision of Prediction Tests", I.A. de la
Roche and D.B. Fowler, Can. J. Plant Sci. 55 241-240, January
1975. The hardness numbers obtained for some cereal grains
are given in Table I hereinafter.
The endosperm fraction, which may be referred to as
flour, that is separated according to the process of the present
invention is essentially free of any oil in the proteinaceous
material. The products of the process of the present invention
are believed to be useful in the food industry either as such
or as a source of other products. For example flour or endo-
sperm fractions are capable of being used as such or when
enriched with protein as nutritional fortifiers in foods, in
cereals, baby foods, cakes and the like; the particular end-use
will depend to a significant extent on the particular protein-
aceous material from which the fraction is derived. For example
fractions derived from barley may be particularly useful in baby
foods and those from buckwheat in oriental foods. Fractions
* denotes trade mark
--10--
IO~S897
derived from peas and beans are significantly de-coloured in
the process of the present invention and may be particularly
useful as nitritional fortifiers. Fractions derived from rye
are characterized by the substantial absence of the taste
associated with that cereal grain. The process of the present
invention is capable of increasing the protein content of in
particular low protein wheat thereby rendering such wheat
!i useful in end-uses otherwise requiring a wheat of higher
natural protein content. Starchy materials i.e. endosperm
fractions of low protein content, especially from wheat, may be
useful in pastries and in known uses for starches. The oils
obtained are useful in a variety of end uses for example as
vegetable oils.
The present invention is illustrated by the following
examples. In the examples the protein content is Kjeldahl
nitrogen content times 6.25.
EXAMPLE I
A proteinaceous material was comminuted, in sequence,
on a knife mill and a pin mill to produce a finely ground
; 20 material. 150 g of the finely ground material was admixed in
the form of a slurry with 300 g of hexane for 5 minutes. The
slurry was then sieved with a 200 mesh TYLER screen. The
material retained on the screen was re-admixed with 150 g of
hexane for 5 minutes and re-sieved through the 200 mesh screen.
The oversized material thus obtained, i.e. that retained in the
screen was dried in a vacuum oven and analyzed for protein.
The undersized material i.e. that passing through
the screen in each instance, was combined and centrifuged for 10
minutes at 1000 G. The hexane miscella was decanted off and a
composite sample of the solid material was analyzed for protein.
The remaining solid material was re-admixed, as a slurry, with
75 g of hexane, poured into a 43 x 123 mm extraction
1~9589~
thimble supported ln a 2~0 ml centri~uge cup and centri~uged at
1000 G for 10 minutes. The hexane ~as decanted off. me
thimble ~ras cut open, the depth of the centrifu~e cake obtained
was measured and a thin layer was taken ~rom the top, middle
and bottom sect~ons of the cake for protein analysis. All
protein analysis were carried out on dried samples using a
KJel-Foss Auto~atic 16210 protein analyzer.
The oil from the hexane miscella was reco~ered us~n~ a
rotary evaporator.
Details o~ the proteinaceous materials used and the
results obtained are given in Table I. In each case the colour
of the centrifuge cake of undersized ~aterial ~,las white.
109~
.............
~ ~ ~ ~ ~ ~Q O a) I~ O ~ CJ tr) o~
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,. ~ ~
~ _
u~ ~ a
~ ~ ~ --I C`J ~l
~q O
h ~ ~ ~) ~ ~ ~ ~ N ~l 1~ l~ ~o a~
Q CU~ O ~ O c0
F~ ~ ~D ~ r~ ~1 <~J C~l N ~f ) ~J C l N t
3 ~ ~ o ~ ~ ~ ~ ~ o o o ~ ~ o
C~ ~ _
u~ ~ o ~ ~ ~ a~ ~ o ~ ~ u~
a),_.............
O O O r-l ~ N ~ ~ C~J O
ct h
_~ ~ ~ O ~ C- O
~; ~ ~ a~ r.CJ __ ~Qr-l ~ 0
~ Cq ~
N
h --`~1r-l ~ N) CJ ~ CO_ CU 0C3 h~ t--
:~ ~ ~D 0 O~ ~O O ~ C5~ ~ 0
D ~2 _ ~1 ~1 ~ ~1 _i
OC~ O~O ~0 ~1~1 0 0
~ ~ ~D .. . . .. . . . . . .
o ~2 _ ~1 ~'1r-~~ CU~J N~1~Ir1~I C. C`J C`J
~ ~~ 0 ~ ~ a~ ~ ~ ~ o a~
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~ ~ ¢ m ~ ' H )~ Z
Zl
r<
P; ~ c~l ~r) ~ 1~ ~ ~ CC C'~ O C~ ~
-13 -
~ 95897
.
TA9LE I (contlnued)
* A ....... ~ield peas (pisum sativum)
..... horse beans (vicia faba)
C ...... na~y beans (phaseoulus vulgzris)
D ...... bucXwheat (not dehulled)
E ...... buckwheat (dehulled)
F ...... barley (not dehulled)
: G ...... barley (dehulled)
~ ....... rye (puma), hardness = 44.1
I ...... trit~cale (rosner), hardness = 47.8
J ...... Fredrick so~t white winter wheat,
hardness = 37.0
E ...... Opal utility spring wheat,
hardness = 61.5
L ...... Neepat~ hard red spring wheat,
hardness = 55.0
; ~ ...... Glenlea spring ut~lity wheat,
hardness = 66.1
- N ...... Cal-15 sprin~ utility wheat,
hardness = 44.8
'
:
:
-14-
1~9~89~
EXA~E II
25 g o~ a co~minuted proteinaceous material were
admixed with 75 g of hexane in a ~iARI~ * blender ~or 10 minutes.
The admlxture thus obtained was poured into a bea~-er, stirred
thoroughly and the liquid fraction containing suspended solids
was decanted off, the hea~J non-suspended solids (residue)
being retained in the beaker. The liquid ~ractlon was centri-
uged at 1000 G for 5 minutes using an extraction th~mble in the
centri~uge cup. The thimble was then cut open and composite
analytlcal-size samples were taken from the top and bottom of
the centrifuge cake obtained. ~fter drying protein analyses were
carried out on the top and bottom sæmples ænd on tne residue.
Deta~ls of the proteinaceous ~æterials and the results
obtained are gl~en in Table II.
In all cases the hexane mlscella obtained was ~Jello~
in colour and the solid samples were off-white.
TABLE II
Protein Content
Proteinaceous of Centrifuged Protein Conten4
Material Samples (~ ?~ es~due (~)
Pxotein~
Type Content(~) TopBottom
~orse Beans 26.3 47.621.7 2~.6
Field Peas 27.1 42.026.7 26.3
(~hole)
Field Peas 21.7 48.514.7 21.7
(split)
EXAMPLE I~
A proteinaceous material ~s coarsel-J ground and then
30- finely ground usin~ a pinmill. A 15 g sa~ple of the co~inuted
proteinaceous ma~exial thus obtained was de-oiled with he:ane
in a So~hle~ extracvion apparatus for one QOUr. T.h.e de-o~led
~terial was a~iYed ~Jith 15 ~ of hexane ~n a TT.~I~,C- blender
* denotes trade ~arli -15-
lO9S89~
for 15 minutes, poured into a bea~er and thoroughly stirred.
The liquid fraction, containing suspended solids, ~as de-
canted off, the heavy non-suspended solids (residue) being
retained in the beaker. ~he liquid fraction W2S centrlfuged at
1000 G for approximately fi~e minutes usin~ an extraction
thimble in the centrifuge cup. me thimble was then cut open
and composite anal~tical-size samples were taken fro~ the top,
middle and bottom sections of the centrifuge ca~e obtained.
- After drying protein analyses ~Jere carried out on the top,
1~ middle and botto~ samples and on the residue.
The abo~e procedure was repeated except that in
separate experiments water in an aL~ount equal to a~proximately
30~ or 100~ of the weight of protein and fibre in the co~minuted
proteinaceous ~aterial was added to the hexane in the ~rA.~IiiG
blender.
Details of the proteinaceous materials and the results
obtained are given in ~able III.
-16-
lOg5897
o ~ u~ ~ t-'o ~
. - - . . - . -
0 c>
~o~
h C~
P~ O
~ O ~ ~ C~J~i CO
_ O ~ . . - .. ..
C~
o~
O
~ ~ Q~ 0
0 v~ ~1 ~ O ~ ~J rl
oc~ ao
~: 'a ~ O N<~ C0 ~ ~ICU CU
L~ C~ ~0 .~3
O ~ ~, * -* *
a~ o ~ ~ ~1 ~1 0 ~ O
~ V & r~
H ¦
o~ 0oo 0oo 0ooc~oo
¢ ~o ~o ~o ~o
3~ ~
~ ~ ~ .
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c) a~ '`
t, ~ C~
s~ ~o
01 ~ C)
o
4,
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a)
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G~ X
o P s~
*
--17 -
~g~
EXUIPLE IV
The procedure of ~xample I was repeated on na~y be~ns
except th~t ~ethanol ~taS used as solvent. The resul~s ~;Tere
as follows:
Proteinaceous ~aterial
Protein Content (~) 24.8
Crude Oil* Wt. (g) 4.8
OYersized Sam~le
Wt. (g) 102
Protein Content ($) 24.8
Composite Sample
Protein Content (~) 21.6
Cake Depth (~m) 43
Undersized Sample
Protein Content (~)
Top 51.4
Middle 12.7
Bottom 18~9
* met,hl~nol-eoluble ~raction
E~IE V
e pro~edure of Example I was repeated except tha~
the 150 g of finely ground proteinaceous mater~ai were ædm~;:e8
ln the ~orm o~ a slurry with 300 g o~ hexane in a I~Jh~ G*
blender. me adm~xing in the ~ARING ble~der was carried out
~or 5 m~nutes and the slurr~ ~hus obtalned was subse~u~n~y
treated as in Example I.
Deta~s of the proteinaceous mater~als used and the
results obtained were as follows:
Protein~ceous ~terial
Iype** D J N
Protein Content (%) 1~.4 9.0 16.1
0~1 ~Jt. (g) 3.7 1.9 2.1
O~ersized Sample
~t- (g) 93 ~9 70
Protein Content (~) 10.6 12.4 16.5
- -18-
1095897
Composite Sample D J N
Protein Content (%) 16.9 8.9 15.3
Cake Depth (mm) 46 60 55
Undersized Sample
Protein Content (%)
Top 39.2 37.9 47.4
Middle 16.4 6.5 10.5
Bottom 7.4 7.4 11.7
** See Example I
The analyses of the "top" samples of this Example
and of Example I indicate the effect of the high speed agitation
in the WARING blender on protein content of fractions.
EXAMPLE VI
A sample of proteinaceous material was admixed at
ambient temperature with 400 ml of hexane in a vertical glass
cylinder measuring 40 cm in height and 6 cm in diameter. The
admixture was vigorously agitated for 30 minutes. The agitation
was then decreased, thereby causing non-uniform distribution
of the proteinaceous material in the hexane, and a major portion
, 20 of the hexane solution was siphoned off and sieved with a 325
mesh TYLER screen. Any oversized material retained on the
screen was returned to the cylinder.
The above procedure was repeated two times, 400 ml of
hexane being added to the cylinder each time.
The oversized material remaining in the cylinder after
completion of the above was dried and analysed for protein
content. The solutions of undersized material i.e. that passing
through the screen on each occasion, were combined and cen-
trifuged. The hexane miscella was decanted off and the under-
sized material thus obtained was dried and analysed for proteincontent. The hexane was evaporated from the hexane miscella
so as to obtain the oil.
--19--
1~95~9~
All protein ~nalyses were made using a macro-scale
K~eldahl method.
Details of the proteinaceous ~aterials and the results
obtained were as follo-.7s:
Run 1 2 3 4
Proteinaceous Material
Ty~e* A B C D E
Weight (g) 90.0 94-3 88.1 93.~ 91.8
Protein Content(~ .4 11.1 11.3 12.6 12.9
O~ersized ~aterial**
Weight (g) 71.6 52.2 55.8 64.o 73-3
Protein Content(O15.1 12.7 13.8 13.2 11.3
Undersized ~ateriæl
T,~eight (g) 6.2 28.1 27.1 20.1 12.2
Protein Content(~)20.5 10.3 8.6 14.1 13.2
Oil
Weight (g) 1.6 1.3 1.0 1.6 1.5
* A ....... Selkirk hard red spring ~rheat
B ...... Fredrick soft winter wheat
C ...... Tetra Petkus winter ~e
D ...... Vanier barley
E ...... a hull-less ba.ley
** in all runs the oversized material was Duff in colour ~nd
the undersized materi21 Yas ~rhi~e. ~ne o-~ersi~ed ~æterial
comprised bran and endosperm.
EXA~IPI2 r~rII
Approximately 3500 g of pin~illed Fredr~c~ winter
wheat were admixed, in the form of a sl~rry, with 15.9 litres
o~ hexane for 10 minutes at a~bient tempera~ure. The resultan~
adm~xture was sieved using a S',~ECO* Vi~ro Energ~ Separator
e~uip~ed with a 325 mesh TYL2R screen. The oversized 2~ter~al
(bran) i.e. that retained on the screen, wæs dried ~n a rotary
~acuum drier ænd analyzed ~or protein content.
The undersized materiæl (~10UL~) i.e. that pa~s'ng
through the screen, ~as agitated so as to form 3 Sl u~ry and
* denotes trade mark
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10~97
pumped through a 10 mm DORR-OLIVER DOXIE TYPE A* hydrocyclone
at an inlet pressure of 2.8 kg/cm2. The overflow fraction was
centrifuged to separate the solid material from the hexane
miscella and the solid material obtained is referred to below
as "First Overflow Solids". The underflow fraction from the
hydrocyclone was passed through the hydrocyclone again at an
inlet pressure of 2.8 kg/cm2. The overflow and underflow
fractions thus obtained were separately centrifuged to separate
the solid material from hexane miscella and the solid materials
obtained are referred to below as "Second Overflow Solids" and
"Underflow Solids" respectively. All the solids were dried in
a rotary vacuum drier and analysed for protein content.
The oil was recovered from the combined hexane miscella
All protein anaylses were carried out on a Kjel-Foss
Automatic 16210 protein analyzer.
The results obtained were as follows:
Weight Protein Content Colour
(g) (%)
Starting Material 3500 9.5
First Overflow Solids13.2 43.2 white
Second Overflow Solids** 382.3 13.~ white
Underflow Solids**955.5 5.1 white
Oversized Material1840 12.1 buff
Oil 40.7 yellow-
green
** The residual oil in the products, as determined by a hot
Soxhlet extraction using hexane as solvent, was 0.1~ for the
Second Overflow Solids and 0.05~ in the Underflow Solids.
The application is a division of copending Application
Serial No. 267 784, filed December 14, 1976.
* denotes trade mark
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