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Patent 1177323 Summary

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(12) Patent: (11) CA 1177323
(21) Application Number: 397327
(54) English Title: SUNFLOWER BUTTER SPREAD AND PRODUCTS THEREOF INCLUDING A PRETREATMENT OF THE SUNFLOWER SEEDS AND THE LIKE
(54) French Title: MARGARINE D'HUILE DE TOURNESOL ET PROCEDE DE PRETRAITEMENT DES GRAINES DE TOURNESOL
Status: Expired
Bibliographic Data
(52) Canadian Patent Classification (CPC):
  • 99/159
(51) International Patent Classification (IPC):
  • A23L 25/00 (2016.01)
(72) Inventors :
  • MACDONALD, BRUCE E. (Canada)
  • GALLOWAY, GEOFFREY (Canada)
  • KAKUDA, YUKIO (Canada)
(73) Owners :
  • CSP FOODS LTD. (Not Available)
(71) Applicants :
(74) Agent: ADE & COMPANY
(74) Associate agent:
(45) Issued: 1984-11-06
(22) Filed Date: 1982-03-01
Availability of licence: N/A
(25) Language of filing: English

Patent Cooperation Treaty (PCT): No

(30) Application Priority Data:
Application No. Country/Territory Date
8106819 United Kingdom 1981-03-04

Abstracts

English Abstract





SUNFLOWER BUTTER SPREAD AND PRODUCTS THEREOF INCLUDING
A PRETREATMENT OF THE SUNFLOWER SEEDS AND THE LIKE

ABSTRACT OF THE DISCLOSURE
A process is disclosed whereby the objectional
grey-green discoloration is removed from sunflower seed,
meal and the like prior to roasting. The system utilizes
a pretreatment of the seeds, meal and the like by chemical
and/or physical means after dehulling and prior to roasting
by the addition of acidic compounds that significantly affect
the discoloration reaction such as those reactions that are
catalyzed by enzymes or oxygen. Similar results may be
obtained by the addition of reducing agents which serve to
prevent the oxidation of the caffeic and chlorogenic acids
or can convert the ortho-quinones back to the reduced state.
The process can also be effected by the addition of bleach-
ing agents, blocking agents, compounds which result in the
breakdown of the ortho quinone-protein complex, antioxidants,
compounds which result in the hydrolysing of the chlorogenic
acid or by the addition of compounds which cause the in-
activation of the enzymes. Finally the process may use
physical treatments. In all cases the roasting process which
follows the pretreatment, is found to stabilize the reaction
and prevent the discoloration from recurring. The pretreated
and roasted material can subsequently be used in the manufacture
of Sunflower butter spread and products thereof.


Claims

Note: Claims are shown in the official language in which they were submitted.



-35-
CLAIMS:
(1) A process for the preparation of sunflower
butter and products thereof prepared from a starting
material such as sunflower seeds, consisting of the steps
of
a) dehulling the sunflower seeds,
b) pretreating the seeds to remove the greyish-
green discoloration thereof, by immersing said seeds in a
solution selected from the group consisting of:
1. reducing agents,
2. acidic compounds,
3. bleaching agents,
4. blocking compounds,
5. compounds which result in the hydrolysis of
chlorogenic acid,
6. compounds which result in the breakdown of
the ortho quinone-protein complex,
7. compounds which result in the inactivation
of enzymes,
8. antioxidants
c) drying and roasting the seeds,
d) cooling the roasted seeds,
e) addition of other ingredients selected from
the group consisting of:
1. sweetening agents
2. stabilizers
I

-36-


3. emulsifiers
4. salt
5. flavoring compounds (artificial and/or
natural)
6. partially hydrogenated oil and/or fat
7. vegetable oil
8. animal fat
9. preservatives
10. marine oil
f) milling, grinding and homogenizing the roasted
seeds,
g) deaerating the resulting butter,
h) chilling the butter and then
i) tempering the butter.
(2) The process according to Claim 1 in which
the pretreatment of the seeds includes the immersion there-
of in a reducing solution selected from the group consist-
ing of
A. Organic reducing agents
1. ascorbic acid,
2. erythorbic acid,
3. hydroquinone
4. formaldehyde
5. ascorbyl palmitate
and
B. Inorganic reducing agent

-37-
1. sodium hydrosulfite,
2. sodium nitrite
3. sodium thiosulfate
4. sodium metabisulfite
(3) The process according to Claim 1 in which
the pretreatment of the seeds includes the immersion there-
of in an acidic solution selected from the group consist-
ing of
A. Weak organic acids consisting of
i. Carboxylic
1. citric
2. lactic
3. tartaric
4. propionic
5. acetic
6. succinic
ii. Amino
1. glutamic
2. aspartic
3. cysteine
iii. Aromatic
1. benzoic
2. phenol
3. salicylic
4. acetylsalicylic
iv. Enol

-38-

1. ascorbic acid
2. erythorbic acid
B. Strong organic acids consisting of
1. trichloracetic acid
C. Strong inorganic acids from the group con-
sisting of
1. hydrochloric
2. phosphoric
3. sulfuric
4. nitric
5. perchloric
D. Weak inorganic acids from the group con-
sisting of
1. nitrous acid
2. boric acid
3. carbonic acid
or
E. Acid salts selected from the sodium and
potassium salts of the acids listed above in parts A, B, C
and D.
(4) The process according to Claim 2 in which
the solution includes
a) 0.05% to 5.0% of the reducing agent by weight
and
b) the seeds are immersed in the solution at a
temperature from between 1°C and 200°C,

-39-
c) for a time period from between 24 hours to 2
minutes depending upon the temperature (b),
d) dried at a temperature from between 30°C to
240°C until the moisture content of the seeds drop to
approximately 8% by weight and then
e) roasting the seeds at the temperature of be-
tween 90°C and 240°C between 2 minutes and 40 minutes de-
pending upon the roasting color required.
(6) A pretreatment process for sunflower seeds
and products thereof consisting of the steps of pretreat-
ing the dehulled seed by the immersion thereof in a solu-
tion selected from the group consisting of
a) reducing agents,
b) acidic compounds,
c) bleaching agents,
d) blocking compounds,
e) compounds which result in the hydrolysis of
chlorogenic acid,
f) compounds which result in the breakdown of
the ortho quinone-protein complex.
g) compounds which result in the inactivation of
enzymes,
h) antioxidants or
i) the utilization of physical treatments.
(7) The pretreatment process according to Claim
6 in which the pretreatment of the seeds includes the im-


-40-

mersion thereof in a reducing solution selected from the
group consisting of
A. Organic reducing agents
1. ascorbic acid
2. erythorbic acid
3. hydroquinone
4. formaldehyde
5. ascorbyl palmitate
and
B. Inorganic reducing agent
1. sodium hydrosulfite
2. sodium nitrite
3. sodium thiosulfate
4. sodium metabisulfite
(8) The process according to Claim 6 in which
the pretreatment of the seeds includes the immersion there-
of in an acidic solution selected from the group consist-
ing of
A. Weak organic acids consisting of
i. Carboxylic
1. citric
2. lactic
3. tartaric
4. propionic
5. acetic
6. succinic

-41-
ii. Amino
1. glutamic
2. aspartic
3. cysteine
iii. Aromatic
1. benzoic
2. phenol
3. salicylic
4. acetylsalicylic
iv. Enol
1. ascorbic acid
2. erythorbic acid
v. Citrus juice or extract from citrus fruits.
B. Strong organic acids consisting of
1. trichloracetic acid
C. Strong inorganic acids from the group consist-
ing of
1. hydrochloric
2. phosphoric
3. sulfuric
4. nitric
5. perchloric
D. Weak inorganic acids from the group consist-
ing of
1. nitrous acid
2. boric acid

-42-

3. carbonic acid
or
E. Acid salts selected from the sodium and po-
tassium salts of the acids listed above in parts A, B, C
and D.
(9) The process according to Claim 6 in which
the solution includes
(a) 0.05% to 5.0% of the reducing agent by weight
and
(b) the seeds are immersed in the solution at
a temperature from between 1°C and 200°C,
(c) for a time period from between 24 hours to
2 minutes depending upon the temperature (b),
(d) dried at a temperature from between 30°C to
240°C until the moisture content of the seeds drops to
approximately 8% by weight and then
(e) roasting the seeds at the temperature of
between 90°C and 240°C between 2 minutes and 40 minutes
depending upon the roasting color required.
(10) The process according to Claim 6 in which
the solution consists of
a) the acid being between 0.01% and 10% by weight,
b) the seeds are immersed in the solution at a
temperature from between 1°C and 200°C,
c) for a time period from between 24 hours to 2
minutes depending upon the temperature (b),

-43-

d) dried at a temperature from between 30°C to
240°C until the moisture content of the seeds drops to
approximately 8% by weight and then
e) roasting the seeds at the temperature of be-
tween 90°C and 240°C between 2 minutes and 40 minutes de-
pending upon the roasting color required.
(11) The process according to Claim 3 or 8 in
which the citrus juice or extract from citrus fruits is
selected from the group consisting of
1. lemon juice
2. lime juice
3. orange juice
4. grapefruit juice
and from the fruit juice or extract from fruits selected
from the group consisting of
1. apples (malic acid, ascorbic acid)
2. cranberries (benzoic acid).
(12) The process according to Claims 1, 2 or 3
in which the starting material is selected from the group
consisting of Sunflower kernels, meat, meal or products
thereof,
(13) The process according to Claims 4, 5 or 6
in which the starting material is selected from the group
consisting of Sunflower kernels, meat, meal or products
thereof.
(14) The process according to Claims 7, 8 or 9

-44-
in which the reducing agent or acid is ascorbic acid.
(15) The process according to Claim 10 in which
the reducing agent or acid is ascorbic acid.
(16) The process according to Claims 6, 7 or 8
in which the reducing agent or acid is erythorbic acid.
(17) The process according to Claims 9 or 10 in
which the reducing agent or acid is erythorbic acid.
(18) The process according to Claim 1 in which
the pretreatment of the starting material includes the
steps of preheating the material by the addition of a
blocking compound which reacts with o-quinone or the free
amino and thiol groups of protein, said blocking compound
being selected from the group consisting of
1. aldehydes and ketones
2. cysteine and glutathione
3. sugars
4. primary and secondary amines
5. other amino acids.
(19) The process according to Claim 1 in which
the pretreatment of the starting material includes the
step of pretreating the material by physical means select-
ed from the group consisting of
1. the application of moist heat,
2. microwave treatment,
3. dry heat,
4. extrusion cooking,

-45-

5. cooking under pressure, and
6. cooking under vacuum.

Description

Note: Descriptions are shown in the official language in which they were submitted.


~1773Z3


SUNFLOWER BUTTER SPREAD AND PRODUCTS THEREOF INCLUDING A
PRETREATMENT OF THE SUNFLOWER SEEDS AND THE LIKE

BACKGROUND OF THE INVENTION
This invention relates to a sunflower butter or
spread and a pretreatment process of the sunflower kernels,
meat, meal or products thereof. These products are superior
in quality to conventional peanut butter or peanut spreads
and may be processed to achieve a smooth and creamy texture,
a regular style, or a chunky or crunchy style. In the
specification and claims, the term "sunflower seeds" includes
sunflower kernels, pearled kernels, cut kernels, meal and
the like.
CONVENTIONAL PEANUT BUTTER CHARACTERISTICS
Conventional peanut butter is processed by roasting
and blanching raw, whole and/or split peanuts followed by
milling and/or 8rinding and/or homogenization to achieve a
homogenous mixture. The resulting product may have added
thereto, salt, sweetening agents and stabilizerswhich
generally improve the quality characteristics and sensory
attributes of the finished product. Stabilize~ usually
consist of high melting point fat component which are
added during the grinding stage or when the product is held
at an elevated temperature. Several patents outline procedures
for stabilizing peanut butter and related products (U.S.
Patents 3,129,102; 3,671,267). A process has also been

1177;~23

- la -

described whereby peanuts are ground in the presence of
solid carbon dioxide to improve the flavour and increase
the shelf life of the finished product (U.S. Patent 4,004,037).
This process reduces the amount o oxygen which is dissolved,
occluded and absorbed from the ingredients.

1177323

--2--



Once the peanut butter has been homogenized, it is
subjected to deaeration and chilling processes which remove
occluded air and produce a crystal matrix, respectively, in
the finished product.
The composition of peanut bu~ter and peanut spread
will ultimately vary according to formulation and raw ingre-
dient composition. A summary of the composition of peanut
butter and spread is shown in Table 1. Results from this
soUrCe indicate rather high levels of protein in peanut butter
(25.2% - 27.8%) compared to peanut spread (20.3%). A study
conducted by Roberson et al., (12), before the Standard of
Identity for peanut butter was established showed a wide range
in moisture (0.67% - 2.69%), fat (44.4% - 54.4%) and protein
(19.45~ - 26~44%) contents of 30 brands of commercial peanut
butter.
Recently, McWalters and Young (13) completed a
thorough study on the quality and compositional characteris-
tics of stabilized, unstabilized and imitation peanut butter.
Table 2 shows the moisture, protein and oil content of smooth
stabilized, unstabilized and imitation peanut butter. Re-
sults showed a wide variance in moisture content - from 0.67%
to 2.22%, with stabilized peanut butters having the highest
average moisture level (2.01%), imitation were intermediate
(1.63~), and unstabilized were the lowes~ (0.74~). More vari-
ation in moisture occurred among the imitation brands than in




. . .

_~ 2a. il77323

TABLE 1: Composition of peanut butter & peanut spread (1).
Proximate ~nalyses
. _.
Car~ohydrate
~isture Protein Fat Fibre Ash %
Description ~ % - S ~ S by DifferenCe
.
PEPNUT BU~ ' ' '
Small amnts added
fat, alt 1.8 27.8 49.4 1.9 3.8 15.3
Small amnts added
fat, ~weetener,salt 1.7 25.5 49.5 1.9 3.8 17.6
Mbderate amnts
added fat,
~#dYser, salt 1.7 25.2 50.6 1.8 3.7 17.0
PE~NUr SPREWD 2.2 20.3 52.1 1.5 3.4 20.5
.


TABLE 2: ~oisture, protein ~ oil content of ~mooth, stabilized,
un~tab~lized and imitation peanut buttera (13).
.
.
. ' ' .
Peanut Butter Brand
Type Code ~ % Mbisture t Protein ~ Oil
STABILIZED 8 1.92a 23.50b 51.87ab
2.03a 24.72ab 50.40bc
13 2.22a 22.03bc 53.32ab
1.77ab 23.73ab 51.08bc
16 2.09a 23.16bc 51.29b~
nean 2.01a 23.43a 51.59xy
UNSmWBIIIZ~w 18 0.8Ibc 25.00ab 54.90a
19 0.67c 26.61a 50.43bc
nean 0.74b 25.81a 52.67x
IMIT~TIOW 12 1.83a 20.19c 47.01d
14 2.20a 11.82e 48.41cd
22 0.86bc 17.02d 50.40bc
nean 1.63ab 16.34b 48.61y
. -
a Values ~n a oolumn followed by a common letter are n~t significan~ly
different at P < 0.01 (a throu~h e) or at P < 0.05 (x,y).

~ ~773Z3
--3--

the other types.
Protein content ranged from 11.82% to 26.61% and
was significantly influenced by the type of peanut butter.
Stabilized and unstabilized butters contained similar and
significantly higher levels of protein (23.43~ and 25.81%,
respectively) than the imitation products (16.34%). The imi-
tation butters were also more variable in protein content -
ranging from 11.82% to 20.19%. Lower protein contents reflect
lower percentages of peanuts incorporated into the formulation.
10Oil content of the various types of peanut butter
; ranged from 47.01~ to 54.90%. Unstabilized butters had the
largest amount of variation in oil content while the stabiliz-
ed products have the least. It is interesting to note that
imitation peanut butters had the lowest oil content in addi-
tion to the lowest pxotein content.
Compositional characteristics of stabilized, smooth
and crunchy style peanut butters are shown in Table 3. In
smooth butters, moisture levels ranged from 0.74% to 2.22~;
~amples produced by national United States manufacturers had
'~ 20the lowest average moisture content (1.36%), chain store brands
were intermediate (1.82%) and those produced by "other" manu-
facturers were highest (2.01%). National brands had the great-
est variation in moisture level.
Protein content of smooth peanut butter produced by
the various manufacturers ranged from 21.84% to 24.72%. This
range is narrower than that quoted by Roberson et al. (12).




. _ . . _ .. ... . . .. . .. . . .. .. ....... . . . .. .. . ..... . ..

3a.
117735Z3
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0 ~ ~ ~ ~ z z z z ,
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~1 IIP ~ U~ i O ~i 0 ~ ~ i Ul
0~ ~ ~ .æ.~. X ~ .


rl ~ ¦ N ~ N N N N N N N N N N N N N ¦ ~
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~ V ¦ ¦ ~I N 117 01~ r~ c ~D ~ 8
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o n
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a ~

~177323


Oil content varied from 48.23% to 55.02% with signi-
ficant differences occurring between brands. With the excep-
tion o$ one brand, all products met the limit of 55% fat.
Moisture, fat and protein levels in crunchy peanut
butter were similar to the smooth style but with a narrower
range of values. No mention was made about the level of chunks
used in the formula. Parker and Melnick ~14) analyzed various
chunk style peanut butters manufactured in the United States
and found between 3.4% and 14.0% chunks by weight. These in-
vestigators subsequently received a patent assigned to CPC
International Inc. for incorporating 15-25% by weight peanut
chunks into peanut butter ~14).
INGREDIENT CHARACTERISTICS
.
The present invention relates to a
peanut butter type of product oonsisting primarily of Sunflower
seeds of either the oilseed or confectionery type, or a mix-
ture thereof. Additional ingredients may/may not be added to
improve the product's quality and sensory properties. These
ingredients include salt, sweetening agents, stabilizers,
emulsifiers and natural or artificial flavours.
Sunflower seeds are the primary ingredient in this
type of product and generally comprise at least 70% by weight
of the total formula. A comparison in composition between
peanut~ and confectionery Sunflower seed is shown in Table 4.
Variations in these figures would be expected due to varieties
and growth conditions.

1177323
4a.

TABLE 4: Composition of peanuts & swlflower see~s ~1).
Proxima~e Analyses
Carbohydrate
Mbisture Protein Fat Fikre Ash
Descripkion % ~ % S ~ ~y ~ifference
. , .
p~5: ' '
raw, with skins 5.6 26.0 47.5 2.4 . 2.3 16.2
raw, without skins 5.4 26.3 48.4 1.9 2.3 15.7
S~ ~;u
.~: , , . .
. y, dbhulled 4.~ 24.0 47.3 3.8 4.~ 16.1

- . : .

,
"

TABLE 5. Fatty Acid Profile ~1).


50q~ FAT FATTY ACIDba P/ ~
Description % TDtal S ~-lrated ~ :1 .C18:~ Ratio
''''' . .
. ,.

PEPNUrS:
. raw with ~kins 47.5 10 20 14
1.4:.1
~;UNEl~ÆR S~ED
KERN~S~ .
,
r~ dehuli0d 47.3 6 9 30 .5.0:1 .

based on total prod~ct weight
. b polyunsatur~te/saturate

1~773Z3

Results indicate that the proximate analyses are
quite similar with approximately 4.8% - 5.6% moisture, 24.0~ -
26.3% protein, 47.3% - 48.4% fat, 1.9% - 3.8% fibre, 2.3% -
4.0% ash and 15.7% - 16.2% carbohydrate by difference ~1).
This lnnovative product would therefore be expected to possess
similar compositional characteristics to peanut butter, peanut
spread or produc~ thereof.
However, the quality of the present invention from
a nutritional point of view would be superior to peanut butter
in view of its higher level of unsaturated fatty acids. Re-
~ults shown in Table 5 indicate that dehulled confectionery
Sunflower seeds have more than twice the level of polyunsatur-
ated fatty acids (C18 2) compared to peanuts. Perhaps more
importantly, the polyunsaturate/saturate level is 5.0:1 for
Sunflower ~eeds compared to 1.4:1 for peanuts. It is expect-
ed that these ratios will vary only slightly depending on
variety of seed or nut (2-8), environment (5-10) and maturity
~4, 6, 11).
Salt level~ generally range from 1% - 2~ by weight
of the formula and contribute towards the flavour and over-
all palatability of the finished product.
Sweetening agents may be added to the product at
levels normally up to 14%, primarily for sweetness and overall
palatability. Several patents have been issued regarding
sweetening agents in peanut butter ~U.S. patents 3,978,246
4,000,322). Examples of sugars which may be added to the con-




, " , . ... . .. .. . .. . . . .. . .. .. . ...... . . .... .... .. ... ..... .. . . . .. .

~177323


fectionery Sunflower products include corn syrup solids, dex-
trose, sucrose, invert sugar, icing sugar, beet sugar, molasses and
honey. Selection of an appropriate sweetening compound will
depend on availability, price and characteristic propertîes
such as sweetness and hydroscopicity.
Stabilizers may be added to achieve desired tex-
tures and prevent oil separation in the butter. Typical exam-
ples include partially hydrogenated fat, fully hydrogenated
fat, monoglyceride esters of fatty acids or mixtures of the
above. These stabilizers set up as a continuous or semi-
continuous stearine structure within the product during cool-
ing. This helps to give the butter a glossy surface and in-
creased stability under a broad range of storage conditions.
Levels may vary up to 10% by weight of the finished product.
Emulsifiers such as lecithin and polyglycerol esters
may also be incorporated into the product to prevent oil
separation. In emulsion systems such as margarine, these sur-
face active agents concentrate at the interface between the
oil and water, lowering the tension and allowing the two
phases to come together.
However, emulsifiers would not be expected to act
in the same manner in a peanut or Sunflower butter in view of
the low moisture content. These compounds are postulated to
form a complex with the protein moieties, thereby forming a
more readily suspendible solid in the oil phase.
Flavouring agents may also be incorporated into the




~ . . ,

1177323
;




-- 7 --



Sunflower products to enhance the flavour sensation. These
flavours may be either natural or artificial in nature and
generally comprise less than 5% on a weight basis of the
formula.
PROCESSING CONDITIONS
Some of the current processing technology for
manufacturing conventional peanut butter and products thereof
can be utilized in developing confectionery Sunflower butter.
Initially, the manufacturing procedure for Sunflower butter
appears to be relatively simple, consisting of roasting
the Sunflower seeds, grinding and/or milling and/or homogeniz-
ing the mixture of ingredients, followed by deaeration,
cooling and filling the product into containers. However,
there are complex chemical and physical changes which arise
during the processlng of Sunflower butter which do not occur
ln the processing of peanut butter and which ultimately
affect the quality of the finished product. It is imperative
that the quality of incoming raw materials be both consistent
and of high standards. The selection of optimum process-
ing equipment, operating parameters, type and quantity
of raw ingredients, and tempering conditions is essential

to maintain a consistent, uniform, high quality product.
The basic processing steps include:

1. Pretreatment
-
Pretreatment of the Sunflower kernels, meat,

- 1177323

- 7a -

meal or the like to remove the greyish-green
discoloration which is normally present therein
due to the presence and subsequent reactions
of chlorogenic and/or caffeic and other phenolic
compounds. This pretreatment will be described
hereinafter.
2. Roasting
Roasting is one of the primary steps in Sunflower
butter production whereby the Sunflower seeds
are subject to radiant heat to reast or
toast them

- ~77323


to a uniform colour and pleasant flavour. This
process may consist of a belt moving continuously
through a series of oven compartments which grad-
ually raise the temperature of the seeds to approx-
imately 160C. Typical residence times are from
10 to 40 minutes. Proctor and Schwartz make a
suitable belt roaster. Sunflower seeds may also
be roasted in a batch-type of operation such as
that manufactured by W.C. Cantrell Co. of Ft.Worth,
Texas. Production rates are three to four batches
per hour with a stock capacity of 1000 to 1200 lbs.
per hour, depending on the desired colour of the
finished product and size of roaster.
The time/temperature relationship is an important
parameter durlng roasting and influences several quality
r~ characteristics, namely:
a) development of optimum colour.
b) development of desirable flavour.
The roasting process for Sunflower butter involves
strict quality control measures to ensure that the product is
not subjected to over-roasting conditions. Since confectionery
Sunflower seeds are smaller in size than most varieties of
peanuts, more care must be taken in selecting precise condi-
tions to attain a well-balanced flavour and optimum colour.
On completion of roasting, it is essential that the
Sunflower seeds are cooled as quickly as possible to prevent
further roasting or darkening of the product. Again, the seeds

~1773;~3

g

may pass through a cooling chamber on a continuous belt or be
cooled in a bin by passing cold air through the product.
It is important to note that fresh roasted Sunflower
seeds have a volatile and perishable flavour. Therefore, they
should be processed as quickly as possible to obtain a high
quality product. Holding roasted seeds for several hours prior
to grinding can result in ~stale" Sunflower butter flavour.
Plavour as related to a Sunflower butter type of pro-
duct is a complex ~ensation involving both taste and
aroma. It is, therefore, imperative that the finished product
flavour be well-balanced. The ~lavour is a pleasant sensation
consisting of:
a) roasted Sunflower seeds and/or peanuts
b1 sweetness
c) saltiness
On the other hand, flavours may develop during pro-
cessing which render the product unacceptable in terms of
quality, namely:
a) bitterness due to over-roasting
b) "green" flavour due to inadequate roasting
c) burnt flavour due to over-roasting
d) rancid flavour due to lipid oxidation
e) oily flavour due to the inability of the mixture
to hold the oil.
Process conditions should be selected to avoid these
flavour defects.




.. . . . . . ...

~77323
-- 10 --

3) Milling/Grinding/Homogenization
This is one of the most important stages in
processing Sunflower butter and relates direct-
ly to the quality of the finished product.
There are generally three types of processing
methods which can be used singly or in combin-
ation: milling, grinding or homogenization -
all of which can produce a quality product with
uniform consistency. Crucial to the selection
o~ an appropriate process is the precise meter-
ing of incoming ingredients and control of oper-
ating parameters such as product temperature
and distance between grinding plates. W.C.
Cantrell Co. offers a Vibra Screw SCR-20 Feeder
~Trade Mark) or the accurate metering of dry
ingredients. Such feeders will ensure a uni-
form consistency in the finished product.
a) _illing
The milling process generally consists of linking
two attrition mills in series, the first providing a coarse
grind and the second a fine grind. For fine grinding, clear-
ance between the plates or discs usually range from 0.003 to
0.032 inches. These mills can be used with a single pass to
produce medium or coarse grades of Sunflower butter.
Maximum temperatures during milling or grinding
should not exceed 82C to prevent "burnt" flavours in the
A

323


finished product. In some instance5 cooling equipment may be
inserted between two mills to keep product temperatures to a
m~nimum. Cryogenic milling with solid carbon dioxiae may
also be used to improve product stability by reducing the
amount of oxygen incorporated during milling.
b~ ~rinding
Grinding or size reduction may also be utilized in
the processing stages and is usually installed as a two-stage
process. Product is fed into a pre-breaker/grinder and then
fed to a size reduction unit to givea smooth, creamy product.
Urschel manufacturers Comitrol equipment for
this process with separate cutting heads for each operation.
The size of the finished particle is determined by
the opening between the cutting blades and depth of cut made
by the blades. The microcut head may vary from 156 to 210
blades, depending on the desired fini~hed product consistency,
and remains stationary. A high speed impellor ~6,000 - 12000rpm)
forces the prebroken seeds against the blades to produce a
smooth consistency. The leading edge of the blade is a sharp
knife which accomplishes size reduction with no metal-to-metal
contact.
c) Homogenization
Homogenization may be used as a unit proces~ or as a
finishing procese for manufacturing Sunflower butter and pro-
ducts thereof. This process produces a fine and creamy texture
as well as a smooth appearance.

-12- ~323

4) Deaeration
The previous grinding or milling procedures in-
corporate air into the but~er which would sub-
sequently decrease the shelf life of the pro-
duct if not removed. Thus, stainless steel
deaeration tanks may be employed to facilitate
the release of entrained air from the butter.
A full sweep agitator removes the produce from
the wall of the vessel and continuously exposes
new surface to allow air to escape under vacuum.
5) Chilling
Chilling is an important aspect of the Sunflower
butter processing and is required to reduce pro-
duct temperatures down to approximately 32-43C
for filling. The outlet temperature will de-
pend on the choice of stabilizer, but should be
as low as tolerable for filling so that the dis-
sipation of heat during tempering is kept to a
minimum. The common equipment used in this type
of operation are either Votator "C" (Trade Mark)
units or Crepaco (Trade Mark) Swept Surface
Heat Exchangers.
Optimum operating parameters must be selected to
promote crystallization and achieve a desirable finished pro-
duct texture. In addition, operating conditions should be
related to tempering conditions to maximize product quallty.

~1773Z3



6) Tempering
Finished product is tempered for a period of up
to 72 hours at 10 - 38C. in roder to optimize
crystallization properties of the product.
7) Chunk Style
In the preparation of a chunk style Sunflower
butter and products thereof, granulated Sunflower
seeds or other suitable nuts are mixed into a
smooth or creamy phase prior to the packaging
process. Unfortunately, the agitation or mixing
required to obtain an even distribution of chunks
in the butter phase other products an end product
which exhibits a greater tendency to oil out. This
is a result of marked disruption of the contin-
uous fat structure in the Sunflower butter.
Oil separation will generally occur in the vicinity
of a Sunflower chunk. Hlgher levels of chunks
will accentuate the problem and produce a Sun-
flower butter which is difficult to spread.
Therefore, many peanut butter manufactueres will
increase the level of hard fat or stabilizer
in the smooth phase to compensate for the oil
separation problem. Similarly, increased levels
of stabilizer are employed in Sunflower butter
to improve spreadability and maintain protection
against oil

~lt~73Z3

-14-

separation. Additional levels of 0.5% to 3.5%
hard fat, monoglycerides, diglycerides, or
blends thereof are commonly utilized.
Quality Characteristics
Quality characteristics as they relate to confec-
tionery Sunflower butter are both numerous and diverse in .
nature. They vary according to ingredients, formulation,
method of manufacture, and tempering and handling conditions.
The end result i8 a product category having a wide
10rangeof quality attributes-
Examples of product composition are shown as follows:
Example 1: 90% Sunflower Seeds
2% Vegetable Oil
2% Hydrogenated Yegetable Oil
4.5% Sugar (dextrose)
1.5% Salt
Example 2: 90% Sunflower Seeds
2% Mono and Diglycerides
2% Hydrogenated Vegetable Oil
4.5% Sugar (dextrose and icing sugar)
1.5% Salt

Example 3: 80% Sunflower Seeds
8.5% Vegetable Oil
2% Mono and Diglycerides
4% Hydrogenated Vegetable Oil
4% Sugar ~dextrose)
1.5% Salt

; ~ 1773Z3
.



-15-

A nutritional profile compares two commercial
brands of smooth style peanut butter against the Sunflower
butter outlined in Example 1. Results are shown in Table 6
and indicate similar values for proximate analyses. The
Sunflower bu~ter had a slightly lower moisture level and
higher ash and fibre content than peanut butter. Protein
contents were similar and ultimately depend on the level of
nuts or seeds in the formula. The concentration of fat, on
the other hand, depends both on the level of nuts or seeds
and the level of added fat or stabilizer.
Mineral contents in the two brands of peanut butter
were similar while the Sunflower butter showed slightly higher
levels, especially in calcium and phosphorus. Iron, which is
a well documented pro-oxidant of lipid oxidation (15), was
present in all products at higher concentrations than expect-
ed (0.0040%- 0.0055%). Watt and Merril (1) quote average
levels of 0.0019% - 0.0020% iron in peanut butter and 0.0015%
iron in peanut spread.
Salt is added to peanut butter for palatability
considerations and was found to vary from 1.27% in Brand #l
peanut butter to 1.51% in Brand #2 peanut butter.
Acidity or pH ranged from fi.65 to 6.70 in peanut
butter to 6.25 in the Sunflower butter. These differences
would not be expected to significantly influence shelf life
or product guality.

15~ 7323

TA~LE 6: Nutritional profile of peanut butter ver3us
- Sunflower butter.

COMPOSITION BY WEIGHT
SUNFLOWER
DESCRIPTION BRAND #1 BRAND ~2 BUTTER

Proximate Analysis: -
Moisture 1.26 2.65 0.50
Pat 53.30 52.10 54.30
Protein (N x 5.46)22.80 21.58 21.S8
Ash 3.11 3.38 4.74
Fibre 1.28 1.44 1.92
Carbohydrate by
Difference 18.25 18.85 16.96
Total Sugars 7.25 10.48 8.12
Viscosity, cps: 6 6 6
; 2 rpm 2.72 x 10 2.00 x 10 3.25 x 16
4 rpm 1.61 x 106 1.03 x 106 1.83 x 10
pH 6.70 6.65 6.25
Salt (by Cl) 1.27 1.51 1.47
(by Na) 1.28 1.42 1.28
Calcium 0.052 0.043 0.072
Phosphorh~ 0-35 0-33 0-74
Potas~lum 0.58 0.57 0.63
Iron 0.0050 0.0040 0.0055
'.

~atty Acid Profile: g/100 g ~at
C16:0 ~.9 9.0 5.9
C18:0 4.0 4.2 6.6
C18:1 45.6 44.3 15.9
C18:2 35.3 34.7 70.0
18:3 1.4 1.3 --
C20:0 0.8 1.8 --
C22:0 3.0 4.7 1.6
Polyun~aturates lP) 36.7 36.0 70.0
Saturates lS) 17.7 19.7 14.1
P/S 2.1:1 1.8:1 5,ol
. .. ,

~ ~.77323

-16-

From a nutritional point of view, fatty acid pro-
files have become increasingly important in the past few
years. Indeed, levels of polyunsaturated and saturated fat
in the diet have been of interest to dietitians, physicians,
the fats and oils industry, government, and of course the
consumer at large.
The nutritional profile indicates that the polyun-
saturated fatty acid content of the Sunflower butter is appro-
ximately twice that in peanut butter. Polyunsaturates ranged
from 36.0% to 36.7% in peanut butter to 70~ in the Sunflower
butter. Another important aspect to note is that the polyun-
~aturatejsaturate ratio is 5.0:1 in the Sunflower product com-
pared to 1.8 to 2.1:1 in the peanut butter samples. These re-
~ults are depicted as typical for these typesof products.
The Sunflower spreads are characteristically greater than
55~ in at content with similar fatty acid profiles.
Other important characteristics of these types of
products are their quality and quantity of protein. The pro-
tein efficiency ratio (PER), a biological measure of protein
quality, i~ 1.7 for peanut butter compared to 2.5 for casein
(17). ~hus, depending on the quantity of protein, peanut
butter fits the label of being either a "good source" or an
"excellent ~ource" of protein. Similarly, Sunflower butter
would be expected to fit into the ~ame category.

~1~77323

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i~773Z3
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19- ~1773Z3
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11773Z3


_ 20 -

With reference to the pretreatment process mentioned
previously, a process is disclosed which eliminates the greyish-
green discoloration which is normally present in Sunflower
kernels, meat, meal or products thereof and results from the
presence and subsequent reactions of chlorogenic acid and/or
caffeic acid. This pretreatment process utilizes chemical
and/or physical treatments to eliminate the colour problems.
Figure 1 shows a suggested reaction for the forma-
tion of colour complexes in Sunflower products.
Figure 2 shows the reactions of o-quinone with
sulfhydryl, amino, imino and activated methylene groups under
alkaline conditions.
Phenolic Compounds
The successful utilization of Sunflower kernels,
meal or flour for human consumption such as Sunflower butter,
spread and products thereof, has been hampered by the detri-
mental properties of phenolic compounds present in these
materials. These compounds produce an objectionable dark
greyish-green colour due to the oxidation of polyphenolic
compounds. Chlorogenic acid has been identified as the major
polyphenolic compound in Sunflower kernels with minor constit-
uents comprising caffeic acid, 3,5-dicaffeoylquinic acid,
and a disubstituted cinnamic acid (19,20). Sabir et al. (20)
reported 3 to 3.5.g per 100 g of Sunflower flour with chlorogenic
and caffeic acids representing about 70% of the total phenolics.
Compounds related to p-coumaric, isoferulic and sinapic acids, as

1~773:23

- 21 -

well as hydroxycinnamic acid-sugar esters were also identified
in the Sunflower flour (26). Many of the phenolic com-
pounds are located in the outer portions of the Sunflower
kernel, just under the testa (21).
The exact mechanism responsible for producing
the discolouration problem is not well defined in the
literature. Sosulski (22) proposed the following reaction
to account for the formation of colour complexes in Sun
flower products (Fig. 1). Atmospheric oxygen or enzyme
catalyzed oxidation results in the formation of quinoidal
compounds and possibly hydroperoxides (22). Both of these
substances destruct labile amino acids, denature proteins
and inhibit enzymes such as indole acetic acid oxidase (23),
trypsin and lipase (19), and arginase (24). Cinnamic acids
and their esters are of particular significance in oilseeds
since they are preferred substrates for phenol oxidase (26).
The ortho-dihydroxyphenols such as caffeic acid,
part of the chlorogenic acid molecule, may be oxidized to
ortho-quinones by copper-containing enzymes present in the
Sunflower material (22). Once formed, ortho-quinones such
as chlorogenoquinone can react nonenzymatically to poly-
merize or may bond covalently to fee amino, thiol or methy-
lene groups of protein. The -amino group of lysine and
the thioether group of methionine may be common targets,
thereby rendering them nutritionally unavailable to the mono-
gastric digestive system (22). The end result is a product
with non-asthetic properties.

~.773Z3
- 21a -

Figure 2 depicts a series of reactions of o - quinone with
-sulfhydryl, amino, imino and activated methylene groups under
alkaline conditions. The initial addition products are in
their reduced (hydroquinone) state and are not brightly
coloured. For example, the reaction of o - quinone with an
amino acid forms the addition product and the concomitant
reduction of quinone to the hydroquinone.



OH

R ~ O + AA ) R ~ OH



In the reduced state the addition product is not colored
green. Howe~er, when the reduced form is oxidized by an unreacted
quinone or oxygen, the dark green color develops,

OH OH

; R ~ OH + quinone ~ R ~ O + hydroq~inone


(colorless) (green)

~1773Z3


As a result of the discolouration problem, numerous
investigators have attempted to remove the phenolic com-
pounds from the kernels, meal or subsequent products. Com-
plete removal of phenolics from Sunflower meal or isolate
has been demonstrated after long periods of refluxing or
shaking with 50-95% ethanol or 70-85% methanol (18,22,27,
28,29~. Aqueous batch diffusion by Sosulski et al. (30)
removed over 90% of the chlorogenic acid from dehulled ker-
nels and the defatted flour retained its white appearance
under alkaline conditions. This process was based on the
principle that low molecular weight substances such as poly-
phenolic acids, simple sugars, minerals and nonprotein
nitrogen compounds will passively diffuse through the semi-
permeable membrances in the plant cells while large mole-
cules such as triglycerides, protein, starch and crude fibre
are retained in the kernel. However, operational costs
for this method are prohibitive due to long extraction
periods, large volumes of water required and high temper-
atures required.
Sosulski et al. (21) later developed a continuous
diffusion process at 80C which eliminated the discolour-
ation problem in meal when solvent ratios and residence
times were high. Results from these studies are shown in
Tables 1, 2 and 3. Testa removal and temperature were found
to be more critical than solvent flow rates for the rapid

~73;~3

- 23 -

diffusion of chlorogenic acid. However, commercialization
of this process is not feasible in light of the large volumes
of extract liquor required which would create a serious
problem of waste disposal or solvent recovery. Product
losses and protein solubilities were also prohibitive.
Fan _ al. (31) attempted to decrease the solvent
requirements for the extraction of chlorogenic acid from
Sunflower seeds and flour. Again~ yields of product from
the countercurrent extraction process were low, thereby
limiting its practical significance.
SUMMARY OF THE INVENTION
The present invention relates to a chemical and/
or physical process which eliminates the discolouration
problem in Sunflower kernels, meat, meal or products there-
of. The source of Sunflowers may be either the confection-
ery or oilseed varieties and must be dehulled prior to ap-
plication of the process. This process may be described
as a pretreatment process, especially when it is applied
to the whole Sunflower kernel after dehulling. Testas may
or may not be removed prior to pretreatment processing.
In any event, it is undertaken prior to the roasting of
seeds.
As discussed, this invention may be applied to
Sunflower meats or meal. These substances may or may not
be ground up in conventional ways prior to treatment

1~77323

_ 24 -

by the process described herein.
The basic invention details a process which may
include one or more of the following reactions. Examples
of typical classes of chemicals which may be utilized in
the process are also provided. The end result of these
processes is the elimination of the grey-green colour and,
in many instances, an improvement in the flavour and palat-
ability of the product. Product yields may range above
9~% and are typically in the range of 95%.
Process treatments may include one
or more of:
1. Addition of acidic compounds that significantly affect
the discolouration reaction. The most obvious reactions
are those catalyzed by enzymes or oxygen. Typical classes
of acids include:
A. Weak organic acids
i. Carboxylic
1. citric
2. lactic
3. tartaric
4. propionic
5. acetic
6. succinic

1177323


ii. Amino
1. glutamic
2. aspartic
3. cysteine
iii. Aromatic
1. benzoic
2. phenol
3. salicylic
4. acetylsalicylic
iv. Enol
1. ascorbic acid
2. erythorbic acid
v. Citrus juice or extract from citrus fruits
such as:
1. lemon juice
2. lime juice
3. orange juice
4. grapefruit juice
vi. Fruit juice or extract from fruits such as:
1. apples (malic acid, ascorbic acid)
2. cranberries (benzoic acid)
B. Strong organic acids
1. trichloracetic acid

:~773Z3
- 26 -

C. Strong inorganic acids
1. hydrochloric
2. phosphoric
3. sulfuric
4. nitric
5. perchloric
D. Weak inorganic acids
1. nitrous acid
2. boric acid
3. carbonic acid
E. Acid salts
The sodium and potassium salts of the acids
in parts A, B, C and D.
2. Addition of reducing agents. These compounds will serve
two functions. They will be preferentially oxidized and
thereby prevent the oxidation of caffeic and chlorogenic
acids or if strong reducing agents are used, they can con-
vert the ortho-quinones back to the reduced state.
Typical reagents for this process are:
A. Organic reducing agents
1. ascorbic acid
2. erythorbic acid
3. hydroquinone

11773Z3
- 27 -

4. formaldehyde
5. ascorbyl palmitate
B. Inorganic reducing agent
1. sodium hydrosulfite
2. sodium nitrite
3. sodium thiosulfate
4. sodium metabisulfite
3. Addition of bleaching agents. This technique will des-
troy the colour complexes which have formed.
Examples include:
1. hydrogen peroxide
2. chlorine
3. sulfur dioxide
4. soidum bisulfite
5. sulfurous acid
4. Inactivation of enzymes
1. heat treatment
2. addition of enzyme inhibitors
3. addition of metal ion chelators
4. adjustment in pH
5. Addition of blocking compounds. These compounds will
react with the o-quinone or with the free amino and thiol

~1773Z3

- 28 -

groups of proteins and prevent the formation of the colour-
ed complex.
Examples of such compounds include:
1. aldehydes and ketones
2. cysteine and glutathione
3. sugars
4. primary and secondary amines
5. Other amino acids
6. Addition of compounds which result in the hydrolysis
of chlorogenic acid. Examples include the following: -
i. Strong acids
1. hydrochloric acid
2. phosphoric acid
3. sulfuric acid
ii. Enzymes
1. esterases
7. Addition of compounds which result in the breakdown
of the ortho quinone-protein complex.
1. strong acid
enzymes
8. Addition of antioxidants. These compounds will slow
any free radical mediated reactions.
1. Butylated hydroxyanisole (BHA~
2. Butylated hydroxytoluene (BHT)

11'773Z3

_ 29 -

3. Propyl gallate
4. Tertiary butylhydroquinone (TBHQ)
5. Gums such as gum guaiac
6. Ethosyquin
7. Tocopherols
9. Utilization of physical treatments:
1. Application of moist heat. Examples in-
clude pasteurization5 tyndallization, auto-
claving, or heating in presence of aqueous
solutions of the one or more of the afore-
mentioned chemicals or classes of chemicals.
2. Utilization of microwave treatments.
3. Dry heat such as oven drying.
4. Extrusion cooking
5. Cooklng under pressure or vacuum
Although several process treatments are disclosed,
perhaps the most important ones are firstly the use of the
reducing agents and secondly the use of the acidic compounds.
The processes for use of these two preferred treat-
ments are similar and dealing first with the use of the
reducing agents, the solution containing them should in-
clude the selected reducing agent in a ratio of between 0.05%
and 5.0% by weight. The seeds or other form of meal and the
like are soaked in the solution at a temperature of between
1C and 100C. Cooking under pressure could utilize higher

11773Z3

- 30 -

temperatures. For example, temperatures could reach 200C
at 225.5 p.s.i.
It will of course be appreciated that the hotter
the solution, the less time is required for the solution to
be absorbed by the seeds until they contain approximately
40% by weight of the solution although this figure can go
as high as 70% by weight.
The time is therefore between 24 hours if the solu-
tion is at 1C down to approximately 2 minutes if the solution
is at the boiling point, namely, 100C.
The preferred temperature is 95C and the preferred
moisture content should be approximately 40/O by weight.
Once this has been reached, the seeds or other form
of meal, are placed in a combination drying and roasting device
the temperature of which is preferably approximately 160C.
However, this temperature may vary from a low of 30C to a
high of 240C.
Drying ends when the moisture content has dropped
to approximately 8% by weight and at that point the roasting
action commences and takes approximately 2 to 40 minutes de-
pending upon the roasting colour required. The desirable
colour is a light toasted colour and once again this depends
upon the temperature selected.
Once the roasting action has been completed, the

~773Z3

- 31 -

remainder of the process as hereinbefore described, may
take place with the roasting action preventing a reverse
of the discolouration from occurring.
When using the acidic treatment, the acid solution
should be between 0.01% and 10% by weight and typically,
0.1% to 1.0% acid is utilized. Otherwise the details of the
pretreatment are the same as that given for the reducing treat-
ment.
Examples of typical pretreatment systems are as follows:
Example 4: Dehulled confectionary Sunflower seed is immersed
in a 2% solution of ascorbic acid at 30C until
the seed moisture content has reached 40% by
weight. The pretreated seed is then dried and
roasted at 160C.
Example 5: Dehulled confectionary Sunflower seed is immersed
in a boiling solution of erythorbic acid (1%
by weight) for 30 minutes. The pretreated seed
is then dried and roasted at 160C.
Example 6: Dehulled Sunflower seed is immersed in a 1%
tartaric acid solution (by weight) at 95C for
20 minutes. The pretreated seed is then dried
roasted at 170C.

il773Z3



REFERENCES
1. Watt, B.K. and Merrill, A.L., Composition of Foods:
raw, processed, prepared, Agriculture Handbook No: 8,
(1975).
2. Carter, J.F., Sunflower science and technology,
Agronomy Series No: 19, Soil Science Socity of
America, Inc., Madison, Wisconsin, (1978), Chapter 9.
3. Holley, K.T. and Hammons, RØ, University of Georgia
Research Bulletin No: 32, (1968).
4. Sanders, T.H., J.A.O.C.S. 57:12, (1980).
5. Worthington, R.E., Hammons, RØ and Allison, J.R.,
J. Agric. Food Chem. 20:727, (1972).
6. Young, C.T., Matlock, R.S. and Waller, G.R., J.A.O.C.S.
49:314, (1972).
7. Young, C.T., Worthington, R.E., Hammons, RØ, Matlock,
R.S., Waller, G.R. and Morrison, R.D., J.A.O.C.S. 51:31
(1974).
8. Brown, D.F., Cater, C.M., Mattil, K.F. and Darrock, J.G.
J. Good Sci. 40:1055 (1975).
9. Kinman, M.L. and Earle, F.R., Crop Science, 4:412, (1964).
10. Cavin, D.T., Can. J. Bot. 43:63, (1965).
11. Worthington, R.E., Proceedings 5th National Peanut Research
Conference, Norfolk, V.A. (1968), Page 87.
12. Roberson, S., Marion, J.E. and Woodroof, J.G. J. Amer.
Dietic Assoc. 49:208, (1966).

il77;~23

- 33 -

13. McWatters, K.H. and Young, C.T., J Food Sci. 43:370,
(1978).
14. Parker, W.A. and Melnick, D., Chunk style peanut butter
U.S. Patent 3,950,568; April 13, (1976).
15. MacDonald, B.E., M. Sc. Thesis, University of Guelph,
Guelph, Ontario, (1978).
16. F.A.O., Amino Acid Content of Foods and Biological
Data on Proteins, Food and Agriculture Organization
of the United Nations, Rome, Italy (1970).
17. ~aighton, A.J., J.A.O.C.S. 36 (1959) Page 347
18. Mikoljczak, K.L., Smith, C.R., Jr., and Wolff, I.A.
J. Agr. Food Chem. 18:27 (1970).
19. Milic, B., Stojanovic, S., Vucurevic, N., and Turcic, M.
J. Sci. Food Agr. 19:108 (1968).
20. Sabir, M.A., Sosulski, F.W., and Kernan, J.A.
J. Agr. Food Chem. 22:572 (1974).
21. Sosulski, F.W., Sabir, M.A. and Fleming, S.E.
J. Food Sci. 38:468 (1973).
22. Sosulski, F., J. Amer. Oil Chemists' Soc. 56:711 (1979).
23. Rabin, R.S. and Kein, R.M. Arch. Biochem. Biophys.
70:11 (1975).
24. Muszynska, G. and Reflier, I., Acta Biochem. Pol. 17:247
(1970).
25. Pierpoint, W.S., Rep. Rothamsted Exp. Stn. Part 2,
Page 199, (1970).

` 11773Z3



26. Smith, A.F. and Johnsen, V.L., Cereal Chem. 25:399
(1948).
27. Joubert, F.J., Biochim. Biophys. Acta 16:520 (1955).
28. Gheyassudin, S., Cater, C.M. and Mattil, K.F.
Food Technol. 24:242 (1970).
29. Pomenta, J.V. and Burns, E.D., J. Food Sci. 36:490
(1971).
30. Sosulski, F.W., McCleary, C.W. and Soliman, F.S.
J. Food Sci. 37:253(1972).
31. Fan, T.Y., Sosulski, F.W. and Hamon, N.W., Cereal
Chem. 53:118 (1976)~


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Administrative Status

Title Date
Forecasted Issue Date 1984-11-06
(22) Filed 1982-03-01
(45) Issued 1984-11-06
Correction of Expired 2001-11-07
Expired 2002-03-01

Abandonment History

There is no abandonment history.

Payment History

Fee Type Anniversary Year Due Date Amount Paid Paid Date
Application Fee $0.00 1982-03-01
Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
CSP FOODS LTD.
Past Owners on Record
GALLOWAY, GEOFFREY
KAKUDA, YUKIO
MACDONALD, BRUCE E.
Past Owners that do not appear in the "Owners on Record" listing will appear in other documentation within the application.
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Document
Description 
Date
(yyyy-mm-dd) 
Number of pages   Size of Image (KB) 
Description 1993-12-16 41 1,101
Drawings 1993-12-16 2 26
Claims 1993-12-16 11 204
Abstract 1993-12-16 1 35
Cover Page 1993-12-16 1 15