Note: Descriptions are shown in the official language in which they were submitted.
~Z~3~08
CASE 1419
"PREPARING EDIBLE SANITIZED FLOURS FROM OIL-BEARING ~EEDS"
. This invention relates to a process for producing
an edibie proteinaceous flour, which is microbiological-
ly acceptab]e, from oil-bearing seeds3 both of the kind
having a high oil contents, such as sunflower, peanut,
cottom and the like and of the kind having a low oil
contents, such as soybean, grape seeds, sesameS carthamum
and others,
More particularly, the present invention re3ates
to a process -For producing sunflower f]our, to be utilized
for human consumption, from doth dehulled and straigh~
sunflo~ver seeds.
The produc-tion of components and intermediates for
the formulation of finished -food products requires, during
progress of processing and conversion of the ra~ materials,
the keeping of thc nu-tritional properties and the con-
formance to the hygienic and sanitary rules for the pro-
ducts to safeguard the consumer's health.
The qu~J.ity of a food is a function of a number of
differenl factols, such as:
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37~1~
2.
chemical composition and quality of the raw materials,
producti.on technologies and materials used in the instal-
lations, hygienic and sanitary conditions of the pro-
duction environment and mode of preservation of the
finished food product (Nickerson, ~T. and Sinskey, A.~.,
1972, Microbiology of Foods and Food Processing- American
Elsevier Publishing Co., New York~.
At present, the installations adopted to the pre-
. paration of food products provide, in the last stages
of processing, or even in any of the intermediate stages,
a sanitizing or a sterilizing run.
More particularly, treatment of the kind referred
to above are vital for proteiniacesous products obtained
from vegetable seeds9 in which the initial bacterial
charge is at tim~ above the limits of acceptance established
by the various legal prescriptions. To fulf;l such re-
quirements, it is necessary, in the industrial practice9
to effect a sterilization stage which, so~etimes, is
carried out under so drastic conditions as to entail
structural modifications or a depreciation of t:he biolo-
gical and nutritional properties of the end products.
(Tateo F., 1977, Detergenza e sanificazione nell'Indu-
stria Alimcntare, AEB Brescia, Italy)
The present invention relates to the industrial
process.ing of dehulled or straight sunflower seeds, for
the productioll of proteinic flours having microbic)locji-
cal specificdti~ons compatible with the use as food for
huma I)S .
~2~370~3
More particularly, the present invention proposes
a process for producing proteinic flours from whole or dehul-
led sunflowerseeds, characterized in that, for the purpose
o~ reducing the bacterial content of the finished flours to
such a level as to prevent noxious fermentations, it comprises
the step of contacting such seeds with an extractant system
consisting of hexane and ethanol , the concentration of
ethanol relative to hexane lying in the range from 1% to 5%
on a volume/volume basis, the ratio of the solids to be
extracted to the extractant system, on a weight/volume
basis lying in the range from 1:5 to 1:20, at an ambient
temperature of from 20 C to 25C and for a time variable
from 30 minutes to 3 hours.
The bland conditions provided for the extraction
process of oil from the sunflower seeds, straight, or de-
hulled as the case may be, in order that proteinic pro-
ducts be obtained with a high biological value ~see Canadian
Pat. No. 1.119.781 granted on March 16, 1982) requires the
use of appropriate solvents in the extraction runs so as to
obtain, irrespective of the raw materials used, proteinic
products which are mibrobiologically acceptable.
In accordance with the invention, the solvent
which is used for the extraction consists of a mixture
composed of hexane and ethanol.
The use of ethanol is justified by its sanitizing
power which is unEolded by the breakage of the cellular
walls dehydration action o~ the alcohol (Verona 0., Picci G.,
Microbiologia degli Alimenti, 1968, UTET~.
The extrac-tion run is carried out with the
aid of such a mixture composed o hexane and ethanol, the
concentration of ethanol relative to hexane ranging from 1%
to 50% on a volume/volme basis.
The solid-liquid extraction is carried out by a
process which is preferably conducted stepwise, the individual
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stages bleing from half-an-hour to 4 hours long, the solid-
liquid, that is, weight by volume ratio being from l:l to
l:40 at a processing temperature from 20C to 60C. The thus
recovered solids are then dried for A period of from l to 60
hours.
All the working details of the process according
to the invention will become apparent from the scrutiny of
the examples to be reported hereinafter.
The examples to follow relate to processes for pro-
ducing edible proteinic flours from sunflower seeds.
The Materials
Ethanol and norm.hexane, supplied by Carlo Erba,
MIlan, I1:aly, as RPE solvent (Erba Pure Reagent).
The culturing media used for the microbiolosical
assays were: Plate Count Agar, Mycological Agar, E,E~
Mossel Broth, Tryptic Soy Broth, Violet Red Bile, Bacto
Brilliant Green Bile Broth, McConkey Agar have been
supplied by~DIFCO, whereas the Clostridium perfrigens
Selective Agar was supplied by Merck.
The Methods for Analysis
The characterization of the chemical components,
moisture, lipids, ash, proteins and crude fibre was carried
out according to the methods by A.O.A.C. (Association
Official Analytical Chemists, 1lth ~diti
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s.
Tlhe phenols have been metereci gaschromatoc~rapllieal-
ly with the direct silylation rnethod.
The soluble sugars were determined colorimetrieal-
ly with t:he method by Dubois M. et al (Anal. Chem., 28
N 3, 350 (1956).
The microbiologieal assays were earrie~ ou-t ae-
cording to the procedures reported by Mossel D.A.A.,
Brechet ~., Lambion R., in "La prevention des infeetions
et des toxi-infections alimentaires", CEPIA, Brussels
(1962).
EXAMPLE 1
This example relates to the preparation of de~oiled,
m:ierobiologieally aeeeptable flour by extraction of oil
from sunflower dehulled seeds wi-th norm.hexane, eontain~
ing ethanc~l at different eoncentra-tions by volume (from
1% to 5%) at the extraetion ratio (wtlvol) of 1:20 and
at the temlperature of 22C. The dryinc~ t;me was 4~ hours
at ambient temperature.
TABIE 1
Chemieal eoml)osi-tion of the ciehulled sunfi()~er seeds, on
dry matter~ pereent (~)
Moisture 6.0
Lipids 60.0
Proteins (Nx6.25)22.0
Ash 2.9
Crucle fibrc 3.5
SoJublc sugars 4,l~
Phcnc)ls (GLC) 1.5
NitrocJcn-free extr. 5.7 (by differellcc)
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6.
The clehulled sunflower seeds hav;ny the chemical
composition reported i.mmediately above in Table 1, were
flaked and cieboiled in ba~h with stirring at a tempera-
ture of 22(`, in the ratio of 1:20 solid:llquid (wt/vol)
in two indivi.clual runs during 1 hour each with nor.
hexane and one step with norm.hexane and ethanol, at dif-
ferent concentrations and with a con-tact time ofone hour.
Table 2 reports the microbiological data at the
dif`ferent concentrations of ethanol~ lhe results which
have been obtained slow the different behaYiour of the
microor~anis!ns towards the same saniti~in~ a~ent: the
la-tter is very active aga.inst vege~ative bacterial strai.ns,
the yeasts and the moulds, whereas the spore-forming
strains are strongly resistant. The flour, prior to be-
ing analyzed, has been dried at the environmental tempe-
rature for 4S hours.
EXAMPLE 2
This example relates to the preparation of de-
oiled, microbiologically acceptable flour by extraction
of the oil ~rom dehulled sunflower seeds with norm.hexane
contailling 5~1 ethanol by volume, the extraction ratio
being 1:20 (solid:liquid) at the temperature of 22~.
The flour has been dried for 12 hours, or for ~S
hours at the cnvironmental tempcrature.
2S Dehullccl s~lnflo~Yer seeds~ the de~ree of pollution
of which was l~nown an~ hav:ing a chemical composition of
-the -type repor~ed in lablc 1, ~Yel~e de-oiled with a mix-
turc o~ norln.l)exanc and cthanr)l (5% by vol of thc latter);
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7.
aftcr havillc; been flalced and after tWQ steps of batch ex-
traction with norm.hexane o-f 1 hour each, with variable
contact times The temperature was 22C, -the extraction
rat;o (soi;d:liquid) was 1:20~ The dryintJ times of the
flour at the environmental -temperature was from 12 hours
to ~8 hours.
The results tabulated in Table 3 show that the sa-
nitizing action of 5% ethanol in normOhexane is appre-
ciable yet after the first 30 mins of contact. The dry-
incJ of the flour at the environmental temperature for
differe,l-t contact times has proven to be ineffective to--
wards the bacterial charcJe of the products which have
been tested.
EXAMPLE 3
This example relates to the preparation of cle-
oiled, microbiologically accep-table flour by extractins
the oil from dehulled sunflower seeds with norm.hexane,
containing 5~ ethanol by volume 9 with an ex-traction ratio
~solid:litluid) 1:5 at -the -temperature o-f 22C.
The chemical composition was that reported in
Table 1 abo~e. Tlle extraction of the oil from the de-
hulled seeds has been carried out with norm.hexane, two
extralc-tion runs 1:20 (solid:liquid), followed by a third
extraction step with 5~ ethanol in norm.hexane in the
ratio of extraction (solid:liquid) of 1:5, the contact
times beintJ clifferent, at the temperature of 22C. The
flour thus obtalned has been allowed to clry at the en-
virorlmental teml)erature, untitr a hood, for 48 hours.
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8.
The results tabulated in Table l~ sho~ the saniti~ing ac~
tion of the e-thanol-hexane mixture also for extraction
ratios (solid:l.i(luid) o-f 1:20 and under, the effect be-
i.ng slightly weaker than -that tabulated in Table 3 of
Exarnp].e 2.
EXAMPLE 4
Tllis example relates to the prepara-tion of de-
oiled, microbiologically acceptable sunflower dehulled
seed flour, by extract;on of the oil with norm.hexane
contai.n.;.n~ cthanol 2~ and 3% by volume, respectively, ~ith
an extrac-t;.ol-i rati.G (soJid li.qui~l) of 1:~0; at the tempe-
rature of 22~C.
The chemi.cal composition of thc sunflower dehulled
seeds was that reported in Table 1 above.
The extraction of oil from the dehulled see~s was
carried out with norm.hexane, by two extraction rurls 1:20
~soli.d:liqui.d), followed by a third extraction sta~e
with 2~ e-thanol in norm.hexane, or 3% e-thanoJ. (hy vol~)
in norm,hexarle, the extraction ratio bein~ 1:20 at the
temperature of 22C. The flour thus obtained was dried at
the environmen-tal temperature for 4~ hours.
The results tabulated in Table 5 sho~ that the sa-
ni-tizin~ action of the ethanol-noIm.hexane rnixture is
appreciable a-t a concentration of 3~ e-thanol in nor.
hexane with a contact time of 3 hours.
EXAMI'LE: 5
lhis cxclmple re~ates to thc preparation of a de-
oi.].ed, rnicrob.i.olo~i.cally acceptable f].our by cxtract;o
1~0~7()8
9.
of the oil -from sunflower dehulled seeds with norm~hexane
containincJ 3~ ethanol by volume, the extractjon ratio bc-
ing 1:20 (sol:id:liquid) with contact tirnes of 19 2 and 3
ho~lrs at a -temperature of 60~C.
The chemical composition of -the dehullecl seeds was
that reported on Table 1 abo~e. The extraction of the oil
frorn the dehulled seeds was carriecl out with norm.hexane,
two extraction runs 1:20 (solid:liquid) followed by a
third extrac-tion run with 3% ethanol in norm.hexane by
volume, with a ratio of 1:20 (solid:liquid extraction)
at the temperature of 60~C and with contact -times of 1,
2 and 3 tlours. The flour thus obtained was dried at room
temperature for 48 hours. As reported on Table 6, it can
be seen that the use of a tempera-ture of 60C does not
improve the sanitizing effect of the ethano] norm.hexane
mixture.
TABLE 2
Effect Ol d fferent concentrations of ethanol in norm.ilexane upon the bacterial charge
of de-oiled s~mnfio~er flour.
Flour de-oiled with
"icrobiological Tests Flaked nor.hexane nor.hex~re nor.hexane ncr.hexane nor.hexane
with l~u ~ith 3~ ~ith 4~ with 5~u
ethanol ethanol ethanol ethanol
Bacterial count N/gram7.105 6.106 7.105 3.105 5.io5 2.105
~ore-form-ng ~jgram 105 6.105 8.10~ 2.~o5 5.io5 105
Yeasts ~/5ram S.103 5.103 C lo2 C 10 ~ 10 C 10
Moulds N/gram 6.104 2.105 60103 2.102 3,102 2 102
Entero~acteriaceae in 1 gram + + +
0.'~ gram + + +
0.01 gram + +
Escher~chia coli in 1 gram
0.1 gram
0.01 gram
TABLE 3
',fect of 5~ ethanol in norm.hexane at d~f~erent contact times, upon the bacterial
charge of de-oiled sunflower flo~r,
Flour de- Flour de-oiled ~ith 5~ ethanol in nor.hexane
oiled with Drying time 48 hours
i~icro2~.010ical Tests Flaked
- nor.hexane Contact tlm~ Contact Contact Contact Sample ~ Sample A
3 ho~rs time lh. time 45 time 30 dried for dried lor
(sample A~ mins. mins~ 12 hours 48 hours
Eacterial Count N/gram /.105 6,1o6 ~.105 2 105 3 1o6 1o6 5~105 7.1~5
S?ore-~C~r~ing ~/gramloS 6.105 105 1o6 3~1o6 1o6 3.105 3.1Q5
Yeasts Nlgram S.103 5.1G' c~ 102 ~ ,0 C 102c~12 2,10 iO
Moulds N/gram 6.10 2,105 2,1~2 2 ~o3 ~ 103 5 103 1o2 2
Entero~acteriaceae in
1 grzm + + _ _ _ _ _
0.1 gram + + _ _ _
0.01 gram ~ T
cscherichia coli in
1 ~ram _ _
0.1 gram
O~Ql gram
TABLE 4
Effect o-, 5~ ethanol in nor.hexane with extrO ratio 1:5 (solid~ uid) at different
contact times, upon the bacterial charge of de-oiled sunflower seed flour.
FLOUR DE-OILED WITH
Microbiological Tests Flaked nor.hexane nor hexane nor.hexane nor.hexane
with 5~ with 5~ with 5%
ethanol ethanol ethanol
(extr.ratio (ex~r.ratio ~extr.ratio
1:5) 1:5) 1:5)
1 hour 2 hours 3 hours
6acterial Count N/gram 7.105 6.105 3.104 4.104 50104
Spore-~orming N/sram ~05 6.105 3.104 4.104 4.104
Yeasts N/gram 8.103 5.103 ~ 10 ~ 10 ~ 10
Moulds N/gram 6.104 2.105 3.103 103 3 103
Enterobacteriaceae in 1 gram + * ~ +
0.1 gram + + +
0.01 gram + +
Esc,herichia coli in 1 gram - _ _ _ _
0.1 gram _ _ _
0.01 gram
TABLE S
Effect of the concentr2tions 2~ and 3~ of ethanol in nor,hexane at different contact
imes, upon the bacterial charge of de-oiled sunflower seed flour.
~lour de-oiled with
nor.hex~ne Witl 2~ ethanol by volume norOhex;ne~ Oe~n~ me
Mikrobiologlcal Tests Flaked nor~hexane l^hour 2-hcur 3-hour 6-hour 30-min l-hour 3-hour
contact con~act contact contact contact contact contact
Bacterial Count N/gram 7.105 6.1o67.105 1o6 7.1056.105 7.105 4.105 3O1U5
Spore-rorming N/gram 105 6.1052.105 lQ5 2.1052.105 5.10 4.105 2.io5
Yeasts N/gram ~.103 5.103 1û2 1o2 1o2 1o2~ 1o2 ~102 C 10
Mouids N/gram 6.104 2.105 3.10 3.10 2.10 2.10 5.10 3 103 2 10
Enterobacteriaceae in
~ gram + + + ~ + +
0.1 gram + + + + + +
0.01 gram + + + +
Escherichia coli in
L gram _ _
û.l gram
0.01 gram
TABLE 6
Effect of the concentration 3~ ethanol by volume in nor.hexane at different contact time
at 60C, upon the bacterial charge of de-oiled sunflower seed flour.
FLOUR DE-OILED WITH
Mikrobiological TestsFlaked nor~hexane nor.hexane with 3~ ethanol at 60C
l hour 2 hours 3 hours
Bacterial Count N/yram 7.105 6.106 5.104 7.104 4.104
Spore-forming N/gram 105 6.105 5.104 7.104 3.10
Yeasts N/gram 8.103 5.103 10 C 10 < 10
MOU1QS N /gram 6.104 2.105 2.103 4,lo2 2.lO
En~erobacteriaceae in 1 gram + + ~ + _
O.l gram + +
O.Ol gram + +
Escherichia coli in l gram
O.l gram
O.Ol gram
