DE3228174A1 - METHOD FOR PRODUCING EDIBLE HYGIENICALLY PERFECT FLOURS FROM OIL-BASED SEEDS - Google Patents

Description

The present invention relates to a process for the preparation of an edible protein-containing flour that is microbiologically is acceptable from oil-containing seeds, both from those with a high oil content such as sunflower seeds, peanuts, Cottonseed and the like, as well as those with a low oil content such as soybeans, grape seeds, sesame seeds, Carthamum or Carthamus grains and others.

In particular, the invention relates to a method of making sunflower meal for both human consumption from peeled and unpeeled sunflower seeds.

The manufacture of components and intermediates for the formulation of final food products requires during of the processing operation and the transformation of the raw materials, the maintenance of the nutritional properties and compliance of hygienic and sanitary provisions for the products to protect the health of the consumer.

The quality of a food depends on numerous different types Factors such as: the chemical composition and quality of the raw materials, the manufacturing technologies and those used in the devices Materials of hygienic and sanitary conditions of the production facility environment and the type of conservation of the Final food product (Nickerson, J.T and Sinskey, A.J.,

1972, Microbiology of Foods and Food Processing - American Elsevier Publishing Co., New York).

At present, the plants intended for the production of food products see in the final process stages or a sanitary treatment or sterilization operation even at any of the intermediate stages.

In particular, the treatment of the type mentioned above is for proteinaceous products made from vegetable grains or Seeds are obtained in which the initial bacterial load is sometimes above that determined by various legal Regulations prescribed tolerance limit is essential. In order to meet such requirements, it is in the industrial Practice required to carry out a sterilization stage, which sometimes takes place under conditions so drastic that structural changes or a reduction in biological ones and nutritional properties of the end products are brought about (Tateo F., 1977, Detergenza e sanificazione nell'Industria Alimentare, AEB Brescia, Italy).

The present invention relates to the industrial treatment of hulled or unpeeled or smooth oil-containing seeds or grains for the production of protein-containing flours with microbiological characteristics associated with the use as human Foods are compatible. For the process of extracting oil from oil-containing smooth or unpeeled or peeled grains or seeds provided mild conditions to achieve protein-containing products of high biological value (DE-OS 29 20 974) required the use of suitable ones Solvents in the extraction operations to produce proteinaceous products regardless of the raw materials used that are microbiologically acceptable.

The solvent to be used consists of a mixture of a hydrocarbon containing one chosen by the oil industry or hydrocarbon compound, generally hexane, and from

an organic compound having an alkyl chain having 1 to 5 carbon atoms and at least one polar group of alcoholic Contains nature, such as ethanol, and which must be thoroughly mixed with the above selected solvent is capable.

The use of, for example, ethanol is made possible by its hygienic effect established by breaking open the cell walls unfolded by the dehydrating effects of alcohol (Verona 0., Picci G., Microbiologia degli Alimenti, 1968, UTET).

The extraction step is carried out using a mixture of a hydrocarbon solvent, hexane, and an organic polar solvent ; Ethanol, at a percentage varying from 1 to 50% on a volume / volume basis.

The solid-liquid extraction is carried out with the aid of a process which is preferably carried out in stages, the individual stages lasting from half an hour to four hours, the solid-liquid ratio at a working temperature of 20 to 60 ^° C. 1: 1 up to 1:40 (as weight / volume ratio).

The solids obtained in this way are then dried for 1 to 60 hours.

It can be seen that the method can advantageously be applied to any mixture consisting of a hydrocarbon compound and an organic compound can be applied. All work details can be found in the examples below.

The examples relate to processes for making edible protein-containing flours or powders made from sunflower seeds. However, these examples are not limiting Invention and can refer to any oil-containing seeds or

Grains are applied. materials

Ethanol and η-hexane from Carlo Erba, Milan, Italy as RPE solvents (Erba Pure Reagent).

The culture media used for the microbiological experiments were: plate count agar, mycological agar, E.E. Mossel broth, Tryptic Soy Broth, Violet Red Bile, Bacto Brilliant Green Bile Broth, and McConkey Agar from DIFCO, whereas Clostridium perfrigens Selective Agar was available from Merck.

Analysis methods

The characterization or determination of the chemical components, of moisture, lipids or lipoids, proteins and raw fibers was made according to the methods of A.O.A.C. (Association Official Analytical Chemists, 11th Edition, 1970).

The phenols were determined by gas chromatography using the direct silylation method.

The soluble sugars were determined colorimetrically by the method of Dubois M. et al (Anal. Chem., 28, No. 3, 350 (1956)).

The microbiological tests were carried out according to the methods described by Mossel D.A.A., Brechet J., Lambion R., in "La prevention des infections et des toxi infections alimentaires ", CEPIA, Brussels (1962) carried out the procedure described.

example 1

The present example relates to the production of de-oiled microbiologically acceptable flour or powder by extraction of oil from exposed sunflower seeds with η-hexane, the ethanol in different volume concentrations (from 1 to 5%)

at an extraction ratio (w / v) of 1:20 and at a temperature of 22 ° C. The drying time was 48 hours at room temperature.

Table I.

Chemical composition of the revealed sunflower seeds, 6.0 based on dry matter, in percent (%) 60.0 humidity 22.0 Lipids or lipoids 2.9 Proteins (N χ 6.25) 3.5 ash 4.4 raw fiber 1.5 soluble sugars 5.7 (by Diffe Phenols (gas-liquid chromatography) renz) Nitrogen-free extract

The revealed sunflower seeds with the specified in Table I above composition were transferred into flakes and batchwise with stirring at a temperature of 22 ⁰ C at a solid-liquid ratio of 1:20 (wt./vol.) In two stages during a Deoiled hour with η-hexane and one stage with η-hexane and ethanol at different concentrations and with a contact time of one hour.

Table II gives the microbiological data for various Ethanol concentrations. The results obtained show the different behavior of the microorganisms the same hygxenic means: the latter is very active against vegetative bacterial strains, the yeasts and the molds, whereas the spore-forming strains are highly resistant. The flour was at ambient temperature before analysis Dried for 48 hours.

Example 2

The present example relates to the production of de-oiled, microbiologically acceptable flour obtained by extracting the oil from exposed sunflower seeds with 5% by volume of ethanol η-hexane at an extraction ratio of 1:20 (pesticide: liquid) at a temperature of 22 ° C.

The flour was dried for 12 hours or 48 hours at ambient temperature.

Uncovered sunflower seeds, the degree of contamination of which was known, with a chemical composition of the type shown in Table I, were flaked with a mixture of η-hexane and ethanol (5% by volume of the latter) and after two stages of a batch extraction with n -Hexane de-oiled for one hour at different contact times. The temperature was 22 ^° C., the extraction ratio (solid! Liquid) 1:20. The drying times of the flour at ambient temperature ranged from 12 hours to 48 hours.

The results given in Table III show that the sanitizing The effect of 5% ethanol in η-hexane is already evident after the first 30 minutes. The drying of the Flour at ambient temperature during various contact times was found to be opposite to the bacterial load of the investigated Products as ineffective.

Example 3

The present example relates to the production of de-oiled microbiologically acceptable flour by extracting the oil from exposed sunflower seeds with η-hexane containing 5% by volume of ethanol at an extraction ratio (solid liquid) of 1: 5 at a temperature of 22 ^° C.

■ The chemical composition is given in Table I above

specified. The extraction of the oil from the revealed grains was carried out with η-hexane in two extraction stages at a ratio of 1:20 (solid liquid) and by a subsequent third stage with n-hexane containing 5% ethanol at an extraction ratio (solid! Liquid) of 1 : 5 carried out at different contact times at a temperature of 22 ^° C. The flour so obtained was allowed to dry under a hood at ambient temperature for 48 hours.

The results given in Table IV show the sanitizing Effect of the ethanol-hexane mixture also for extraction ratios (solid! Liquid) of 1:20 and below, the effect being slightly weaker than that given in Table III of Example 2.

Example 4

The present example relates to the production of de-oiled microbiologically acceptable flour from exposed sunflower seeds by extracting the oil with η-hexane containing 2 % by volume or 3% by volume of ethanol at an extraction ratio (solid: liquid) of 1:20 at a Temperature of 22 ° C.

The chemical composition of the revealed sunflower seeds was as given in Table I above.

The oil was extracted from the revealed grains with η-hexane in two extraction stages at a ratio of 1:20 (solid liquid) / followed by a third extraction stage with 2% by volume of ethanol in η-hexane or 3% by volume. % Ethanol in η-hexane, the extraction ratio being 1:20 at a temperature of 22 ^° C. The flour so obtained was dried at ambient temperature for 48 hours.

The results given in Table V show that the sanitizing Effect of the ethanol ~ n-hexane mixture at a concentration of .3% ethanol in η-hexane with a contact time Is clearly noticeable from 3 hours.

10 -

Example 5

The present example relates to the production of de-oiled, microbiologically acceptable flour by extracting the oil from exposed sunflower seeds with η-hexane containing 3% by volume of ethanol, the extraction ratio being 1:20 (solid: liquid), with contact times of 1.2 and 3 hours at a temperature of 60 ⁰ C.

The chemical composition of the grains revealed was that given in Table I above. The extraction of the oil from the revealed grains was carried out with η-hexane in two extraction stages at a ratio of 1:20 (solids! Liquid), followed by a third extraction stage with η-hexane containing 3% by volume of ethanol at a ratio of 1:20 (solid: extraction liquid) carried out at a temperature of 6O ⁰ C and with contact times of 1.2 and 3 hours. The flour thus obtained was dried at room temperature for 48 hours. From Table VI it can be seen that the use of a temperature of 6 0 ⁰ C does not improve the hygienic effect of the ethanol-n-hexane mixture.

• T ä 'b' ö "1 1 'ä" ¹ II

Effect of various ethanol concentrates in n-hexane with regard to bacterial
Loading of de-oiled sunflower meal.

Number / g in flakes
passed
leads n-hexane .1O ⁶ Flour defoiled with * OK ⁵ . n-hexane with '
4% ethanol .1O ⁵ n-hexane
with 5%
Ethanol • - Number / g 7.10 ⁵ 6th .ίο ⁵ · 5 .ίο ⁵ ·. 2.10 ⁵ - Microbiological
.Testing Number / g 10 ⁵ , 6th .1O ³ 10 ² 5 10 • io ⁵ ·. - bacteria Number / g P.10 ³ 5 .1O ⁵ < .1O ² . <10 ² spore forming I.
Enterobacteriaceae, Ln 1 g 6.10 ^ 2 + 3 2.1O ² - Yeasts + -. Molds +. · - 0.1 g - - • 0.01g - - - Escherichia coli in 1 g - - - - . 0.1 g n-hexane with
1% ethanol 0.01g 7.1O ⁵ n-hexane with
3% ethanol s.io ^ 3 <10 ² 2 6.1O ³ <J Λ. 2 - -

K) CX)

Table III

Effect of 5% ethanol in η-hexane at different contact times with regard to the bacterial loading of de-oiled sunflower meal.

. ■ in
Flakes Meal de-oiled Meal with de-oil 5% ethanol in n- Contact
duration
45 min. ' -Hexane Sample A ge
dries
while
2 hours i I.
I. - passed
leads with Drying time 48 hours 3.1O ⁶ 5.1O ⁵ - Microbiological tests 7.10 ⁵ n-hexane Contact duration
3 hours
(Sample A) Contact
duration
1 hour 3.10 ⁶
■ -Contact
duration
30 min. 3.10 ⁵ - Sample A ge
dries -.
while "
48 hours Bacteria - number / g; 10 ⁵ 6.1O ⁶ 2.1O ⁵ 2.10 ⁵ . <I0 ² - IG ⁶ 2.16 7.1O ⁵ spore forming_ number / g. P.10 ³ • 6.10 ⁵ 10 ⁵ 10 ⁶ IG ⁶ ίο ² . ■ 3.10 ⁵ - Yeast number / g 6.10 * 5.1O ³ <10 ² <ίο ² · <1G ² 10 - Molds number / g ..2.1O ⁵ 2.1O ² 2.1O ³ - 5.1O ³ - ίο ² ; Enterobacteriaceae-in * - - • i "g + - - - - 0.1 g + + · - - - • 0.01 g + - - ■ - - Z Escherichia coli in - - - Day - -. - - - 0.01 g - - -

T a b ο 1 1 e 'IV

Effect of 5% ethanol in η-hexane at an extraction ratio of 1: 5
(Solid: liquid) at different contact times with regard to the
bacterial load in de-oiled flour from sunflower seeds.

I. Arizähl / g 0.1- G in
Flakes
passed
leads —— flour n-hexane 10 * de-oiled with η-hexane with 5%
Ethanol -
[Extraktiorisver-
hSltnis-t: 5) "
1 hour η-hexane with 5%
Ethanol
(Exträktionsvejj-
ratio 1: 5) '
2 hours ■ η-hexane with 5%
Ethanol
(Extraction ver
ratio ... 1: 5)
3 hours • - Number / g 0.01 <f 7.1O ⁵ ' 6th * .io * '..' · 5.10 * - ί
i
I microbiological tests Number / g in ¹ - 1 G 10 ⁵ 6th ίο ³ - '. ■ 3MO ^. * .10 * - Bacteria '^; Number / g 0.1 G 8.10 ³ ' 5. 10 ⁵ - <10 <io ■ <10 . spore forming - Enterobacteriaceae 'iri 1 0.01 G 2. 3/10 ³ IG ³ 3.1O ³ Yeasts G· T- + - Schiirrasl mushrooms - - Escherichia coli + - - - ■. - - - ■ · - - - -

ro ro co

T a b e 1 1 e · · V

Effect of the concentrations of 2% and 3% ethanol in η-hexane at different
Contact times with regard to the bacterial load of de-oiled flour from sunflower seeds.

Microbiological ._.
Tests "" ^r in n-hexane > . flour de-oiled with 2 hours.
Contact 3 hours.
Contact • 6 hours
Contact • - n-hexane with 3% by volume of ethanol 3.10 ⁵
2.1O ⁵ I.
Bacteria. "Number / g
spore forming number / g Flakes
passed
leads 6.10 ^δ
-6.10 ⁵ j. IG ⁶
IG ⁵ .7.1O ⁵
"2.1O ⁵ ' ÖMO ⁵
2.10 ⁵ ' 30 min.
Contact 1 hour. 3 hours
ContactJContact Yeasts "number / g 7.1O ⁵
IG ⁵ 5.1O ³ + n-hexane with 2; vol .-% ethanol IG ² IG ² IG ² - ·· ■ 7.10 ⁵
5.-1O ⁵ · ■
* .10 ⁵ 2.1O ² Umbrella mushrooms number / g 8.1O ³ • 2.10 ⁵ 1 hour
Contact 3.10 ³ 2.1O ³ 2.10 ³ ^ 1O ² - CIG ² ■ Enterobacteriaceae in ^: 6.10 * - ■ - 7.10 ⁵
2.1G? ' 5.10 * .3.1O ³ . - 1 . G - IG ² 0.1 g - 3.10 * • r + - 0.01 g + ■ " Escherichia coli in 4th - - - ¹ "9 + ■ - ' - - - 0.1 g - + - - - ■ - 0.01 g ■ - - - - - - - - -

κ: is:

Tabel

VI

Effect of the concentration of 3 vol .-% ethanol in η-hexane at different contact times at 60 ⁰ C on the bacterial load of de-oiled sunflower flour from grains.

ι; Testing • Escherichia coli 0.1 - in flakes n-hexane • -oil · »- mi * - • . - % Ethanol at
,'2 hours 6O ⁰ C
3 hours ■ I microbiological 'Number / g 0.01 G convicted 6Λ0 ⁶ . • h-hexane with 3
1 hour - • 7.10 * bacteria Number / g · ,, in 1 G . 7.1O ⁵ 6.10 ⁵ ■ •. 5.10 * - 7.10 * 3.10 * • spore-forming Number / g 0.1 ' G ίο ⁵ - '5.10 ³ . 5.10 * .- <19 <ΙΟ Yeasts ■ - , Number / g 0.01 G 8.10 ³ • 2.10 ⁵ <10 '* .1O ² Σ.10 ² Schiirrosl mushrooms Biterobacteriaceae in 1 G .6.10 * + 2'.10 ³ + - G + · + - ■ - + ■ - - - - - -

NJ K) OO

Claims (8)

Claims 1. Process for the preparation of edible microbiologically Acceptable protein flours from oil-containing smooth or undeveloped or exposed seeds or Grains by extraction with one of a hydrocarbon-containing or hydrocarbon compound and a mixture consisting of an organic compound. 2. Extraction method according to claim 1, characterized in that that the organic compound has an alkyl chain having 1 to 5 carbon atoms and at least one polar group of alcoholic Nature has. 3. Extraction method according to one of the preceding claims, characterized in that the oil-containing seeds or grains are preferably selected from among those of the sunflower, the peanut, the cotton, the soybean, among grape seeds and those of sesame or carthamum. . 4. Extraction method according to one of the preceding claims, characterized in that the organic compound is preferably Is ethanol. 5. Extraction method according to one of the preceding claims, characterized in that the hydrocarbon compound η-hexane is. 6. Extraction process according to one of the preceding claims, characterized in that mixtures are used, that of a hydrocarbon solvent and an organic compound in one of 1 to 50% on a v / v basis varying percentage. 7. Extraction method according to one of the preceding claims, characterized in that the extraction temperature varies ^{from 20 0} C to 6O ^{0 C.} 8. Extraction method according to claim 7, characterized in that it is at a solid-liquid ratio which varies from 1: 1 to 1; 40.