FI122664B - Fractionation of nature's raw products and separation of nutrients from them - Google Patents

Description

FRACTION AND SETTING-UP OF NATURAL RAW MATERIALS

The present invention relates to a process for fractionation of natural raw materials by dry methods to different phenolic composition components. The invention further relates to a stripping fraction formed by the method.

Berry raw material is underutilized in Finland. Breads are abundant in Finland and they are functional products that include phenolic compounds, carbon-10 hydrates and dietary fiber. In Finland, however, no efforts have been made to enrich and isolate their most valuable components into pharmaceutical preparations or product enhancements in an economically meaningful way. On the other hand, the Maija raw material exported from Finland is used to make phenolic concentrates by expensive adsorption process, which phenolic compounds, which are natural antioxidants, generally contain high levels of flavonoids in berries. In these concentrates, the phenol content is 25-50 times that of the phenol lipid of the starting material.

In known enrichment processes, phenolic compounds in an acidic aqueous solution are adsorbed to the resin in industrial adsorption columns. The columns are washed with adsor-20 non-carbohydrate sugars, leaving only the fraction containing mainly phenolic compounds on the resin surface. Phenolic compounds are removed from the resin by elution with a water-ethanol solution. The ethanol is evaporated and collected. The phenolic compounds remain in the aqueous solution of the base product, which is usually dried in a spray-dry to a powder. The most energy consuming operations of the process include distillation and evaporation of ethanol and drying steps. Such adsorption operations produce standardized phenol extracts from the berries, typically with a phenol content of 25% by weight. The products are sold as drug-specific CD-ROM preparations.

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Phenolic compounds are very common in berries and contribute to the coloring of berries eu 30. For example, the color of blueberry and shrubbery is largely due to anthocyanins, which are phenolic compounds that are abundant in blueberries. Raspberry, varnish as well

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similarly, honey berries are rich in ellagitannin and cranberries and lingonberries are high in flavonols. In addition to such 2 plates, which are abundant in Finland, for example, phenolic compounds can be enriched from grapes, especially dark grapes.

Blueberry has interesting anthocyanins, which are predominantly dolphinides and have a content of 0.3 to 0.8% fresh weight, depending on growth conditions. In their simplest form, such products are prepared by drying and milling berries or by concentrating and drying maize juice to give concentrations of up to 5-10% by weight on a dry basis (WO 03084559, DE1767614).

10 There is thus a need for a novel process for extracting useful substances from various berries in a simple and energy efficient manner.

BRIEF DESCRIPTION OF THE INVENTION It is an object of the present invention to utilize gentle and simple process steps for enriching nutrients or drug-like substances or substances suitable for such with certain fractions of natural raw materials from which they can be separated.

In particular, it is an object of the present invention to provide a process by which nutrients 20 or drug substances can be extracted and enriched from a berry raw material by utilizing energy-efficient process steps.

The present invention thus relates to a process for fractionating natural raw materials such as berries and separating the nutrients from the formed fractions, wherein the raw material is dried and ground.

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More precisely, the process according to the invention is characterized by what

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x is shown in the characterizing part of claim 1.

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<J> c \ i 30 The berry peel fraction formed by the process of the invention has

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the use of the method according to the invention is characterized by what is claimed in claim 15.

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The invention allows for a more economical utilization of the dishes because the invention seeks to separate the structural parts of the berries or other natural raw materials into various components by dry methods. Preferably, the raw material is a dried whole or, more preferably, a cake, which remains after the juice of the dish is pressed. It is essential to make the compression process and subsequent drying process such that bioactive components such as anthocyanins are not destroyed.

The invention makes it possible to separate from the dish a fraction having a multiple phenol (anthocyanin) content per dry matter compared to the anthocyanin content of an untreated dish. For example, Lätti et al. According to the analysis, the highest anthocyanin content in freeze-dried Finnish blueberry in 2007 was 3.8% by weight. In the method, the juice is squeezed from a berry, and then the phenol (anthocyanin) is enriched from the dried squeeze cake. The proportion of press cake from the starting raw material is generally 10-20% by weight, depending on the efficiency of the pressing process. The extruded cake can be obtained by the process according to the invention from a fraction having a phenol (anthocyanin) content of at least 8% by weight, preferably 15-20% by weight.

Detailed Description of the Invention

The present invention relates to a process for fractionation of natural raw materials, such as dishes, and separation of nutrients from the formed fractions, wherein the raw material is dried and milled. Said drying is preferably carried out at a temperature of -40 ° C to 50 ° C according to the drying method and, accordingly, said grinding is carried out gently so that the berry seeds are separated from the pulp and peel without breaking. If the moisture content is slightly higher, i.e. 10-15%, during drying, the shell part o 25 can be distinguished by abrasive grinding in Large pieces. After drying and milling g, the seeds are separated from the raw material and a second light milling is carried out on the seedless pulp and peel formed so that the nutrients g therein are not damaged to form a fine powder which is screened or graded.

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Separated nutrient from other peelings.

sj- oj 30 LT) O) Section '' Light Grinding '' means that the grinding is done gently

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low mill energy mill. These include, for example, mills with a rotating rotor and a stationary stator with adjustable spacing. Preferably, this is meant a plate mill or a similar mill.

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The invention also relates to a peel fraction made from a berry raw material containing up to 20% by weight, preferably 10-17% by weight, preferably 12-16.5% by weight, of bioactive components such as natural antioxidants.

Berries such as blueberry, shrubbery, lingonberry, blackcurrant, raspberry, lacquer, cranberry or honey berry or a mixture thereof are preferably used as the raw material of the invention. The dark grape is also suitable as a raw material for the invention.

Most commonly, the raw material for the process of the invention is blueberry, lingonberry or blackcurrant squeeze cake or other similar berry squeeze cake. Pickle is an economically good starting point because it is a by-product of juice making. So far, the cake has been mainly a waste product. Seeds with low phenolic content have been isolated from some commercial press cakes. However, according to the present invention, if desired, a phenol-containing seed fraction which also contains nutritive cutin may be isolated.

According to a preferred embodiment of the invention, the juice yield is increased using enzymes. The cake thus formed has fewer sugars with a low glass transition, which in a small amount facilitates drying and subsequent grinding and rating operations. The sugar content which inhibits harmful separation can be reduced by washing the cake with water or an aqueous maltodextrin solution, which increases the glass transition and facilitates grinding and grading operations. The cake thus obtained is dried at a low temperature where the sugar component is predominantly glassy rather than amorphous.

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According to another preferred embodiment of the invention, the berry raw material, which may be a dried whole berry or preferably a by-product of a juice extraction, is dried in a freeze dryer at a temperature of -40 ° C to 0 ° C, or preferably by convective dry

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at about 40 ° C. A suitable dryer may, in addition to a freeze dryer, be a fluidized bed dryer or a belt bed dryer or other similar dryer.

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In dry methods, the raw material is preferably an enzyme-pressed blueberry or blackcurrant or other dish cake. The cake is dried in a controlled manner by a pressing and drying process which allows the preservation of functionally valuable constituents of the Maize material, such as phenolic compounds, and provides a dried product from which the various structural components of the dish, seeds, peel and pulp, are pulverized. and subsequent rankings. The highest phenolic content is in the shell part which should be separated as clean as possible from the other components (example-5 kit 1 and 2).

The low temperature dried Maija raw material is suitably ground with a grinding grinder, which removes the bowl seeds from the dry pulp and skin without breaking the seeds. A suitable refiner is, for example, a KT mill (Kone-10 industrial Oy, Helsinki, 0.15 kW, 2800 rpm) with a rotating rotor and a stationary stator. The clearance between the rotor and the stator can be adjusted. The mill produces a shaking and slightly shearing and striking effect, whereby the milling energy is not enough to break down the seeds in the bowl structure, but they are detached from the matrix and transported whole with the peel and fruit pulp. Preferably, a disk mill 15 or an impact mill with a controlled stroke is used to achieve a milder milling process. Most preferably, a grinding machine such as a plate mill is used, with a grinding grinding method that is the lightest for the raw material.

The mill separates the seeds from the pulp and 20 peel powder from the disintegrated berry matrix. Preferred ways to separate the seeds from the rest of the berry matrix are air classification and screening.

The seedless pulp and peel thus obtained is further ground with a suitable mill, which is preferably a pin mill. After milling, the physiological berry is obtained

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Due to the different grindability of the parts, a certain particle size distribution, preferably cm 0.050-0.75 mm, preferably 0.100-0.350 mm. The powder is graded according to size differences (g) either by screening or preferably by air classification. Suitable classifiers include, among others, x. channel classifier, or zig-zag classifier. Phenols are enriched in the peel fraction where they are present

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more than the pulp. As the particle size decreases to the said size range, the fraction (or portion of the envelope) of your peel can be better distinguished from the pulp fraction.

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The crust which remains larger in size during grinding and can be relatively cleanly separated from the pulp contains, in addition to the phenolic compounds, cutin, which is a good dietary fiber supplement, which is also very fine to produce. As the juice yield has been increased by enzymes, the proportion of squeezer cake has decreased as some of the cell walls have broken down and released more juice. The cake consists predominantly of seeds, a part of the rind and a part of the fruit attached to it. The shell portion to which the phenolic compounds are attached can be separated from the seeds into a fibrous fraction which preferably contains, in addition to the phenolic compounds, cutin.

The present invention can be utilized, inter alia, in the preparation of extracts enriched in phenolic compounds such as anthocyanin, ellagitannin or flavonols or a mixture thereof. The concentration of these compounds in the extracts may be up to 25% by weight, preferably 10 to 25% by weight, most preferably 15 to 25% by weight. Optionally, the extracts are additionally rich in fibers and other fibrous compounds such as cutin, preferably in a concentration of up to 25% by weight, more preferably 10-20% by weight, most preferably about 15% by weight.

Examples 15

Example 1 - Fractionation of Raw Material

The bilberries were freeze-dried, whereby, during drying, the bilberry's flesh and seeds are partially packaged into a separated fraction from which the rind can be easily isolated. The can 20 portion was cleanly separated from the flesh and seeds by lightly grinding with a counting wheel and separating the shell portion separately by the air stream that carried the shell portion from the seeds and the pulp portion on the table. The anthocyanin (AC) content of the shell part was obtained at 19.1% by weight. Thus, most of the anthocyanins of blueberries are contained in the shell and remain well in the earth at temperature drying.

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cm Example 2 - fractionation of the raw material cp

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Door x Freeze-dried blueberries were milled on a KT mill with a clearance setting of 8.

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The bilberry shell was separated from the sieve 0.750 mm by pneumatic air flow. The anyanide content of the fraction was 12.6%.

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Table 1. The anthocyanin content of the blueberry fractions ground on a counting mill by mouth a

Screen aperture Anthocyanins 355-475 pm 2.7% 250 - 355 pm 7.9% less than 250 pm 6.1%

Thus, with a high proportion of seeds, the anthocyanin content is low. Seeds can be efficiently separated by screening at 355 to 400 µm if they remain intact in the milling process. In a very fine powder, the anthocyanin content also decreases as the pulp fraction increases.

Example 3 - Use of Enzyme Assisted Cake, Raw Material Fractionation and Separation of Peel Section 10

The frozen industrial press cake, which used commercial Pec-tinex enzyme preparations to ensure juice extraction, was dried in a convection oven at 40 ° C.

A dip cake mill (KT mill), a Frisch laboratory mill with a 1 mm sieve, and a Hosokawa-Alpine 100 UPZ pin mill at 17000 rpm were used to grind the dried cake. Fractions passing through a sieve less than 1 mm were screened using a Buhler sieve set. The fractions from the different mills are described in Table 1.

^ 20 Table 2. Distribution of fractions obtained with various mills ^ Screen aperture Fritsch 1 mm sieve Counting mill Mill mill g 630 pm 22 g 9.5 g 1 gc 355 pm 35 g 58.4 g 9 gc 250 pm 15 g 27.4 g 6 g σ> 180 pm 9.1 g 14.7 g 6 g ____ ίο less than 180 pm 18 g 25.4 g 26 go ---- o

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After gentle counting mill milling, a powder having a permeability of anthocyanes of less than 250 µm was obtained. Less than 250 pm, the seed-free fraction was ground in a Frisch 8 mill equipped with a 0.14 mm sieve. This fine fraction was subjected to an air jet sieve screen. Nothing went through the 45 μηι screen. A small portion of the powder collected from the sieve vacuum chamber passed through the sieve at 71 pm and 100 pm. The fraction milled with a pin mill was the smallest size. It was classified for analysis in the fine fraction with a British Rema Mini Split classifier at settings of 3500 rpm / 220 m3 / h. Fractional analysis results are shown in Table 3.

Table 3. Results of analysis of milled and screened fractions

Grinder Screen size Anthocyanins (mm) (% by weight)

Pellet mill Φ> 1 8.8

0,2 <0.250 16J

Fritsch Mill Φ <0.100 15.6 0.100 <Φ <0.250 15 ^ 6 Φ <0.071 Ϊ5 / 7

Pin Miller Rating fine fraction 13.8 4000/220

As can be seen from the table, the fine grinding of the fraction below 250 µm only eliminated the fraction with an air 10 classification, where the anthocyanin content, 13.8%, was lower than the anthocyanin content of the starting material, 16.1%. The differences in screening were smaller because both the peel and the pulp were ground to a fairly homogeneous powder.

The results show that properly treated blueberries, which do not suffer from heat damage during the process, can be mechanically separated from anthocyanic concentrates.

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Example 4 - Use of an cake without enzyme treatment, fractionation of the raw material and separation of the crust

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Q) 20 Dried blueberry squeeze cake from a commercial jam making process consisting of seeds and peel and pulp was dried at about 40 ° C and milled using a Salt Mill (KT mill). The powder was screened on metal screens to give the fractions and anthocyanin concentrations shown in Table 4.

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Table 4. Analysis results for different size fractions

Screen size pulp AC content (mm) (g) (wt%) Φ> 0.475 ITS E5 0.250-0.475 2Ä 4 Φ <0.250 ϊΰ> 7/7

The seed fraction is largely retained on a sieve of 0.475 mm and finely divided anthocyanic concentrates.

Example 5 - Enzyme Assisted Cake Cake Formation, Raw Material Fractionation and Seed Separation

Blueberry was pureed. Crushed blueberries were treated with Pectinex Smash XXL L. Enzyme was added: Pectinex Smash 10 nkat / g, or 0.29 ml / 1 kg brush (active.

10 34900 nkat / ml), and Alcalase 2.0T and blueberry puree were treated with enzymes for 2 hours at 45 ° C. The juice was pressed with a Hafico High Pressure Tincture Press H P5 press to give the cake 12-14% by weight of the starting material and the cake dry matter to be as high as 40% by weight. The cake was washed with water and squeezed again. The cake was dried on an Aeromatic fluidized bed dryer at 36 ° C with an air flow rate of 93% to dry matter.

The dried cake was ground with a counting mill (KT mill) with a pass (setting 5) where the seeds do not crush. The seeds were separated using a British Rema air separator. The proportion of coarse fraction, i.e. seeds, remained high, about 81-88%, and the coarse fraction still contained cell walls. The fine fraction accounted for 12.2% by weight and had an anthocyanin content of 2020 7.7% by weight.

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Thus, the coarse fraction of the air classification was screened with wire mesh screens, leaving all seeds jr 0.475 mm, with little seed pellet and anthocyanins cd enriched in smaller particle size (Table 5).

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Table 5. Analysis results for fractions of different size classes

Screen size pulp AC content (mm) (%) (% by weight)

0.250-0.475 66 6J

Φ <0.250 36 8J

From the seed fraction over 0.475 mm, the cell wall and the peel fraction were separated and the fraction was milled on a KT mill and sieved on a 0.250 mm sieve. The anthocyanin content of the fraction remaining on the sieve was 9.1% by weight. In other words, the husk portion remains in the seed fraction, from which it can be further separated by screening or air grading after grinding the seed-free husk fraction.

Example 6 - Fractionation of Raw Material and Separation and Analysis of Different Fractions 10

The blueberry fraction, which had passed a 0.250 mm sieve, milled on a KT mill mill was classified with a British Rema classifier at 3500 rpm and an air flow rate of 220 m / h for fine and coarse fractions (see Table 6).

15 Table 6. Analysis of fine grain and coarse grain to yield

Fraction fraction AC content (% by weight) (% by weight)

Fine ae 60 7.3

Coarse fraction 40 8.5

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The anthocyanin is mainly enriched in the coarse pellet granule and the less granular fine pulp granule.

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ir 20 Example 7 - Drying and Fractionation of Raw Materials and Separation and Analysis of Different Fractions Q_ <j) Sounding

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having an anthocyanin content down to 0.2% by weight, was milled on a KT mill with a clearance of 1 setting 6 and sieved on a 0.8 mm sieve. The fraction passed through the sieve was milled on a counting mill 11 (KT mill) with a clearance setting of 4 and air graded on a British Rema classifier at 2500 rpm / 220 m3 / h. The seed-free fine fraction was screened to give the fractions described in Table 7 with an anthocyanin content greater than 10 times the starting material.

5 Table 7. Anthocyanin content of fine fraction of blueberries ground in a pulverized mill (KT mill) and subsequently air-classified

Screen size portion AC content (mm) (%) (wt%) 0.315 34 2 ~ 22

0.210 -0.315 17 2J

0.100-0.210 27 2J

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Claims (15)

1. Process for fractionation of natural raw ingredients selected from berries and grapes and separation of nutrient-rich fractions from other formed fractions, in which process the raw material is dried and ground, characterized in that - the drying is carried out at a temperature ranging from -40 to 50 ° C. , the grinding is easily carried out in such a way that the seeds of the raw material are separated from the pulp and peel portion without being separated, and from the dried and ground raw material the seeds are separated and a second light grinding is carried out in the formed free-free pulp and peel fraction in such a way that the nutrients therein are not damaged, forming a powder, wherein the shell portion remains in larger pieces separable from the pulp portion, and which powder is sieved or classified in such a way that a phenol-compound shell powder fraction can be separated from the other fractions. 2. A method according to claim 1, characterized in that the natural raw material is derived from berries, preferably it is dried whole berries or a by-product for pressing juice from whole berries pressed pressed cake, preferably a pressed cake. Method according to claim 2, characterized in that the whole berries are blueberries, American blueberries, lingonberries, blackcurrants, raspberries, cloudberries, cranberries or oak berries or a mixture thereof. Method according to claim 2 or 3, characterized in that the pressed cake used as a carrier ingredient is produced by enzyme-assisted juicing, wherein enzymes are supplied to the whole berries in a sufficient quantity to change the sugars contained in the berries. sugar with a low glass transition, whereby the juice exchange of the pressing rises to 80 - 90% by weight g and the formed pressed cake becomes easier to classify. The process according to claim 1 or 2, characterized in that the drying is carried out in a freezer dryer at a temperature of -40 ° C - 0 ° C. CM Process according to claim 1 or 2, characterized in that the drying is carried out by convective drying, preferably by means of a fluid bed dryer or continuous dryer, at a temperature of about 40 ° C. Method according to any of the preceding claims, characterized in that the grinding of the fox is carried out by means of a rubbing grinder with a rotating rotor and a stationary stator, by means of which the seeds are detached from the shell and the pulp of the raw material without being decomposed. Process according to Claim 7, characterized in that the seeds released from the shell and the pulp are separated by air classification or salting. Method according to any one of the preceding claims, characterized in that the free pulp and peel fraction is subjected to a second grinding, preferably by means of a tapping disintegrator, whereby a particle size distribution is obtained, which is preferably from 0.050 to 0.75 mm, after which the powder formed is classified according to size differences, either by partial settling or by air classification. Process according to any of the preceding claims, characterized in that nutrients containing bioactive components such as phenols, preferably anthocyanin, ellagitannin or flavonol, or a mixture thereof, are separated from the saturated or air-classified shell powder fraction. . Method according to any of the preceding claims, characterized in that the halide of the separated nutrients in the formed shell fraction forms up to and including. 20% by weight, preferably 25 to 10% to 17% by weight, most preferably to 12% to 16.5% by weight. i (M 0 2 g> 12. A shell fraction formed from a carrier raw material in accordance with a method according to any of claims 1-11, characterized in that it contains nutrients containing bioactive components in such a way that The phenol content of the fraction is at least up to 8 wt.%, <£ J up to 20 wt.%, calculated on the basis of the shell fraction. An oo CM 3 shell fraction according to claim 12, characterized in that the bioactive components are phenols, preferably anthocyanin, ellagitannin. or flavonol or a mixture thereof, and optionally, also, cutaneous. Peel fraction according to claim 12 or 13, characterized in that it is produced by drying the carrier material at a temperature of -40 - 50 ° C, by grinding the dried raw material in such a way that the carrier seeds are separated from the pulp. and the peel portion without being disrupted, by separating the seeds from the dried and ground raw material and by subjecting the formed seedless pulp and peel fraction to a second grinding, forming a fine powder which is sown or classified for to separate the peel fraction from the pulp fraction. The use of a method according to any of claims 1-11 for separating nutrient-rich fractions from a carrier raw material. OJ δ {M (M O and (M x and CL and c \ i m and o o CM