CZ20001226A3 - Treatment process of lupine seeds containing alkaloids, oils and proteins - Google Patents

Abstract

Method of treatment and processing of lupine seeds, for production of lupine seed products by specific fractionation it consists of a combination of the following steps: comminution and / or shaping lupine seeds into platelet flakes indirectly introducing heat into the platelet-shaped flakes far-reaching exclusion of water, de-oiling of flakes by introducing a solvent to obtain lipids and flakes reduced lipid content, removing bitterness in flakes reduced lipid content by aqueous procedure removing bitterness to obtain a purified product with reduced alkaloids and aqueous extract.

Description

Process for treating and processing lupine seeds containing alkaloids, oils and proteins

Technical field

The invention relates to a process for the treatment and processing of lupine seeds containing alkaloids, oils and proteins for the production of lupine seed products by selective fractionation.

BACKGROUND OF THE INVENTION

Proteins are considered to be raw materials for the food and food processing industries and are used for numerous applications in industrial chemistry, eg for the production of binders or adhesives, emulsions for photographic layers as well as cosmetics, only a few of which are named.

As proteins are an essential component of animals and plants, they are renewable natural raw materials that can be produced on an industrial scale, for example, from milk, soybeans and wheat. Lupine seeds, respectively. lupine seeds, which are similar to soybeans in their composition with respect to protein levels, percentages of crude fibers and oils, are particularly important for protein production. Growing lupins and processing lupine seeds to produce desirable protein products are therefore of particular interest since lupines can be grown in areas not suitable for soybeans, such as in Western Europe or Australia.

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The direct use of lupine products, especially for food applications, is limited due to the plant's own characteristic bitter substances, the so-called alkaloids, and even in the case of the so-called bitter lupins that are suitable from a cultivation point of view are even completely excluded. When processing lupine seeds, it is therefore necessary to exclude alkaloids in order to obtain products for use as food products. At the same time, the extracted alkaloids can be selectively used as active ingredients in agriculture and pharmacy, giving a complete utilization of the scupines, respectively. bitter lupine, which is also extremely economically interesting.

German patent DE 537.265, which was published in 1931, for example, discloses a method for the useful utilization of theupins with the removal of their bitterness by successive extraction with aqueous solutions. This bitterness removal is accomplished by successively extracting the lupine chips in the wet state, adding the appropriate acid, and then dissolving the salts formed in the acid bath.

In addition, WO 83/00419 discloses a method and apparatus for eliminating characteristic bitter substances from bitter lupine seeds, according to which lupines in very finely ground form are countercurrently flushed with lupine extract solutions of various concentrations using water as the solvent.

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An improved method of removing bitterness bitterness can be found in WO 97/12524. which discloses the initial crushing of lupine seeds to form coarse sand-like granules having a diameter of between 200 to 600 µm, and then heat treatment of the plant seeds, thereby achieving selective deactivation of the enzymes present in the plant seeds. The thermal effect is generated directly by the preheating technique, ie by direct introduction of hot steam into the crushed or pulverized seeds. After this preheating operation, the plant seeds are subjected to a bitterness removal process, which comprises two steps, the first extraction step resulting in the separation of alkaloids and other non-nutrients. Finally, the plant seeds are mixed with fresh drinking water as a solvent in an acidic environment for countercurrent extraction. This mixing operation may preferably be carried out in several stages until a non-nutrient-enriched extract and a leachable purified product that is rich in protein and litter or bulk feed are formed. The purified product produced from the first extraction step is added in a second step with water as a solvent to an alkaline medium. As a result of the extraction in the second step, both the purified product by the respective raw materials and protein milk proteins are produced.

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All of the previously described bitterness removal methods are based on a common goal, i.e. firstly to produce proteins in the purest form possible, and secondly, to obtain as completely as possible the bitterness-free raw materials for the food or food processing industry.

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However, the above-described methods also entail various substantial disadvantages: on the one hand, plant seeds, and especially lupine seeds, have a percentage of oils of about 10-15%, which contain not only pure oil, such as trigly cerin, but also lipophilic cunt linear components such as carotenoids, lecithins or lipophilic alkaloids. In particular, these latter components can be leached only inadequately by the known bitterness removal methods, so that the bitter-free end products contain the inevitable residual components of the lipophilic alkaloids.

Although the known method of WO 97/12524 provides the deactivation of enzymes present in plant seeds, which precedes the bitterness removal process, whereby the occurrence of enzymatic oxidation of the unsaturated fatty acids present during the storage of the bitterness-free products from the process may be avoided, produce a rancid odor which would be disadvantageous for use in the food sector; however, this inactivation is carried out that the plant seeds are, although the enzymes are pre-heated, which means subjected to hot steam, which, inactivated, is also inevitably harmful to the accumulated proteins such that they lose their natural form and properties.

Finally, the formation of crushed lupine seeds also contributes to the success of the bitterness removal process. E.g. the shape of the coarse sand granules proposed in W'O 97/12524 is inappropriate if it surrounds a relatively large volume from which the individual components to be extracted,

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• 9 0 »· must be eliminated, which means that the substances to be extracted can leave the coarse sand lupine seed components to be free of bitterness, the less easily the greater the distance from the inside of the volume to the outside each coarse sand granule. On the other hand, it is proposed in WO 83/00419 to comminute lupine seeds to be debased to form an ultrafine flour having a grain size of between 1 gm and 50 µm, but this gives rise to problems in engineering processes where liquid and solid are separated. phase due to the fine grinding of the lupine seeds to form the meal, although the individual extraction paths within the 'dusty grain' are kept very small. This requires complex filtration steps, which are costly in engineering and include a significant cost and time factor in industrial applications.

SUMMARY OF THE INVENTION

The present invention is based on the problem of proposing a process for the treatment and processing of lupine seeds containing alkaloids, oils and proteins for the production of lupine seed products by selective fractionation in such a way that the products, proteins in the purest form and be free of the characteristic bitter substances as completely as possible, while the operational steps to be taken one after the other should require the smallest possible industrial costs. On the one hand, particular attention must be paid to the fact that the proteins being treated must remain unchanged in their natural form, whereas the enzymes contained 0 · 0 0 0 0 0 0 0 0 0 0 0 0 0 0

00 «00» »··· * · 00 in lupine seeds are deactivated, and in particular lipophilic alkaloids must be extracted largely as completely as possible. The method is intended to include the simplest, mutually matched steps of the process to substantially improve the degree of bitterness bitterness achieved hitherto, or substantially reduce engineering costs with the same bitterness removal result.

In accordance with the present invention, in a method for treating and processing lupine seeds containing alkaloids, oils and proteins, for the production of lupine seed products which may have either a penetrating taste or a risk. bitter dandruff, or poor in characteristic bitter properties, the following steps of the process are carried out by selective fractionation:

First, the lupine seeds are peeled and the husks are divided. For further steps of the process it is particularly advantageous to sort the lupine seeds by shape and size before or during the peeling. For this procedure, sieves of appropriate mesh size may be used to carry out the sorting operation. The peeling operation is carried out by the so-called cold process, in which lupine seeds are halved and subsequently dehulled. Then the fleshy seed kernel is crushed or comminuted, respectively. shaped so as to form platelet-like flakes which are exposed in this form to indirect heat transfer when water is largely eliminated. These flakes are preferably formed by fefe fefe fefe fefe fefe fefe fefe fefe fefe fefe fefe fefe fefe fefe fefe fefe fefe fefe fefe fefe fefe fefe fefe fefe fefe fefe fefe fefe fefe fefe fefe fe ·· ·· fefe using flocculation rollers having an intrinsic temperature below the denaturing temperature of lupine proteins, ie less than 40 ° C.

Due to the slight indirect heat transfer, the enzymes contained in lupine seeds are deactivated, while proteins still largely retain their original shape and functional properties since they do not come into direct contact with water, which would damage the natural properties of these proteins.

In accordance with the present invention, the flakes are now subjected to a selective de-oiling process using an appropriate solvent, preferably hexane, which allows the extraction of the lipids contained in the platelet-like flakes. In particular, the extracted lipids also relate to all lipophilic alkaloids contained in lupine seeds which can be isolated by de-oiling so that only lipophilic alkaloids are still present as characteristic bitters in hexane-soaked platelet flakes, which can then be extracted in the subsequent bitterness removal process. . Then, the benzenes are preferably slightly removed from the hexane-impregnated meal, for example with supercritical hexane.

What has proven to be particularly suitable is the indirect heat treatment of the de-oily flakes, which can be carried out, for example, by means of a heat sink or trough.

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In order to remove bitterness of platelet-like flakes which are free of benzene and have a reduced lipid content, these flakes are subjected to an aqueous fractionation process consisting essentially of two steps:

Initially, the de-oily flakes are introduced into an aqueous acidic environment, where all of the substances present in the flakes are dissolved and can be dissolved in the acidic region. As a result, an acidic aqueous extract is obtained, which mainly contains alkaloids and also a bitter-free purified product, insoluble in an acid medium, consisting essentially of a flocculent material.

The flakes thus extracted, also referred to as flour, can then be subjected to further subsequent extraction, which is aimed at producing isolated proteins or appropriate thickenings. Aqueous systems are also included in the subsequent extraction, which may be connected in several successive stages. The solid and liquid phases may be separated by decantation which provides the protein extract as well as the protein extracts or portions thereof as a product, with the protein fraction remaining in the remaining flocculant capable of being controlled by the specific conditions of the process such as pH, extraction time and temperature.

If the purified product, insoluble in acids, is placed in an aqueous alkaline medium in which they are dissolved

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0 · 0 0 · ·· 000 ·· 00 All those substances that dissolve in the alkaline range, ie at pH values higher than 7.5, a purified product with reduced alkaloid content is obtained as a final result, which is available immediately after the second of the process, wherein the purified product is free of any lipophilic alkaloids or acid-soluble alkaloids.

Overview of the drawings

The invention will be described below, without limiting the general inventive idea, by way of example embodiments with reference to the drawing in which:

Figs. 1, 2 are schematic views of a given method of de-oiling and removing bitterness of alkaloid-containing lupine seeds.

EXAMPLES AND INDUSTRIAL APPLICABILITY

Giant. 1 is a schematic block diagram of the first 3 stages of the method. In the first step 100, lupine seeds are prepared, in the second step of the process 200, de-oiling is performed and the bitterness is removed in the third step of the process 300.

Lupine seeds as a raw material are the starting point of a given process, when they are crushed or ground and peeled in the preparation stage. Lupine seeds that are in this way «to» this to in »4 to« to »to This is then separated into, then formed into flakes, preferably in a subsequent rolling operation, which means that the lupine seeds are compressed to form seed fragments, having a typical plate thickness between 300 and 400 μιη. Already during the rolling operation, heat can be selectively and indirectly introduced into the lupine seeds by heating the used rolls. In addition, heat pans on which lupine seeds can come can be used. As a result of this heat transfer, the basic seed enzymes are deactivated so that later enzymatic fat oxidation processes that can lead to rancid odors can be prevented beforehand. The lupine seed, which is shaped to form the flakes and which has been enzymatically deactivated, is now transferred to a subsequent de-oiling process 200, in which the flakes are exposed to hexane as a solvent for the extraction of any lipophilic substances, such as e.g. , triglycerins and crude lecithins, but especially lipophilic alkaloids. This is typically done in a continuous or rotary extractor. The liquid phase is subjected to a distillation process in which hexane is first recovered as the solvent used to make hexane available for reuse, and secondly, the extracted crude oil R can be purified by λ / another refining operation not illustrated in the figure. In addition, the purification of the crude lecithins is continued while using the acid.

Hexane-impregnated de-oily flakes that are present after the extraction process at de-oiling stage 200 are insulated • 44 »4 Τ ··· · * ··

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4 44 4 4444 • 44 44 4 * 4 · 4 4 «44 as lightly as possible from the solvent, ie they are solvent-free. In this process, it is of particular importance that the solubility of the proteins be maintained as far as possible on an industrial level or be selectively modified. Finally, the hexane-soaked flakes are freed of solvent under low water conditions, for example, using an overheated solvent.

The oily flaked lupine seeds thus prepared are free of any alkaloids still present in the lupine seeds during the bitterness removal 300. Depletion of bitterness is carried out in a manner known per se in several stages in an aqueous process in which the alkaloid extraction can proceed continuously, to the vasicontinuously or discontinuously, as shown in Fig. 1.

First, the de-oily flakes are introduced into an acidic environment in which all of the substances, and in particular alkaloids, are soluble in an aqueous acidic medium, preferably at a temperature lower than room temperature. This stage of the operation is carried out in several stages, as can be seen in the bitterness removal process 300 in Fig. 1. At each stage of the process, an appropriate isolation of the aqueous extract present at that stage from the purified acid-insoluble product is performed, preferably by centrifugation. using the appropriate decanter. Finally, the decanter is cooled and rinsed with water or aqueous extract in the area of the solids trap.

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Implementation of selective recycling of the aqueous extract from one stage of the process to the immediately preceding stage of the process and additional or alternative selective extrusion of the aqueous extract from the respective stage of the process to increase the concentration of the purified acid-insoluble product has proved particularly advantageous for improved isolation of the aqueous extract from the purified acid insoluble product.

E.g. it is possible to selectively adjust the ratio between the purified acid-insoluble product and the aqueous extract to less than 10: 1 at a particular stage of the process, e.g., the first stage, by admixing one portion of the aqueous extract from the immediately following process step, e.g. extract of the second stage so as to obtain an appropriate concentration of the components dissolved in the aqueous extract which is as high as possible. Similarly, the ratio between the purified acid-insoluble product and the aqueous extract, e.g. in the second stage of the process, can be set to a value greater than 10: 1 by separating one portion of the aqueous extract at this stage of the process. Thus, the concentration gradients of the substances to be dissolved can be increased within the liquid phase while the given extraction is accelerated. An appropriate flow divider is used to separate this one portion of the aqueous extract. A separate partial flow can be used for other applications or can be discarded.

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The treated flakes then arrive at the protein extraction step 400 of Figure 2, in which the flakes are, for example, exposed to an alkaline environment maintained at temperatures above room temperature, preferably between 35 ° C to 45 ° C, while fractionating between the purified product. and protein extracts. The precipitation of proteins from the protein extract may be carried out in an acidic medium. Whey produced during protein precipitation, having a pTI value corresponding to the pH value of the acidic environment for removing bitterness bitterness inside the removal step 300, can be recycled again to the bitterness removal process 300 in a closed circuit. Whey produced during fractionation as well as protein precipitates contain more than 85% solid state proteins, whey is preferably produced by means of an appropriate decanter. Then the whey thus produced is subjected to subsequent purification by settling in the respective separator and heat treatment. The whey was preferably cleaned a second time in a separator.

The whey thus purified twice is recycled again to the process, with the solids produced from the first separation in the protein strand being further processed, while the solids produced in the second separation are separated.

The reduced protein residue was passed as a flow of substance to the processing stage of the respective raw materials, where the purified product is obtained in the area of the raw material processing plant 6 00 where the flakes are neutralized

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4 44 by an appropriate supply of acid and are then dried. On the other hand, the protein extract produced during the protein precipitation stage can provide the protein product directly by appropriate neutralization with addition of an alkaline medium and subsequent drying. As an alternative, it is possible to modify the functional properties of the respective portions of the protein extract at step 500 of the process 500 by suitable heat treatment or selective application of radio frequency fields, resulting in a purified protein product upon drying.

In addition to obtaining products from the purified product corresponding to the pretreatment as well as protein products, the characteristic bitter extracts can also be selectively derived from the bitterness removal process and are also produced in the form of an extract containing the characteristic bitters, e.g. . Finally, the bitter extracts are selectively separated from the bitterness removal process 30 which, after suitable treatment steps such as fine separation, neutralization and evaporation, yields the final product.

It is also possible to mix the extract containing the characteristic bitter substances with the husks removed in step 100 of the process. The extract thus produced and fixed to the skin can then be dried. An essential aspect of the present inventive method of treating and processing lupine seeds containing alkaloids, oils and proteins is that lipophilic alkaloids, which are extracted very widely within the generational process

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990,000 were difficult to eliminate from lupine seeds in the previous de-oiling step. In this way, it can be largely avoided that the alkaloids are still present in the products obtained at the end of the process. The crushing or grinding of the lupine seeds according to the invention to form the respective flakes contributes equally to the condition that, firstly, the characteristic bitter substances contained in the lupine seeds can be completely eliminated from these seeds and secondly that the liquid and solid phases can be from an industrial scale is not problematic. In addition, the extraction behavior of alkaloids in aqueous systems is substantially improved by eliminating lipophilic components in seeds. This produces advantageous effects in particular on the necessary residence times at the various stages of extraction.

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List of reference numbers

100 Seed preparation, flake formation, deactivation

200 De-oiling

00 Removing bitterness

400 Protein production

500 Protein purification

600 Processing of purified product

700 Processing of bitter characteristics

Claims (25)

A method for treating and processing lupine seeds containing alkaloids, oils and proteins for the production of lupine seed products by selective fractionation, comprising the following steps: comminuting and / or shaping the lupine seeds to form platelet-like flakes, indirectly introducing heat into the platelet-like flakes, water being largely eliminated, de-oiling platelet-like flakes by introducing solvent to obtain lipids and lipid-reduced flakes, lipids by an aqueous bitterness removal process to obtain a purified reduced alkaloid product and an aqueous extract. Method according to claim 1, characterized in that said crushing or crushing of the plant seeds is carried out by means of a flake-forming roller after the pre-comminuted peeled or unpeeled seeds contained in the plant seeds. Method according to claim 1 or 2, characterized in that said lupine seeds are classified according to their shape and size before comminution and / or shaping, and are subsequently peeled. fe fe • fe • fe • fefefe • • fefe fe * fefefe • fefefe • fefe feef fefe feefefe fefe fefe fefe fefe fefe fefe fefe 1 8 Method according to any one of claims 1 to 3, characterized in that said peeling operation is carried out in accordance with a so-called cold process in which lupine seeds are halved and separated from the husks. Method according to any one of claims 1 to 4, characterized in that said flocculation is carried out by means of flocculation rollers having a temperature below the denaturing temperature of the lupine proteins, preferably below 40 ° C. Method according to any one of claims 1 to 5, characterized in that the platelet-like flakes have a platelet thickness of less than 1 mm, preferably 200-400 µm. The method according to any one of claims 1 to 6, characterized in that the seeds proper to the enzymes are deactivated by indirectly introducing heat with proteins which mostly retain their natural properties. The method of claim 7. characterized in that said indirect heat introduction is performed by preheated flocculation rolls, by means of which the plant seeds are comminuted and directly heated. Method according to any one of claims 1 to 8, 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 00 00 0 0 0 0 Characterized in that industrial hexane, pentane, hexane, heptane, or heptane is used as the solvent for de-oiling said platelet-like flakes; supercritical CO ₂ . The method of any one of claims 1 to 9, wherein said platelet-like flakes are solvent-free under low water conditions or in the absence of water. Method according to claim 10, characterized in that said solvent removal step is carried out with a superheated solvent, which is preferably hexane or industrial hexane. Method according to any one of claims 1 to 11, characterized in that said indirect introduction of heat into already de-oily flakes is carried out by means of a heat pan. The method according to any one of claims 1 to 12, characterized in that said de-oily and solvent-free flakes are transferred to a bitterness removal process having the following two stages: in the first stage of the process, the flakes are introduced into an aqueous acid medium to isolate the substances soluble in the acid medium to obtain an aqueous extract as well as a purified acid-insoluble product, 0 0 * 00 »» 0 * 00 000 0000 • · · 0 0 000 0 0 · 0 0 000 00 0 000 00 0 • ·· # 0 0000 0 · 0 00 0 · ··· 00 00 - in the second stage of the process, the purified product, insoluble in the acidic region, is introduced into an aqueous alkaline medium to obtain aqueous extracts as well as the purified products insoluble in both the alkaline and acidic regions. The method of claim 13, wherein said aqueous acidic medium has a temperature below room temperature in the first stage of the process. A method according to claim 13 or 14, characterized in that the isolation of said aqueous extract from said purified acid-insoluble product is carried out by centrifugation using a decanter or settler and that said decanter is cooled and rinsed with water or extract in the catcher region. or solids separators. Method according to any one of claims 13 to 15, characterized in that in the second step of the process, the temperature during extraction in an aqueous alkaline medium is higher than room temperature, preferably between 35 ° C and 45 ° C. A method according to any one of claims 13 to 16. characterized in that said first stage of the process is carried out in a multi-stage aqueous acid process, wherein in the step of said process, to adjust the ratio between < - &gt; 4 4 4 4,000 44 4 4 4 4 0 0 4 * · 4 4 4 4 4 4 4 444 44 44 444 94 94 by said purified acid-insoluble product and aqueous extract to a value less than 10: 1, after which one part of said aqueous extract is admixed to the immediately following step of the process. 18. The method of claim 17, wherein, to adjust the ratio between the purified acid-insoluble product and the aqueous extract to greater than 10: 1, one portion of the aqueous extract is separated in an immediately subsequent process step. The method of any one of claims 13 to 18, wherein said aqueous extraction process is a closed circuit providing the following stages of the process: the de-oily flakes are suspended in water at a pH of about 3.5-5.5 to extract alkaloids; in the production of proteins, the suspended flakes, the so-called purified product, are mixed with lye at a pH between 6.5 and 8.5; divided by the decanter into purified product and protein extract, the acidic medium is again added to the protein extract so as to achieve a fractionation of whey and protein precipitates, and the whey is completely delivered to the pre-extracted flakes again at a pH of about 3.5-5.5 . «· To * 00 0 0 000 000 « 0 0 0 0 0 000 0 0 0 φ 0> 00 0 · 0 000 00 0 • 0 00 0 0000 0 · 0 00 00 · 00 00 00 Method according to claim 19, characterized in that the separation of whey and protein precipitates containing more than 85% of proteins in solids, preferably more than 90% of proteins in solids, is carried out by means of a decanter. Method according to claim 20, characterized in that the whey thus produced is subjected to a subsequent purification by means of a separator, then a heat treatment and then a second purification or clarification in the separator. The method of claim 21, wherein the twice clarified whey is recycled to the process with the solids produced in the first separation in the protein branch, which is further processed, while the solids produced in the second separation are separated. A method according to any one of claims 19 to 22, characterized in that the production of proteins is carried out at several pH values such that fractionation of the proteins is carried out. A method according to any one of claims 19 and 23, characterized in that the protein-reduced residue has a protein content of less than 20%. 4 4 444 4 4 4 · 4 4 4 4 4 4 4 4 4 4 4 4 44 44 And that the percentage of coarse materials is greater than 60%, preferably greater than 70%, and that the percentage of soluble carbohydrates is less than 5%, preferably less than 1%. A method according to any one of claims 2 to 24, characterized in that the husks separated before de-oiling are mixed with said alkaloid-containing aqueous extract which is extracted at a pH of from 3.5 to 5.5 and then dried.