ES2745091T3 - Procedure for obtaining inulin from plants - Google Patents

Abstract

A procedure for obtaining inulin comprising: a) finely grinding the plant material containing inulin, in which particle sizes of the plant material of 500 μm or less are generated, which are smaller than the size of the plant cells containing inulin , b) suspending the finely ground vegetable material in an aqueous liquid with a water content of at least 50 volume percent (volume%), at a temperature in a range of 5 to <60 ° C, where the inulin is released from the plant material and suspended in particulate form in the liquid, c) separating the plant particles from the liquid, in which the inulin which is suspended in particulate form remains in the liquid, d) separating the inulin which is suspended in the form of liquid particles.

Description

DESCRIPTION

Procedure for obtaining inulin from plants

The present invention relates to a process for obtaining inulin from plants.

In recent decades, the demand for foods that contain less fat and more natural raw materials has increased considerably. As a substitute for fats, many substances have already been proposed, such as carbohydrate or protein-based products, or synthetic fat substitutes, such as fatty acid sugar polyesters. However, these always have disadvantages, such as low heat stability, unsatisfactory "mouthfeel" or an unwanted effect on humans or the environment.

It has long been known that inulin is suitable for use in food. Due to the low energy values available to inulin humans, the use of inulin as a fat substitute ensures a large decrease in the calorific value of the final product. Additionally, inulin is used as a prebiotic additive and dietary fiber in food.

Inulin is extracted from plants with warm or hot water in the prior art. Extraction is a separation procedure in which certain components are extracted from solid or liquid mixtures of matter using suitable solvents (extractants) (Rompp Lexikon der Chemie [Rompp Chemistry Lexicon], keyword extraction, tenth edition, Thieme Verlag , 1997).

Inulin extraction from chicory roots is the most commercially important procedure for obtaining inulin. Suitable techniques for isolating inulin from chicory roots include, for example, crushing chicory roots and extracting the inulin with hot water from the crushed material. The most varied procedures for producing inulin from plant sources, including extraction, purification and fractionation, have already been disclosed.

WO 1999037686 A1, DE 4316425, EP-A 627490 and US 2002098272 describe the extraction of inulin from chicory roots with hot water, that is, water heated and maintained at more than 70 ° C, or boiling water.

WO 2007128559 describes a process for obtaining inulin in which artichoke roots are crushed, by treating the roots crushed with hot water an extract is obtained, inulin is precipitated from the extract and inulin is precipitated again at least one time.

US 2,555,356 describes a process for obtaining Jerusalem artichoke inulin in which the Jerusalem artichoke tubers are crushed, a juice containing inulin is extracted from the crushed tubers and the juice is stored for 24 hours or more at approximately 0 ° C to crystallize the inulin that is present in dissolved form in the juice.

The object of the present invention was, among others, to provide an alternative method for obtaining inulin from plants. This object is achieved by the method according to claim 1. The subclaims refer to special embodiments of the process according to the invention.

The present invention relates to a process for obtaining inulin, which comprises:

a) finely grind plant material containing inulin, in which particle sizes of plant material of 500 pm or less are generated that are smaller than the size of plant cells containing inulin,

b) suspend the finely ground plant material in an aqueous liquid with a water content of at least 50 percent by volume (% by volume), at a temperature in a range of 5 to <60 ° C, in which the inulin it is released from plant material and suspended as particles in the liquid,

c) separating the plant particles from the liquid, in which the inulin that is suspended in the form of particles remains in the liquid,

d) separating the inulin that is suspended in the form of particles from the liquid.

The process according to the invention differs from the conventional extraction of the prior art in that the inulin obtained as a product of the process is suspended in the liquid and does not dissolve. The inulin that is obtained as a product in the course of additional steps of the process is isolated in the form of plant particles. In conventional extraction, which is described, for example, in WO 1999037686 A1, DE 4316425, EP-A 627490 and US 2002098272, the inulin contained in the plant is extracted from the plant material quantitatively or virtually quantitatively using a liquid extractor and Inulin is subsequently obtained from the solution. In contrast to US 2,555,356, inulin is not crystallized first by cooling a previously pressed plant juice in which inulin is present in dissolved form, but is already released from finely ground plant material in the form of undissolved particles by adding a liquid.

The term "inulin", in the context of the present invention, is taken as a polyfructane, whose molecules They consist of a beta-2-1 linked chain of fructose molecules.

Preferably, but not necessarily, this chain has an alpha-D-glucose reducing unit at the end of it. Inulin according to the invention is a polydispersed mixture of molecules of different chain length. The plant material used in the process according to the invention can originate from all plants containing inulin, such as, for example, from plants of the Cynara genus, such as artichoke (balloon artichoke, Cynara scolymus, recently also assigned to species Cynara cardunculus L.), thistles (Cynara cardunculus L.) chicory (Cichorium intybus), Jerusalem artichoke (Helianthus tuberosus), dahlia (Dahlia) or dandelion (Taraxacum).

The term "plant material" comprises not only whole plants that contain inulin, but also parts of plants that contain inulin, such as, for example, roots, tubers, stems, flowers, leaves. When the plant material is mentioned later in this document, the plant material containing inulin is understood. In one embodiment of the process according to the invention, the plant material consists of plant roots, preferably artichoke roots (Cynara cardunculus or Cynara scolymus) or chicory (Cichorium intybus). The term "fine crushing" means that, at the end of the crushing process, the plant material reaches particle sizes that are smaller than the size of the inulin-containing plant cell. This achieves cell breakage and accessibility of the inulin that is stored in the plant's cells. A guide value for the desired particle size is a particle size of 500 micrometers or less (<500 micrometers), preferably 400 micrometers or less (<400 micrometers), even more preferably 300 micrometers or less (<300 micrometers), and , most preferably up to 200 micrometers or less (<200 micrometers), in which this value may differ depending on the type of plant material used and should match according to the size of plant cells containing inulin.

For the present procedure it is not necessary that the plant cells containing inulin be broken quantitatively. That is, after fine crushing, larger particles may be perfectly present. However, attempts are made to make the proportion of broken plant cells as large as possible to achieve the highest possible inulin yield.

Advantageously, the plant material, before fine crushing, is free of adherent impurities, for example, by intensive washing with water, in which, in the case of artichoke roots, a high pressure cleaner can also be used. In the case of roots, washing can also be done in the frozen state of the roots to keep the loss of root material mass as low as possible.

The plant material can be crushed in a plurality of stages, from coarse to fine, and by means of all devices that are familiar to those skilled in the art. The roots can be pre-ground first thickly, for example, by cutting.

For more crushing, preference is given to crushers, foragers, mills or granulators, in which a Rotoplex 28/40 or RO20 / 12 granulator (pilot plant scale) from Hosokawa / Alpine is particularly tested. When the artichoke roots (Cynara Cardunculus, Cynara Scolymus) are used as plant material, the product obtained is a crushed root material in the form of generally fibrous pieces.

The final fine crushing can proceed by mashing the plant material. The mash can be made in conventional devices, in which it has been shown that a RA-12 Ultra Turrax or Rietz disintegrator from Hosokawa is particularly advantageous. The puree preferably proceeds with the addition of liquid, such as water, in which the amount of liquid is preferably established such that a free flowing puree is obtained. The weight ratio of liquid to plant material is, for example, in the range of 0.8 / 1-6/1.

If, during the formation of the puree of the plant material, liquid is added, such as water, the fine crushing and the suspension of the finely ground plant material in the liquid is carried out in a single stage. In principle, fine crushing and suspension can proceed successively by not adding the liquid or at least most of the liquid until after the fine crushing.

As already mentioned above, the process according to the invention differs from the conventional extraction of the prior art in that the inulin obtained as a product of the process, in the suspension of the finely ground plant material, is suspended in the liquid and not It dissolves in it. The procedure is not restricted to certain returns. Therefore, in addition, only a relatively small proportion of the inulin released from the plant can be suspended in the liquid and obtained as a product after carrying out the additional steps of the process.

The term "suspend" in the present invention means that a suspension is produced which ultimately comprises finely ground plant material (plant particles), inulin released from the plant material and a liquid. The term "suspension" designates a heterogeneous mixture of matter of a liquid and undissolved solids finely distributed therein, in which the solid in this case comprises finely ground plant material and inulin released from plant material. The finely ground plant material may comprise plant cells that did not break during fine crushing and in which the inulin that is not released is present. Inulin that is released from plant material and suspended is present in the form of particles. According to the invention, part of the inulin can pass into the solution, in particular, short chain inulin. The inulin that is finally obtained as a product of the process, however, is present in undissolved form in steps b), c) and d) of the process as suspended particles. The inulin particles can be crystalline.

The finely crushed plant material (plant particles) is thoroughly mixed with the liquid to release the inulin. The release of inulin from plant particles or from altered plant cells can also be described as elution or washing. For this, in the process step b) liquid is added to the finely ground plant material. For example, a stirrer or a wet mill can be used for mixing. The plant particles are suspended and kept in suspension during this. The inulin that is present in the plant cells is released from the plant cells during the suspension of the plant particles and passes into the liquid in which they are suspended.

To increase the yield of the product, the process can be carried out in such a way that the inulin released from the plant material is predominantly suspended in the liquid and is accessible as a product of the process. The expression "predominantly suspended in the liquid" means that more than 50% by weight of the inulin released from the plant material does not dissolve in the liquid, but is suspended in the form of particles. In advantageous embodiments of the process, an even greater proportion of the inulin released from the plant material does not dissolve in the liquid, but is suspended in it. In this way, the yield of the process product can be further increased. In such advantageous embodiments, at least 60% by weight, preferably at least 70% by weight, even more preferably at least 80% by weight, of the inulin released from the plant material remains in suspension.

For a given chain length profile of the plant inulin, through the choice of temperature and type of liquid, it is possible to control whether the inulin dissolves or suspends in the liquid or to what extent. The solubility of inulin molecules depends firstly on the temperature and the type of liquid and, secondly, decreases with increasing chain length. The chain length of an inulin molecule is identical to its degree of polymerization and indicates from how many units of monosaccharides the inulin molecule is formed. The chain length is also abbreviated hereinafter as "GP" (degree of polymerization).

The liquid used for the suspension is an aqueous liquid. An aqueous liquid is defined herein as a liquid consisting predominantly of water or consisting solely of water. The term predominantly in this sense means a content of at least 50 percent by volume (% by volume).

Said aqueous liquid preferably has a water content of> 60% by volume, more preferably> 70% by volume, even more preferably> 80% by volume and, most preferably,> 90% by volume. The liquid comprising water has in another embodiment a water content of 50 to <100% by volume, more preferably from 60 to <100% by volume, even more preferably from 70 to <100% by volume, even more preferably from 80 at <100% by volume and, most preferably, from 90 to <100% by volume.

A liquid component, which may be present in addition to water, is, in one embodiment, a liquid that is miscible with water. Therefore, the liquid that is used to suspend the finely ground plant material is, in this embodiment, a liquid comprising water and another liquid (or liquid component, respectively) that is miscible with water. Said mixture comprises water in amounts (% by volume) as defined above. A liquid component, which may be present in addition to water, is, in another embodiment, a polar liquid. Therefore, the liquid that is used to suspend the finely ground plant material is, in this embodiment, a liquid comprising water and another polar liquid (or liquid component, respectively). Said mixture comprises water in amounts (% by volume) as defined above.

Liquid mixtures such as, for example, a mixture of water and alcohol are conceivable. As alcohol, ethanol and isopropanol are preferred. The higher the proportion of the alcohol chosen, the lower the solubility of inulin. In a preferred embodiment, the liquid used for the suspension is water, which means water without any other liquid added.

In an advantageous embodiment of the process, the inulin suspended in the liquid consists essentially of, that is, at least 95% by weight, of inulin molecules having a chain length greater than 10. For this, the liquid and the temperature of The suspension is selected in such a way that at least fructooligosaccharides (oligofructans) having a GP in the range of 3 to 10 and also mono and disaccharides pass into the solution during suspension of finely ground plant roots. If water is selected as a liquid, then this objective can be achieved even at a temperature of approximately 20-30 ° C, preferably at 20-25 ° C.

When the temperature of the suspension increases, long-chain inulin molecules also dissolve more and more. Long chain inulin molecules are preferably defined as inulin molecules with a GP> 10. By selecting the temperature of the suspension, it is therefore possible to determine what proportion of the long-chain inulin molecules dissolves in the liquid or does not dissolve in the liquid, but remains in suspension . The size of this proportion also depends on the properties of the liquid. For example, in the case of an alcohol / water mixture, the solubility of inulin may be lower than in the case of pure water at the same temperature. In addition, it should be noted that the solubility of inulin decreases with increasing chain length. Therefore, when the temperature rises, the molecular weight of the undissolved inulin shifts to higher values.

In a special embodiment of the invention, the plant material used is the artichoke roots (Cynara Cardunculus L., Cynara Scolymus, artichoke). In this embodiment, it is possible to obtain an inulin having a particularly high average degree of GPp polymerization between 40 and 80, more preferably between 50 and 80. In this regard and in relation to the present invention, the term "between" is also intended to include the numerical limits indicated respectively. Very particularly preferred, an inulin according to the present invention can be obtained from artichoke roots having the following characteristics: a GPp of 50-80 and a GPn of 41 66. The value of GPp (average degree of polymerization by weight) and GPn (average number of degree of polymerization) is determined using GPC-RI-MAL ¹ S. An exact description of this procedure is disclosed in WO 2006/108697. The molecular weight of a monomer used in conversions is 162 g / mol.

In a special embodiment of the process according to the invention, the suspension has a temperature below 60 ° C, preferably up to 50 ° C, more preferably up to 40 ° C, even more preferably up to 30 ° C. In this case, the type of liquid is not restricted. Preferably, water is used. Other advantageous temperature ranges are 5 to <60 ° C, 5 to 50 ° C, 5 to 40 ° C, 5 to 30 ° C, 5 to 25 ° C, 10 to <60 ° C, 10 to 50 ° C, 10 to 40 ° C, 10 to 30 ° C, 10 to 25 ° C, 15 to <60 ° C, 15 to 50 ° C, 15 to 40 ° C, from 15 to 30 ° C, from 15 to 25 ° C, from 20 to <60 ° C, from 20 to 50 ° C, from 20 to 40 ° C and from 20 to 30 ° C.

In a particularly advantageous embodiment of the process, the suspension has a temperature of 20-25 ° C, in which all the liquids mentioned above can be used. In this embodiment, a suspending liquid is used that has room temperature in the range of 18-25 ° C, preferably at 20-25 ° C. Preferably, in this embodiment, the liquid and the plant material, before mixing, each has a temperature at these intervals. In this embodiment, a separate heat or cooling supply can be dispensed with. The advantage of these embodiments is that during the suspension of the roots of finely ground plants in the liquid, it is not necessary to supply external heat energy or cooling energy, which makes the process particularly energy efficient. The mechanical energy introduced through the suspension mixture is not considered in this case.

At a later stage of the procedure, called step c) earlier herein, the plant particles are separated from the liquid, with the suspended inulin remaining in the liquid. The term "plant particles" means the product obtained after the fine crushing of the plant material, that is, therefore, finely ground plant material. At this stage of the procedure, the suspended inulin that is released from the plant material in the previous stage of the procedure does not need to remain quantitatively in the liquid. Depending on the separation device and the process conditions, part of the suspended inulin can be separated along with the plant particles. The type of plant particles depends on the plant material used. In the case of plant roots, they consist mainly of fibers and woody particles.

The plant particles can be separated by centrifugation, decanting or using a mechanical separation device, for example a sieve or a jet extractor. In the case of a sieve or a comparable separation device that separates according to the particle size, the separation limit of the separation device is preferably selected such that the smallest possible amount of inulin particles suspended in the particle is separated. liquid, but that the plant particles separate as quantitatively as possible. The particle size of the suspended inulin may be <100 micrometers or <50 micrometers, preferably <40 micrometers, more preferably <30 micrometers, even more preferably <25 micrometers, especially preferably <20 micrometers and, most preferably, <10 micrometers In the case of inulin from artichoke roots, the particle size of the suspended inulin can be up to about 10 micrometers.

In a special embodiment of the process according to the invention, step c) is carried out at a temperature below 60 ° C, preferably up to 50 ° C, more preferably up to 40 ° C, even more preferably up to 30 ° C. Other advantageous temperature ranges are 5 to <60 ° C, 5 to 50 ° C, 5 to 40 ° C, 5 to 30 ° C, 5 to 25 ° C, 10 to <60 ° C, 10 to 50 ° C, 10 to 40 ° C, 10 to 30 ° C, 10 to 25 ° C, 15 to <60 ° C, 15 to 50 ° C, 15 to 40 ° C, from 15 to 30 ° C, from 15 to 25 ° C, from 20 to <60 ° C, from 20 to 50 ° C, from 20 to 40 ° C and from 20 to 30 ° C. It is understood in this case that in step c), the suspension has a temperature in the ranges mentioned above.

Step c), in an advantageous variant of the present invention, is carried out at the same temperature as step b) of the process.

In a further embodiment, step c) is carried out at a temperature in the range of 18-25 ° C, preferably 20-25 ° C and without external heat supply. This is understood that in step c), the suspension has a temperature in said intervals.

To increase the yield of the process, the plant particles, after they are separated from the liquid, can be re-crushed and repeated the steps of the procedure a) -c).

After stage c) and before stage d) an intermediate stage can be included, in which inulin precipitated, if any, is suspended in the liquid again.

In the last stage d), the suspended inulin is separated from the liquid, to obtain the product of the process, in which the separation does not have to be quantitative. The separation can be carried out, for example, by means of a centrifuge or hydrocyclones. In addition, devices such as sieves and filters, and also all other separation devices known to those skilled in the art can be used to separate particles in the micrometer range of liquids.

In an advantageous embodiment, step d) is carried out at the same temperature as steps b) and c). The corresponding temperature ranges are mentioned later in the description of steps b) and c). This can prevent, at this stage, low molecular weight saccharides and low molecular weight inulin fractions that were previously dissolved, precipitated again from the solution and fed to the product. Lowering the temperature in stage d) could lead to such a result. This is not desired, in particular, when the product to be obtained is an inulin having a high average molar mass. This embodiment is important, in particular, when the steps of procedure b) and c) are carried out at temperatures above 18-25 ° C or 20-25 ° C. In a further advantageous embodiment, step d) is also carried out at 18-25 ° C, preferably at 20-25 ° C. The inulin obtained can be dried by all methods known to those skilled in the art, such as, for example, air drying, spray drying, vacuum drying and lyophilization, and also roller drying.

In such procedures, additional steps may be present in addition to the steps described a) - d). Those that can be mentioned are, for example, the described cleaning of the plant material before carrying out stage a), or additional purification and / or drying stages that follow stage d), or additional stages between stages a ) -d).

In one embodiment of the process, steps a) and b) described above directly follow each other without any intermediate stage. In a further embodiment of the process, steps b) and c) described above immediately follow each other, without any intermediate steps. In still a further embodiment of the process, steps c) and d) described above are followed immediately without any intermediate steps. These embodiments can be combined in any combination. In a special embodiment, in the case of the steps of the procedure a), b), c) and d), no intermediate stage type is provided, whereby all the stages described a), b), c) and d) They follow each other directly. In this embodiment, however, additional steps may be provided upstream of stage a) and downstream of stage d). Those that can be mentioned are, for example, the described cleaning of the plant material before carrying out stage a), or more purification and / or drying stages that follow stage d).

In one embodiment of the process, the inulin that is separated in step d), hereinafter also referred to as the product of the process, can be purified in one or more additional steps, if a purification appears to be necessary. After the product of the process separates from the liquid, impurities may still be present, such as, for example, very fine plant particles, sludge and coloring substances. The product of the process can be purified, for example, by recrystallization, (ultra) filtration, dissolution and precipitation with a solvent, for example, with ethanol or isopropanol, or chromatography.

In the case of a filtration, the product of the process can be completely dissolved in a solvent with heat supply and, subsequently, the solution can be filtered, to separate very fine solid particles. In addition, a purification can also proceed, treating a solution of the process product with activated carbon. Using the techniques mentioned above it is possible, in addition to a purification, to also fractionate the process product to achieve a longer average chain length of the product, as described in patent application EP-A-0627490.

The purified inulin can be dried using all the procedures known to those skilled in the art, such as, for example, air drying, spray drying, vacuum drying and lyophilization, and also roller drying.

Figures:

Figure 1 shows a flow chart of a special embodiment of the process in which artichoke roots are used as inulin-containing plant material.

The artichoke roots (from Cynara Cardunculus / Cynara Scolymus) 101 are first crushed 102 , in which the coarse crushing is performed here. For crushing 102 , for example a Hosokawa / Alpine 28/40 granulator, an Urschel laminator or similar device can be used. Water is then added to the root pieces 103 . The water / root mass ratio can be set, for example, in 1/1 -6/1.

The mixture of crushed artichoke roots and water is mashed 104 . For the formation of mash 104 , a Rietz RA-12 or RP6 (pilot plant scale) disintegrator from Hosokawa or one from Stephan Industrieturrax, for example, can be used, for example. A suspension containing inulin and very fine root particles 105 is obtained which are subsequently mixed intensively 106 , for example, by stirring, to release as much inulin as possible from the root cells. In this case, part of the inulin, in particular the shorter chain fractions, can be dissolved in the water. To what extent this occurs depends on the temperature of the water and the temperature at which steps 104 and 106 of the process are carried out.

In the next stage, the fine root particles are separated 107 . This can be achieved, for example, by allowing the suspension to rest, allowing the fine root particles to settle and subsequently decant. In the decantation process, the inulin particles form a dense precipitate on which the fine root particles form a phase that can be decanted. Alternatively, the suspension can also be centrifuged under suitable conditions or screened through a suitable sieving device, to separate the particles from the root. The conditions are selected in such a way that in step 107 , the inulin for the most part remains undissolved in the aqueous phase or as a precipitate and does not separate together. As an intermediate, an inulin suspension 108 is obtained. If the root particles are separated by decantation or centrifugation, the precipitated inulin can be suspended again in the aqueous phase to obtain an inulin suspension. If root particles are separated by sieving, this is not necessary.

Finally, undissolved inulin separates 109 from the suspension. This is achieved, for example, by using a centrifuge that has a sufficiently high gravitational field that allows the fine particles of inulin to be separated. As a byproduct, water 110 is obtained which may contain a proportion of low molecular weight inulin in dissolved form and also other soluble components of the artichoke root. The product of the process is obtained as an inulin pellet 111 .

Inulin pellet 111 can be dried and / or subjected to additional purification steps if it appears to be necessary. Examples:

Example 1: Making an inulin isolation of artichoke roots (Cynara Scolymus) at room temperature

1.1 Crushing / granulating machine

Frozen artichoke roots (Cynara scolymus / Cynara cardunculus L.) were processed. The roots were allowed to stand overnight at room temperature and processed the next day. Straight roots with the least possible number of lateral shoots were used. The thin stems of the root were removed with a kitchen knife. 720 g of artichoke roots were used. These were processed in 2 mm thick sheets using a sausage slicer. The initial pieces were subjected to crushing and stuck in the cutting channel. The machine occasionally turned off and the cutting channel was cleaned. The final pieces were not cut into pieces less than 3 cm. The yield of the cut sheets was 522 g. The difference of 198 g corresponded to the soil, foreign matter and final pieces of artichoke root.

1.2 Manual selection / peeling / rolling

The cut artichoke slices were selected by hand. During this it was observed that the bone marrow could be separated very easily from the skin by pressing. The peeling time was 16 min. The yield of the artichoke core material was 336 g and the yield of the artichoke skin or foreign matter was 181 g. Artichoke sheets were processed successively using a domestic Genius machine to laminate the artichoke to a size of 4 mm x 4 mm. Production time 11 min.

1.3 Crushed using the Waring and Ultra Turrax blender

The 336 g of artichoke sheets were loaded with 336 g of water in the Waring blender (400 watt apparatus without speed display) and then pre-crushed.

By means of the size of the sheets, the pre-grinding proved to be free of problems and, optionally, can be omitted. The crushed artichoke sheet dough was decanted into a 5 liter glass beaker and 500 ml of water was poured. This mass was crushed using the Ultra Turrax (1 min in stage 3, corresponding to 6,400 rpm). The time was deliberately selected to be short, since the particle size should not be too small. In the subsequent sieving through 90 µm and 63 µm, it was observed that the fibrous solid appeared to be swollen and the particle size was large. The liquid obtained was designated number 1 and reserved. An aliquot of the screened solids was then removed (64 g of solids, which had been frozen and lyophilized). The remaining solids were mixed with 1.4 liters of water and crushed using Ultra Turrax in step 2 (5,200 rpm) for 5 minutes. Then, the mixture was decanted again through the sieve mentioned above. The liquid obtained was designated number 2. Then an aliquot of the screened solids (30 g of frozen and lyophilized solids) was removed. The remaining residue was mixed with 2 liters of water and triturated for 2 minutes at maximum (10,000 rpm) using Ultra Turrax. The liquid obtained was designated number 3.

The skin with foreign matter was processed at a later time. 181 g of artichoke skin with foreign matter was crushed with 470 g of water in the Waring blender for 5 minutes, then decanted in a glass cup and mixed with 1.6 liters of water. Then Ultra Turrax was used at 10,000 rpm for 5 minutes. The crushing product was, as already described, sieved, and the liquid obtained was designated 4. The solids were frozen and lyophilized.

1.4 Centrifugation

Each centrifugation was performed at 4000 rpm for 10 minutes. The obtained 1-4 liquids were processed successively without mixing according to the following procedure: the liquid obtained, after sieving, was transferred to a 750 ml container and centrifuged. After decanting, the precipitates were combined and diluted with maximum water to achieve purification. The mixture was then transferred to 50 ml Falcon tubes and then the slime layers were separated.

For additional analytical purposes, all liquids obtained for each work stage were collected and concentrated using a rotary evaporator. The remaining liquids were deeply frozen and dried using the lyophilization unit.

Example 2: Production of inulin suspensions to determine the solubility of inulin at different temperatures

The starting material used was inulin from artichoke root which was obtained according to Example 1.

In each case, approximately 20 mg of inulin was suspended in water at various temperatures (20; 30; 40; 50; 60 ° C). Lot: A 1% solution (water at room temperature (RT)) was suspended for 20 minutes at 300 rpm at various temperatures in Eppendorf tubes (repeated inversion).

Subsequently, the suspensions were centrifuged for 5 minutes at 13,000 rpm to separate undissolved inulin. The supernatant containing dissolved inulin was removed and transferred to another Eppendorf tube. The sediment and its supernatant were lyophilized (48 h).

Analysis: the inulin obtained from the sediment and the supernatant was analyzed by gel permeation chromatography (GPC-RI). The empty weights of all Eppendorf tubes used were recorded. For the preparation of the GPC-RI analysis, based on the determined masses of lyophilized residues, a 1% solution was produced. The batches were dissolved for 20 minutes at 95 ° C and 300 rpm (repeated inversion). After the dissolution operation, the 1% solutions were diluted to 1:10 with DMSO and centrifuged with 0.22 jm filter inserts for 5 minutes at 8,000 rpm.

To determine the inulin masses in the supernatant and sediment, a calibration curve was prepared using the Raftiline HP® standards and an artichoke inulin having a GPp = 69. With the help of the calibration curve, the peaks in The GPC diagram could be assigned to an absolute mass.

Table 1: Results:

continuation

The experiment does not represent the complete procedure according to the invention. It is a model experiment to obtain approximate evidence of the product yield of the process according to the invention and the chain length profile of the product of the process. For this artichoke, inulin (Cynara scolymus) was suspended at various temperatures. The product of the process is suspended inulin undissolved, in this document the inulin in the sediment.

From the table it can be seen that, with an increase in temperature, more inulin in percentage passes to the solution and less inulin remains suspended. At 95 ° C, virtually all inulin dissolves. Therefore, the performance of the process according to the invention decreases with an increase in temperature.

Additionally, it can be seen that the average molar masses of the inulin in the sediment and of the dissolved inulin increase with increasing temperature. First, with increasing temperature, more and more relatively long chain inulin passes into the solution, so the average molar mass of dissolved inulin increases. Secondly, at elevated temperatures, only the very high molecular weight inulin fractions remain undissolved, so the average molar mass of the undissolved inulin also increases. If it is desired to obtain, as a product of the process, a product having a molar mass as high as possible, then an elevated temperature will be used. At a temperature of 60 ° C, in the model experiment, a GPp of the product of 67-68 is achieved and at a temperature of 20 ° C, a GPp of 56-57 is achieved. However, at the same time, in the model experiment, the yield decreases from about 68% (20 ° C) to about 12-13% (60 ° C).

The model experiment shows that in the process according to the invention, at a temperature of 20 ° C, that is, without further heat supply, a relatively long chain inulin (GPp 56-57) of artichoke roots is expected with a relatively high yield (68%).

Example 3

3.1 Materials

Artichokes (Cynara Scolymus) of the Gobbo di Nizza variety, quantity 50 kg, dried in the sun, stored loose were used.

3.2 Preparation of the material:

The roots were unpacked and placed loose in the greenhouse.

20 kg of roots were cleaned using a high pressure cleaner and placed again to dry.

Start of the experiment:

- cut into pieces (approximately 4)

- grated in Agrobloc with the thickest insert

- the grated material is vacuum packed in plastic and stored refrigerated overnight.

15 kg of grated material was processed using Industrieturrax (1.4 mm hole width) and loaded into a large container (50 l).

Masses: 15 kg of grated material, 30 kg of water resulted in 45 kg of material crushed with Turrax, later called finely crushed material.

3.3 Small experiment 1

Finely crushed material: 502 g

Water: 1000 ml

- remove, sift, press, discard the cake from the press

1,112 g liquid centrifuge at 4,000 rpm, 10 min

The supernatant was passed through a 20 pm sieve: no fibers were visible in the sieve.

36 g sediment, 502 g of finely crushed material ~ 10%. Approximately 5 g ~ 1% inulin was expected.

The sediment was collected with 193 ml of water and another 124 g of water was added thereto.

The total mass, 353 g, was passed through a 20 pm sieve that was quickly plugged. Approximately 10 ml passed. In the microscope at 10 x 100 times, crystals were seen (filtrate 1).

The remaining 340 g were placed in a centrifuge at 4,000 rpm, which produced 27 g of sediment. 10 g of them were transferred to a Falcon tube.

10 g of sediment was dissolved in the microwave at more than 88 ° C. The fibers could be seen clearly.

The total residual sediment of 17 g was heated to> 88 ° C and again passed through a 20 pm sieve that was immediately plugged. Minimum filtering 2.

Filtering 2 (hot, 1-3)

Filtering 3 (residue in the sieve, liquid phase)

Sieve residue 4 (residue in the sieve, solid phase)

3.4 Large experiment 1

Finely crushed material 10 kg

Water 32 l

- remove, sift, 125 pm, manual press

- produced 33.5 l of liquid, 8.022 kg of press cake

- centrifuge, 12,000 g, 7,000 rpm, 10 min, in plurality of lots

- the sediments were combined, the water content was determined through Karl Fischer. Karl Fischer value: 75.75% water content

Samples:

1 Finely crushed, untreated material, diluted 1: 2, crushed in the Turrax

2 Residue in sieve, press cake after sifting

3 Supernatant after the first centrifugation

4 Sediment 1

5 Sediment 2, supernatant

6 Sediment 2, lower layer

Two phases of sediment 2 were obtained.

Samples 1-6 for analysis

Samples 4-6 for the determination of dry matter

Samples 4-6 for examination by optical microscopy

Masses:

Total sediment after the first centrifugation (sample 4) 806 g

Supernatant after the first centrifugation (sample 3) 331

3.5 Supplementary experiment 1

Sediment sample 1,600 g

Water 1,200 g

- centrifuge, 12,000 g, 7,000 rpm, 10 min

Two phases are clearly recognizable and two samples were taken.

Sample 5 supernatant, sludge

Sample 6 bottom layer, very solid

Masses:

Sediment 2, supernatant, 306 g

Sediment 2, lower layer 287 g

3.6 Complementary experiment 2

Sediment 2, supernatant, sample 5

Sediment 2, bottom layer, sample 6

Observation:

In sample 6, a precipitate was immediately deposited, in sample 5 a slight precipitate with the addition of ethanol.

10 ml of alcohol and 5 ml of the sample were centrifuged.

This produced 500 g of sieve residue 2 which was washed with water.

Samples:

7 press cake, washed

8 liquid press cake

3.7 Analysis of the sample material

The starting materials were lyophilized samples.

Sample preparation and isolation were carried out on the scale of an Eppendorff tube.

The starting material of this inulin isolation was an artichoke root puree (<1.4 mm). PR 1-PR 8 samples were taken during the preparation procedure and frozen at -80 ° C for preparation for lyophilization. After lyophilization, the sample material was ground and prepared for analysis as indicated below. The PR 1, PR 2 and PR 7 samples were homogenized in the Retsch GM 200 knife mill (2 x 10 seconds, at 10,000 rpm).

Samples PR 1, PR 2 and PR 7 were treated as detailed.

- weigh 100 mg of the powder in a 2 ml Eppendorff tube

- mix carefully with 1 ml of water and gently invert

- incubate 1 h at 95 ° C and 300 rpm

- then centrifuge the Eppendorff tube (5 min, 13,000 rpm)

- remove the supernatant and transfer to a new Eppendorff tube, also store at 95 ° C

- again mix the sediment with 1 ml of water

- try again for 1 h at 95 ° C and 300 rpm

- centrifuge the liquid again (5 min, 13,000 rpm)

- pipette supernatant 2 to supernatant 1

PR 3-PR 6 and PR 8 samples were dissolved in 2 ml of DMSO for 20 min at 300 rpm and at 95 ° C in the heating block with stirring. Samples were diluted for GPC-RI analysis to 1: 2 or 1: 4 with DMSO. Weights and dilutions can be seen in the Fructane table of contents.

Table 2: Analytical data, calculated on the basis of the GPC-RI analyzes

continuation

Table 3: Calculation of mass remains

Claims (8)

1. Procedure for obtaining inulin comprising: a) finely grind the inulin-containing plant material, in which particle sizes of the plant material of 500 µm or less are generated, which are smaller than the size of the plant cells containing inulin, b) suspend the finely ground plant material in an aqueous liquid with a water content of at least 50 percent by volume (% by volume), at a temperature in a range of 5 to <60 ° C, in which the inulin it is released from plant material and suspended as particles in the liquid, c) separating the plant particles from the liquid, in which the inulin that is suspended in the form of particles remains in the liquid, d) separating the inulin that is suspended in the form of particles from the liquid. 2. The method according to claim 1, wherein the inulin which is separated from the liquid is purified. 3. Method according to claim 1, wherein step c) is carried out at a temperature of 5 to <60 ° C. 4. Method according to any one of the preceding claims, wherein the plant material used is plant roots. 5. Method according to claim 4, wherein the roots of the plants are artichoke roots (Cynara scolymus or Cynara cardunculus L.) or chicory roots (Cichorium intybus). 6. Method according to claim 5, wherein the roots of the plants are artichoke roots and the product of the process is an inulin having an average degree of GPp polymerization, determined by GPC-RI-MALLS, from 40 to 80. 7. Method according to any one of the preceding claims, wherein the solid particles are separated from the liquid by means of a decanter or sieve. 8. Method according to any one of the preceding claims, wherein the undissolved inulin molecules are separated from the liquid using a centrifuge.