EP2704595A1 - Procédé de production d'isomaltulose à partir de sèves - Google Patents

Procédé de production d'isomaltulose à partir de sèves

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Publication number
EP2704595A1
EP2704595A1 EP12717789.7A EP12717789A EP2704595A1 EP 2704595 A1 EP2704595 A1 EP 2704595A1 EP 12717789 A EP12717789 A EP 12717789A EP 2704595 A1 EP2704595 A1 EP 2704595A1
Authority
EP
European Patent Office
Prior art keywords
strain
klebsiella
isomaltulose
seq
sucrose
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP12717789.7A
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German (de)
English (en)
Inventor
Axel Hengstermann
Stefan MÜNZNER
Jürgen HABERLAND
Manuel HOLTKAMP
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Evonik Industries AG
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Evonik Industries AG
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Publication date
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Publication of EP2704595A1 publication Critical patent/EP2704595A1/fr
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    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00—Preparation of compounds containing saccharide radicals
    • C12P19/24—Preparation of compounds containing saccharide radicals produced by the action of an isomerase, e.g. fructose
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/30—Artificial sweetening agents
    • A23L27/33—Artificial sweetening agents containing sugars or derivatives
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/30—Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/105—Plant extracts, their artificial duplicates or their derivatives
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00—Preparation of compounds containing saccharide radicals
    • C12P19/12—Disaccharides
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs

Definitions

  • the invention relates to a process for the isomerization of a sucrose-containing vegetable juice to isomaltulose.
  • DE1049800 describes a process for the fermentative production of isomaltulose from sucrose-containing plant juices by means of the bacterial strain Protaminobacter rubrum. Alternatively, enzymatic conversion to dead organisms may also take place. The cell mass is separated in batches by centrifugation at the end of the reaction and the product is worked up further. This method can be found in the literature in H. Schiweck, alimenta 19, 5-16, 1980 again.
  • EP0001099 describes a process for the continuous fermentation of the bacterial strains Protaminobacter rubrum (CBS574.77) and Serratia plymuthica (ATCC 15928) with simultaneous isomerization of the sucrose to isomaltulose with, inter alia, thick or thin juice as substrate, the substrate solution itself being a nutrient medium for the growth of the cells , The cells are separated from the product solution by centrifugation after the reaction. A separate from the actual isomerization cultivation of biocatalytically active organisms in a different medium than the substrate medium is expressly found to be disadvantageous.
  • DE3241788 describes a process for the preparation of 1-OaD-glucopyranosido-D-fructose from aqueous sucrose solutions with free cells of the bacterial strains from the group Protaminobacter rubrum (CBD574.77), Serratia plymuthica (ATCC 15928), Serratia marescens (NCIB 8285), Leuconostoc mesenteroides (NRRL-B-512F) and Erwinia rhapontici (NCPPB 1578).
  • Dick syrup may be used in the described method, and this also serves as the carbon source for the growth process of the cells. In the case of immobilized cells, use is made of pure sucrose solution.
  • EP0983374 describes a process for the simultaneous production of isomaltulose and betaine with immobilized bacterial strains from the group Protaminobacter rubrum (CBD574.77), Serratia plymuthica (ATCC 15928) and Erwinia rhapontici (NCPPB 1578).
  • the manufacturing process is based on molasses, a composition obtained at the end of the sugar manufacturing process.
  • the use of thick juice as a substrate is not possible in this process and requires an explicit depletion of the sucrose by, for example, crystallization.
  • WO97 / 44478 describes a process for the preparation of isomaltulose with living, immobilized bacterial strains from the group Protaminobacter rubrum (CBD574.77), Serratia plymuthica (ATCC 15928) and Erwinia rhapontici (ATCC 29284).
  • the manufacturing process is based on molasses or pure sucrose solution.
  • EP0028900 describes a process for the preparation of immobilized cell isomaltulose of the bacterial strain Erwinia rhapontici (NCPPB 1578). The preparation is based on a pure sucrose solution with a maximum admixture of 15% v / v molasses.
  • EP0625578 uses bacterial strains from the group of Protaminobacter rubrum (CBS 574.77), Serratia plymuthica (ATCC 15928), Serratia marcescens (NCIB 8285), Leuconostoc mesenteroides (NRRL-B 512 F (ATCC 1083 a)) and Erwinia rhapontici (NCPPB 1578).
  • CBS 574.77 Protaminobacter rubrum
  • Serratia plymuthica ATCC 15928
  • Serratia marcescens NCIB 8285
  • NRI-B 512 F ATCC 1083 a
  • Erwinia rhapontici NCPPB 1578
  • EP0392556 and EP1257638 describe the use of bacterial strains from the group of Klebsiella terrigena JCM 1687, Klebsiella sp. No. 88 (FERM BP-2838) and Klebsiella singaporensis LX3 and LX21.
  • Immobilized cell isomerization processes are described in DE3133123 and EP0915986 and are used in the context of the immobilization processes of the enzyme catalysts of the calcium alginate or of the ion exchangers.
  • the object of the present invention was therefore to provide a process which makes it possible to recover purified isomaltulose from a readily available sucrose source.
  • sucrose-containing plant juices for the production of isomaltulose using immobilized enzyme complexes is able to accomplish this task.
  • the present invention therefore provides a process for the preparation of isomaltulose comprising the process steps
  • sucrose-containing solution at least one selected from thick juice or thin juice, preferably syrup, is used.
  • the invention advantageously provides for the use of sucrose-containing plant juices as substrate for the isomerization.
  • the present invention is achieved by the present invention Substrate mixtures, the same yield and even a higher selectivity in the isomerization as achieved with high purity sucrose.
  • An advantage of the present invention is that the increased lifetime of the immobilized cells in combination with a crude plant juice as a substrate results in a substantially higher resource efficiency since the purification step to high purity sucrose is saved.
  • Another advantage of the present invention is that the direct use of thick juice saves energy and resources.
  • Another advantage of the present invention is that the use of the thick juice no buffer solutions or other additives to stabilize the enzymatic activity are necessary, but a natural stabilization of the enzymes used takes place.
  • Another advantage of the present invention is that the use of the thick juice during isomerization, the content of the cariogenic monosaccharides fructose and
  • Glucose can be reduced compared to the use of purified sucrose solution.
  • enzyme complex an at least one active enzyme-comprising composition or mixture composition which may also be complex in nature, such as a living cell
  • enzyme complex are fusion proteins in which the at least one active enzyme has at least one other Polypeptide is linked, but also a purified enzyme itself may be an enzyme complex in the context of the present invention.
  • immobilized enzyme complex is to be understood as meaning an enzyme complex which is bound to a matrix or enclosed by a matrix, so that the enzyme complex is restricted in its free diffusion or in its free movement in an aqueous solution, slowed down, for example.
  • the term "thin juice” is to be understood as meaning the product which is present in the sugar production from sugar beet or sugar cane after juice purification. "Thin juice typically contains 10-20% by weight of sucrose, based on the total juice.
  • the term “thick juice” is to be understood in the context of the present invention, the thickened “thin juice” containing more than 20 wt .-% sucrose based on the total juice.
  • sucrose-containing solution advantageous thick juice
  • this may optionally be diluted with water to a volume ratio of 1: 5, based on thick juice to water, whereby a more controllable isomerization is obtained.
  • the dilution of the thick juice with water is chosen so that at the beginning of process step A) in the thick juice a sucrose concentration of 20-80 wt .-%, in particular from 30-50 wt .-% based on the total juice is present.
  • thin or thick juice of sugar beet is to be used advantageously, with thick juice of sugar beets being particularly preferred.
  • the enzyme contained in the enzyme complex is preferably at least one sucrose glucosylmutase of the enzyme class EC 5.4.99.1 1.
  • sucrose glucosyl mutases from Protaminobacter rubrum, in particular the strain Protaminobacter rubrum CBS 574.77 and those with Seq ID Nos.
  • Protaminobacter ruber Z12 Serratia plymuthica, in particular the strain Serratia plymuthica ATCC 15928; Serratia odorifera, in particular the strain Serratia odorifera 4Rx13 (SEQ ID NO: 7); Serratia marcescens, in particular the strain Serratia marcescens NCIB 8285; Leuconostoc mesenteroides, in particular the strain Leuconostoc mesenteroides ATCC 1083 a; Erwinia rhapontici, especially the strain Erwinia rhapontici ATCC29283 (SEQ ID NO: 1), NCPPB 1578, DSM 4484 (SEQ ID NO: 8), NX-5 (SEQ ID NO: 9) and WAC2928 (SEQ ID NO: 10); Erwinia sp., In particular the strain Erwinia sp.
  • Agrobacterium radiobacter in particular the strain Agrobacterium radiobacter MX-232
  • Klebsiella terrigena in particular the strain Klebsiella terrigena JCM 1687
  • Klebsiella sp. in particular the strains Klebsiella sp.
  • Klebsiella pneumoniae in particular strain Klebsiella pneumoniae 342 (SEQ ID NO: 4); Klebsiella singaporensis, in particular the strain Klebsiella singaporensis LX21; Pseudomonas mesoacidophila, in particular the strain Pseudomonas mesoacidophila MX-45 (SEQ ID NO: 2); Pantoea dispersa, in particular the strain Pantoea dispersa UQ68J (SEQ ID NO: 3); Klebsiella planticola, in particular the strains Klebsiella planticola CCRC 191 12, MX10 and UQ14S (SEQ ID NO 13); Enterobacter sp., In particular the strain Enterobacter sp.
  • FMB-1 (Seq ID NO. 16), SZ62 and Ejp617 (Seq ID NO 14); Azotobacter vinelandii DJ (SEQ ID NO: 15) is used in the method according to the invention, with Protaminobacter rubrum CBS 574.77 and Protaminobacter ruber Z12 being particularly preferred.
  • the enzymes can be used in purified form as polypeptides. For ease of purification, these may be present as fusion proteins, with, for example, a tag which facilitates ready purification, such as a His-iag, a Strep-tag, a GST-iag or an MBP-iag, fused to the enzyme.
  • the enzyme complex is whole cells, which are preferably selected from the group Protaminobacter rubrum, in particular the strain Protaminobacter rubrum CBS 574.77; Protaminobacter ruber Z12; Serratia plymuthica, in particular the strain Serratia plymuthica ATCC 15928; Serratia odorifera, in particular the strain Serratia odorifera 4Rx13; Serratia marcescens, in particular the strain Serratia marcescens NCIB 8285; Leuconostoc mesenteroides, in particular the strain Leuconostoc mesenteroides ATCC 1083 a; Erwinia rhapontici, especially the strain Erwinia rhapontici ATCC29283, NCPPB 1578, DSM 4484, NX-5 and WAC2928; Erwinia sp., In particular the strain Erwinia sp.
  • Agrobacterium radiobacter in particular the strain Agrobacterium radiobacter MX-232
  • Klebsiella terrigena in particular the strain Klebsiella terrigena JCM 1687
  • Klebsiella sp. in particular the strains Klebsiella sp.
  • Klebsiella pneumoniae in particular the strain Klebsiella pneumoniae 342; Klebsiella singaporensis, in particular the strain Klebsiella singaporensis LX21; Pseudomonas mesoacidophila, especially the strain Pseudomonas mesoacidophila MX-45; Pantoea dispersa, in particular the strain Pantoea dispersa UQ68J; Klebsiella planticola, in particular the strains Klebsiella planticola CCRC 191 12, MX10 and UQ14S; Enterobacter sp., In particular the strain Enterobacter sp.
  • the immobilization of the enzyme complexes can be carried out, for example, in the form of CLEAs (insoluble crosslinked enzyme aggregates) (Cao, L. et al., 2000, Cross-linked enzyme aggregates: a simple and effective method for the immobilization of penicillin acylase, Org. Lett, 2 : 1361-1264) or on solid support materials of natural or synthetic origin.
  • CLEAs insoluble crosslinked enzyme aggregates
  • Natural materials are, for example, polysaccharides such as alginate, agarose, sepharose, cellulose and its derivatives (eg DEAE or CM cellulose). Modified sepharoses, such as epoxy-activated, cyanogen bromide activated, NHS activated, thiol activated sepharose, may also be employed. These sepharoses are commercially available, for example, from GE Healthcare, BioRad, Sigma and Pierce.
  • polystyrene derivatives polyacrylates, in particular epoxide-activated acrylic resin beads (Eupergit), polymethacrylates, polyacrylamides, vinyl and allyl polymers, polyesters or polyamides.
  • inorganic supports materials based on silicon or aluminum oxides or mixtures thereof are possible.
  • Immobilization of the enzyme complexes can also be achieved by encapsulation in polymeric porous gels, for example hydrophobic sol-gel materials of RSi (OCH 3 ) 3 or mixtures of RSi (OCH 3 ) 3 and Si (OCH 3 ) 4 (Reetz, MT; Zonta, A Simpelkamp, J .; Rufinska, A .; Tesche, BJ Sol-Gel, Technol 1996, 7, pp. 35-43) or from porous polymeric silica gels (Elgren, TM; Zadvorny, OA; Brecht E, Douglas, T., Zorin, NA, Maroney, MJ & Peters, JW).
  • polymeric porous gels for example hydrophobic sol-gel materials of RSi (OCH 3 ) 3 or mixtures of RSi (OCH 3 ) 3 and Si (OCH 3 ) 4 (Reetz, MT; Zonta, A Simpelkamp, J .; Rufinska, A
  • the enzyme complexes used in the process according to the invention are preferably immobilized in polysaccharides such as alginate, pectin, carrageenan, chitosan or polyvinyl alcohols, such as lenticates, or mixtures thereof, in particular in alginate; See, for example, Shimizu, H., et al. (1997) Screening of novel microbial enzymes for the production of biologically and chemically useful compounds, in: Advances in biochemical engineering biotechnology, Vol58: New Enzymes. For Organic Synthesis (Scheper, T., ed.) Pp. 45-88, Springer, New York.
  • a particularly preferred immobilization for any form of the enzyme complexes used in the method according to the invention is the method described in EP201 1865, in which the enzyme complexes immobilized on an inert support are provided with a silicone coating obtained by hydrosilylation. It is inventively preferred that in process step B) a pH of 4 to 9.5 is present. This pH is advantageously adjusted by means of an acid, in particular an inorganic acid, preferably from the group of sulfuric acid, hydrochloric acid or acetic acid.
  • process step B) a temperature of 20 to 40 ° C, preferably from 25 to 35 ° C, measured in the sucrose-containing solution.
  • process step C) the enzyme complex is separated from the isomaltulose; This is done for example by filtration, sedimentation or centrifugation. Due to the immobilization character of the enzyme complex, this separation is facilitated over non-immobilized enzyme.
  • the immobilized enzyme complex is used in the form of a fixed bed through which the sucrose-containing solution flows (H. Schiweck, Zuckerind. (1990), 15 (7), 555-565).
  • a fixed bed through which the sucrose-containing solution flows
  • process steps A) to C) take place continuously, and thus merge into one another up to simultaneously.
  • step D) isomaltulose seed crystals are added, in particular in an amount of 0.01 to 10 wt .-% and particularly preferably 0.1 to 1 wt .-% based on the theoretical calculated amount of crystal.
  • the speed of sound is measured with a commercial probe to determine the speed of sound. Typical manufacturers of sound velocity probes are Sensotech (Magdeburg, Germany) or Anton Paar (Graz, Austria)
  • a preferred process according to the invention is characterized in that process step D) in a temperature range from 50 ° C to 70 ° C, preferably from 55 ° C to 65 ° C, more preferably from 58 ° C to 62 ° C and in a pressure range of 70 mbar to 200 mbar, preferably from 100 mbar to 180, more preferably from 1 10 mbar to 140 mbar is carried out.
  • process step D) is carried out in a temperature range from 58 ° C. to 62 ° C. and in a pressure range from 110 mbar to 140 mbar.
  • process step D By varying the degree of evaporation different solids contents or yields can be approached, this can be controlled for example over the residence time in process step D). It is advantageous and thus preferred if in process step D) so much water is removed, so that based on the resulting suspension, these 20 wt .-% to 70 wt .-%, preferably 30 wt .-% to 65 wt .-% , More preferably 40 wt .-% to 60 wt .-% isomaltulose as a solid.
  • process step E all processes known to those skilled in the art for the separation of solids from liquids can be used, for example centrifugation, sedimentation, decantation, separation in the gravitational field and filtration.
  • a process preferred according to the invention is characterized in that the separation in process step E) takes place by centrifugation.
  • the washing in step F) is carried out with water, in particular with water, which has a temperature of 20 ° C to 90 ° C, preferably from 30 ° C to 80 ° C, particularly preferably from 50 ° C to 70 ° C.
  • step F) for washing in particular the water used for washing, the feed solution of process step C) is supplied.
  • a preferred process according to the invention is thus characterized in that the feed solution of process step C) containing isomaltulose and water contains the liquid used for washing in process step F);
  • the feed solution particularly preferably contains the liquid used for washing in process step F) and the direct isomerization product of a sucrose-containing vegetable juice.
  • the method according to the invention is characterized in that it additionally comprises the method steps G) cooling the mother liquor from process step E) to obtain a second suspension of isomaltulose crystals,
  • step D) and process step F) in a temperature range of 50 ° C to 70 ° C, preferably from 55 ° C to 65 ° C, particularly preferably of 58 ° C is carried out to 62 ° C and in a pressure range from 70 mbar to 200 mbar, preferably from 100 mbar to 180, more preferably from 1 10 mbar to 140 mbar.
  • step D) also method step F) in a temperature range of 58 ° C to 62 ° C and in a pressure range of 1 10 mbar to 140 mbar is performed.
  • a preferred process according to the invention is characterized in particular by the fact that in process step G) the mother liquor from process step E) is from 10 ° C. to 30 ° C., preferably from 15 ° C. to 25 ° C., more preferably from 18 ° C. to 22 ° C. is cooled, the pressure preferably corresponds to the surrounding air pressure of 0.9 to 1, 1 bar.
  • Process step H) of the preferred process according to the invention the same processes for the separation of solids from liquids can be used as in process step E) of the process according to the invention to obtain a second isomaltulose-containing solid and a second mother liquor;
  • Process step H) is preferably carried out at 10 ° C to 30 ° C, preferably at 15 ° C to 25 ° C, more preferably at 18 ° C to 22 ° C.
  • the second isomaltulose-containing solid can be further processed into end products or - as proposed - in process step I) in the feed solution of process step C) are added, it being preferred that the second isomaltulose-containing solid after addition to the feed solution of process step C) in this solved present.
  • process step I) is carried out in the process according to the invention.
  • An inventively preferred method is thus characterized in that the feed solution of process step C) containing isomaltulose and Contains water;
  • the feed solution particularly preferably contains the second isomaltulose-containing solid from process step H) and the liquid used in step F) for washing.
  • Figure 1 Exemplary, technical process control of crystallization
  • Protaminobacter rubrum (CBS574.77) were cells with 1 - 5 mL of a sterile nutrient medium consisting of 50 g / kg sucrose, 15 g / kg corn steep liquor, 7 g / kg ammonium sulfate, 0.5 g / kg yeast extract, 1 g / kg of potassium dihydrogen sulfate, 0.41 g / kg of magnesium chloride heptahydrate, 0.004 g / kg of manganese chloride tetrahydrate, 0.047 g / kg of iron citrate monohydrate and 926 g / kg of water, if necessary adjusted to pH 7.2, washed off.
  • This suspension served as inoculum for the preculture containing 200 mL of the above nutrient solution in a 1 L shake flask.
  • a 2-liter fermenter containing one liter of sterile production medium consisting of 50 g / kg sucrose, 15 g / kg corn steep liquor, 3 g / kg ammonium sulfate, 4 g / kg ammonium hydrogenphosphate, 0.5 g / kg yeast extract, 1 g / kg potassium dihydrogen sulfate, 0.41 g / kg magnesium chloride heptahydrate, 0.004 g / kg manganese chloride tetrahydrate, 0.047 g / kg iron citrate monohydrate and 926 g / kg water, adjusted to pH 7.2, inoculated such that the initial optical density (OD 6 oo) was 1.
  • sterile production medium consisting of 50 g / kg sucrose, 15 g / kg corn steep liquor, 3 g / kg ammonium sulfate, 4 g / kg ammonium hydrogenphosphate, 0.5 g / kg yeast extract, 1 g / kg potassium dihydrogen
  • the resulting suspension was mixed with water and a 4% alginate solution in a volume ratio of 1: 1. This suspension was then immobilized by dropping into a 2% CaCl 2 solution. The resulting spheres were post-cured with polyethlyeneimine and glutaraldehyde. The biocatalyst obtained is storable for several weeks at 4-10 ° C.
  • the resulting immobilized cells are placed in a temperature-controlled column reactor and heated to 20-35 ° C and continuously flowed through with diluted syrup from sugar beet with a content of 41 wt .-% sucrose based on the total thickness of the syrup.
  • composition after isomerization is shown in Table 1.
  • Example 2 Crystallization of the isomerized thick juice stage 1
  • the starting material was an isomerized thick juice from Example 1 available.
  • the solid was then washed at a speed of 500 rpm on the centrifuge with 90 g ultrapure water. For subsequent spin-drying, the centrifuge was set to a speed of 4000 rpm. It could be removed a loaded amount of wash water of 225.3 g. From the filter cloth 574 g of washed solid could be recovered. The solid had a residual moisture content of 3%. The solid-liquid separation thus results in a mass difference of 153.7 g or a relative mass loss of 10.1%.
  • the separated solid had the following composition, with the indicated water being water of crystallization of isomaltulose:
  • the mother liquor was then treated in a further stage. This was done via a so-called. Cooling crystallization of 60 ° C to about 20 ° C.
  • the one aqueous solution containing the mother liquor with a mass of 857.9 g was added back into the crystallizer and tempered at 60 ° C.
  • the temperature was slowly cooled in 0.2 K / min increments.
  • 1.8 g of seed crystals with a particle size ⁇ 20 ⁇ m were added.
  • the seed amount corresponds to about 0.5-1% of the expected amount of crystal.
  • the addition can be carried out, for example, via a suspension of the seed crystals in isopropanol.
  • the suspension was heated with stirring for about 30 minutes at 20 ° C. From the crystallizer 575.8 g of suspension could be removed and added at a speed of 500 rpm in the centrifuge. This corresponds to a mass difference at the beginning of the crystallization of 56.8 g or a relative Fahler of 8.9%.
  • the speed was increased to 4000 rpm.
  • a crystal wash was not intended for stage 2, since the recovered solid in the later process in stage 1 is redissolved and recrystallized shall be.
  • 334.8 g of mother liquor and 180.8 g of solid were obtained. The solid had a residual moisture content of 6%.
  • a yield based on the read employed in step 1 isomaltulose calculate: v _ m solid 'C X RF)' X isomaltulose; solid m in pfkristalle _ 80.8 x (1 - 0.06) ⁇ 0.869 - 1,8 _. 7,.
  • Example 3 Example of a technical process control of crystallization
  • FIG. 1 A possible technical process control of a preferred method according to the invention is shown in FIG. 1:
  • the feed solution (1) is used at the beginning of the process to remove the non-washed solid (14) from the crystallization stage S2 (H) / solid-liquid separation (I) and the wash water (10) from the crystal wash (E / F).
  • the mixture (3) is then used in the evaporation crystallization S1 (D).
  • evaporation at 60 ° C and a pressure of 130 to 150 mbar of a corresponding water content (5) exceeded the solubility of isomaltulose, so that crystallized isomaltulose and suspension (4) from the evaporation crystallization (D) on the solid-liquid-T tion / crystal washing (E / F) can be driven.
  • the isomaltulose crystals are separated from the mother liquor (11).
  • the mother liquor-containing solid is washed with ultrapure water (7).
  • the wash water (10) is fed back against the test procedure the feed stream for workup again.
  • the washed crystals (6) are used for product preparation (J).
  • the product preparation can be carried out as drying or as a solution station with ultrapure water (9).
  • the mother liquor (11) is fed to a cooling crystallization (G).
  • the solution is cooled down from 60 ° C to a temperature of 20 ° C. In this case, the solubility limit of isomaltulose is exceeded so that isomaltulose crystallizes out and a suspension (12) is formed.
  • the suspension (12) is fed from the cooling crystallization (G) to the solid-liquid separation (H).
  • the generated crystals (14) are separated from the mother liquor (13).
  • the crystals are not washed.
  • the mother liquor (13) leaves the procedure.
  • the solid (14) is redissolved for recrystallization in the isomaltulose feed stream (1).
  • buffer tanks, etc. are not listed for possible batchwise operation of the crystallization stages.

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  • Mycology (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
  • Immobilizing And Processing Of Enzymes And Microorganisms (AREA)
  • Enzymes And Modification Thereof (AREA)
  • Micro-Organisms Or Cultivation Processes Thereof (AREA)
  • Non-Alcoholic Beverages (AREA)

Abstract

L'invention concerne un procédé d'isomérisation d'une sève à base de saccharose pour former de l'isomaltulose.
EP12717789.7A 2011-05-05 2012-05-04 Procédé de production d'isomaltulose à partir de sèves Withdrawn EP2704595A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102011100772A DE102011100772A1 (de) 2011-05-05 2011-05-05 Verfahren zur Herstellung von Isomaltulose aus Pflanzensäften
PCT/EP2012/058228 WO2012150332A1 (fr) 2011-05-05 2012-05-04 Procédé de production d'isomaltulose à partir de sèves

Publications (1)

Publication Number Publication Date
EP2704595A1 true EP2704595A1 (fr) 2014-03-12

Family

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Family Applications (2)

Application Number Title Priority Date Filing Date
EP12702557.5A Not-in-force EP2704594B1 (fr) 2011-05-05 2012-02-08 Procédé de production d'isomaltulose à partir de jus de végétaux
EP12717789.7A Withdrawn EP2704595A1 (fr) 2011-05-05 2012-05-04 Procédé de production d'isomaltulose à partir de sèves

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EP12702557.5A Not-in-force EP2704594B1 (fr) 2011-05-05 2012-02-08 Procédé de production d'isomaltulose à partir de jus de végétaux

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EP (2) EP2704594B1 (fr)
CN (2) CN103501636A (fr)
AU (2) AU2012251903A1 (fr)
BR (2) BR112013028369A2 (fr)
DE (1) DE102011100772A1 (fr)
TW (1) TW201307565A (fr)
WO (2) WO2012150051A1 (fr)

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DE102016210478A1 (de) 2016-06-14 2017-12-14 Evonik Degussa Gmbh Verfahren zur Entfeuchtung von feuchten Gasgemischen
EP3257568B1 (fr) 2016-06-14 2019-09-18 Evonik Degussa GmbH Procede de deshumidification de melanges gazeux humides par des liquides ioniques
DE102016210484A1 (de) 2016-06-14 2017-12-14 Evonik Degussa Gmbh Verfahren zur Entfeuchtung von feuchten Gasgemischen
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DE102016210481B3 (de) 2016-06-14 2017-06-08 Evonik Degussa Gmbh Verfahren zum Reinigen einer ionischen Flüssigkeit
EP3257843A1 (fr) 2016-06-14 2017-12-20 Evonik Degussa GmbH Procédé pour préparer un sel tres pur d'imidazolium
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CN114703211A (zh) * 2022-02-16 2022-07-05 李宪臻 一种融合卷曲螺旋结构域的蔗糖异构酶活性包涵体
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Publication number Publication date
BR112013028410A2 (pt) 2019-09-24
EP2704594B1 (fr) 2016-04-27
BR112013028369A2 (pt) 2017-03-01
TW201307565A (zh) 2013-02-16
AU2012251903A1 (en) 2013-10-24
CN103501637A (zh) 2014-01-08
DE102011100772A1 (de) 2012-11-08
WO2012150332A1 (fr) 2012-11-08
CN103501636A (zh) 2014-01-08
EP2704594A1 (fr) 2014-03-12
WO2012150051A1 (fr) 2012-11-08
AU2012251596A1 (en) 2013-10-24

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