WO2014189163A1 - 유청 막 투과액 또는 유청 막 투과 분말로부터 타가토스의 제조 원료가 되는 갈락토스를 제조하는 방법 - Google Patents
유청 막 투과액 또는 유청 막 투과 분말로부터 타가토스의 제조 원료가 되는 갈락토스를 제조하는 방법 Download PDFInfo
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- WO2014189163A1 WO2014189163A1 PCT/KR2013/004544 KR2013004544W WO2014189163A1 WO 2014189163 A1 WO2014189163 A1 WO 2014189163A1 KR 2013004544 W KR2013004544 W KR 2013004544W WO 2014189163 A1 WO2014189163 A1 WO 2014189163A1
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- membrane permeate
- whey
- solution
- powder
- whey membrane
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- 108010046377 Whey Proteins Proteins 0.000 title claims abstract description 94
- 102000007544 Whey Proteins Human genes 0.000 title claims abstract description 94
- 239000005862 Whey Substances 0.000 title claims abstract description 93
- 239000012466 permeate Substances 0.000 title claims abstract description 73
- 239000000843 powder Substances 0.000 title claims abstract description 53
- 229930182830 galactose Natural products 0.000 title claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 30
- BJHIKXHVCXFQLS-PQLUHFTBSA-N keto-D-tagatose Chemical compound OC[C@@H](O)[C@H](O)[C@H](O)C(=O)CO BJHIKXHVCXFQLS-PQLUHFTBSA-N 0.000 title claims abstract description 27
- 239000007788 liquid Substances 0.000 title abstract description 6
- 239000002994 raw material Substances 0.000 title description 16
- 102000004169 proteins and genes Human genes 0.000 claims abstract description 47
- 108090000623 proteins and genes Proteins 0.000 claims abstract description 47
- 238000000034 method Methods 0.000 claims abstract description 39
- 239000007787 solid Substances 0.000 claims abstract description 31
- 239000002244 precipitate Substances 0.000 claims abstract description 29
- 150000003839 salts Chemical class 0.000 claims abstract description 16
- 239000012528 membrane Substances 0.000 claims description 77
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 70
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 claims description 32
- 239000008101 lactose Substances 0.000 claims description 31
- 230000008569 process Effects 0.000 claims description 20
- 235000000346 sugar Nutrition 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 238000000909 electrodialysis Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000006227 byproduct Substances 0.000 claims description 12
- 108090000790 Enzymes Proteins 0.000 claims description 11
- 102000004190 Enzymes Human genes 0.000 claims description 11
- 238000004042 decolorization Methods 0.000 claims description 5
- 238000000746 purification Methods 0.000 claims description 5
- 230000000593 degrading effect Effects 0.000 claims description 4
- 238000013375 chromatographic separation Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000006317 isomerization reaction Methods 0.000 abstract 1
- 235000018102 proteins Nutrition 0.000 description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 11
- 230000008859 change Effects 0.000 description 11
- 229940088598 enzyme Drugs 0.000 description 10
- 230000001965 increasing effect Effects 0.000 description 10
- 238000005119 centrifugation Methods 0.000 description 8
- 238000001556 precipitation Methods 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- 238000010612 desalination reaction Methods 0.000 description 7
- 150000002500 ions Chemical class 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 239000003765 sweetening agent Substances 0.000 description 6
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 5
- WQZGKKKJIJFFOK-PHYPRBDBSA-N alpha-D-galactose Chemical compound OC[C@H]1O[C@H](O)[C@H](O)[C@@H](O)[C@H]1O WQZGKKKJIJFFOK-PHYPRBDBSA-N 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 235000003599 food sweetener Nutrition 0.000 description 5
- 239000008103 glucose Substances 0.000 description 5
- 239000006228 supernatant Substances 0.000 description 5
- 150000001720 carbohydrates Chemical class 0.000 description 4
- 235000014633 carbohydrates Nutrition 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000007071 enzymatic hydrolysis Effects 0.000 description 4
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000002198 insoluble material Substances 0.000 description 4
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 description 3
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 3
- 238000004587 chromatography analysis Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000004445 quantitative analysis Methods 0.000 description 3
- 102100026189 Beta-galactosidase Human genes 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 108010059881 Lactase Proteins 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 108010005774 beta-Galactosidase Proteins 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000003544 deproteinization Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000003925 fat Substances 0.000 description 2
- 235000019197 fats Nutrition 0.000 description 2
- 239000002778 food additive Substances 0.000 description 2
- 230000001939 inductive effect Effects 0.000 description 2
- 238000004255 ion exchange chromatography Methods 0.000 description 2
- 239000003014 ion exchange membrane Substances 0.000 description 2
- 229940116108 lactase Drugs 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 238000010979 pH adjustment Methods 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 235000021391 short chain fatty acids Nutrition 0.000 description 2
- 150000004666 short chain fatty acids Chemical class 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 150000008163 sugars Chemical class 0.000 description 2
- PKAUICCNAWQPAU-UHFFFAOYSA-N 2-(4-chloro-2-methylphenoxy)acetic acid;n-methylmethanamine Chemical compound CNC.CC1=CC(Cl)=CC=C1OCC(O)=O PKAUICCNAWQPAU-UHFFFAOYSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 238000009010 Bradford assay Methods 0.000 description 1
- FERIUCNNQQJTOY-UHFFFAOYSA-M Butyrate Chemical compound CCCC([O-])=O FERIUCNNQQJTOY-UHFFFAOYSA-M 0.000 description 1
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Natural products CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 1
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- LKDRXBCSQODPBY-OEXCPVAWSA-N D-tagatose Chemical compound OCC1(O)OC[C@@H](O)[C@H](O)[C@@H]1O LKDRXBCSQODPBY-OEXCPVAWSA-N 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 208000008589 Obesity Diseases 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000003011 anion exchange membrane Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 235000019784 crude fat Nutrition 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 235000013365 dairy product Nutrition 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
- 230000036425 denaturation Effects 0.000 description 1
- 208000002925 dental caries Diseases 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000011033 desalting Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000019621 digestibility Nutrition 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 238000006911 enzymatic reaction Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000013402 health food Nutrition 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000000968 intestinal effect Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 210000002429 large intestine Anatomy 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000007567 mass-production technique Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000037323 metabolic rate Effects 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013615 non-nutritive sweetener Nutrition 0.000 description 1
- 235000020824 obesity Nutrition 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 235000013406 prebiotics Nutrition 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 210000000813 small intestine Anatomy 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 235000021092 sugar substitutes Nutrition 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 235000021119 whey protein Nutrition 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H3/00—Compounds containing only hydrogen atoms and saccharide radicals having only carbon, hydrogen, and oxygen atoms
- C07H3/02—Monosaccharides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/42—Electrodialysis; Electro-osmosis ; Electro-ultrafiltration; Membrane capacitive deionization
- B01D61/422—Electrodialysis
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
-
- 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
- C12P19/02—Monosaccharides
Definitions
- the present invention relates to a method for producing galactose, which is a raw material for producing tagatose, from whey permeate or whey permeate powder (hereinafter referred to as 'DWP').
- 'DWP' whey permeate or whey permeate powder
- Tagatose is an ideal sugar replacement sweetener that can satisfy consumers' desires, with a sweetness almost equivalent to sugar (about 90%) or a low-calorie sweetener that is about 30% sugar.
- tagatose is a stereoisomer of galactose, which is known to be used as a low-calorie sugar substitute sweetener having low metabolic rate and low absorption rate in the body, without side effects.
- Tagatose absorbs only about 20% of the intake from the small intestine, and the remaining 80% is transported to the large intestine where the intestinal microbes live, selectively producing lactic acid bacteria, thereby producing short-chain fatty acids. butyrate) has a prebiotic property that produces large amounts (up to 50% of total short-chain fatty acids).
- Tagatose is a low-calorie natural sugar of 1.5 kcal / g, and is recognized as the General Recognized As Safe (GRAS) by the US FDA, and is used as a functional sweetener in foods, beverages, health foods, and dietary additives.
- GRAS General Recognized As Safe
- tagatose is not commonly present in nature but is a rare sugar contained in dairy products and some plants, a mass production technique must be developed from inexpensive raw materials to be used as a low-calorie functional sweetener.
- U.S. Pat.Nos. 5002612 and 5078796 use lactase to hydrolyze lactose or lactose-containing substances into a mixture of galactose and glucose, optionally remove glucose, and then chemically isomerize galactose to tagatose.
- Whey membrane permeate or whey membrane permeate contains protein, ash (including salt), and other impurities in addition to carbohydrate (lactose) components.
- lactose carbohydrate
- the precipitate is removed by inducing a solidification reaction without changing the sugar content and generating a reaction by-product from the dissolved solution of the whey membrane permeate or the whey membrane permeate through physical and chemical pretreatment such as pH adjustment and heat treatment.
- Economical protein removal was achieved by using activated charcoal without using a conventional relatively expensive adsorption method or ion chromatography method to remove proteins from the dissolved whey membrane permeate or the dissolved solution of whey membrane permeate powder.
- the whey membrane permeate or whey membrane permeate powder solution in which the solid precipitate and the protein are removed as described above may be removed by electrodialysis to remove salts, ash or both, and the method according to the present invention may be Pretreatment of the precipitate and protein removal has the advantage of minimizing the degree of contamination of the electrodialysis membrane and increasing the desalination efficiency during electrodialysis.
- the present invention develops a process for effectively and economically removing proteins, ash (including salts), and other solid precipitates, which are components other than lactose in whey membrane permeate or whey membrane permeate powder, which are by-products in the production of whey isolate proteins.
- This overcomes the supply and cost dependence of refined lactose and / or crystalline lactose, which is a raw material for tagatose production at present, and has an effect of directly or indirectly improving the production cost of tagatose.
- the present invention also provides a technology that can economically utilize whey membrane permeate or whey membrane permeation powder, which are by-products of the production of whey isolate proteins, which have relatively high industrial utilization.
- 1 is a flow chart showing the overall process of the method for producing galactose according to an aspect of the present invention.
- Figure 2 shows the result of the solidified precipitate dry weight removed as a result of 20% (w / v) DWP solution dissolved in pH 6.8, heat treatment, centrifugation at 70 °C for 30 minutes.
- Figure 3 shows the deproteination rate results of protein removal after each powder activated carbon (A to F) treatment.
- Figure 4a is a graph showing the result of protein removal rate according to the temperature and time condition changes after treatment with activated carbon A in the powdered activated carbon of Figure 3,
- FIG. 5 is a photograph showing deproteinization and decolorization results when activated carbon A is treated in the powdered activated carbon of FIG. 3.
- 6 is a graph showing the electrical conductivity and the rate of change of current according to the change in electrodialysis operation time.
- a method for preparing galactose from a whey membrane permeate or whey membrane permeate powder solution comprising removing ash, salt or both from the protein-removed whey membrane permeate solution or whey membrane permeate powder solution. It is about.
- the method for producing galactose according to the present invention is based on whey membrane permeate or whey membrane permeate powder generated as a by-product during the manufacturing process of whey isolate protein, and in the case of whey membrane permeate, solid precipitates are removed without further treatment. Can be carried out.
- whey membrane permeable powder When whey membrane permeable powder is used as a raw material, it can be dissolved in solvent water to prepare a whey membrane permeable powder solution for processing thereof, and solid precipitates can be removed therefrom.
- 'whey separated protein' refers to whey protein separated and recovered through a membrane permeation process using whey as a raw material.
- 'whey membrane permeate' refers to a membrane permeate that is a by-product that occurs during the process of preparing the 'whey separated protein'.
- the term 'whey membrane permeation powder' refers to a powder obtained by concentrating and drying the whey membrane permeate.
- the step of removing the solid precipitate produces a solid precipitate from a solution of whey membrane permeate or whey membrane permeate powder by a heat treatment process of 40 to 90 ° C., adjustment to pH 3 to 9, or both, and the resulting solid
- the precipitate can be carried out by separating and removing the precipitate by a conventional method such as centrifugation.
- the heat treatment at 40 to 90 ° C., the adjustment to pH 3 to 9, is performed without changing the sugar content or generating the reaction byproduct in the solution of the whey membrane permeate or the whey membrane permeate powder.
- Precipitating the solid component in the powder solution has the effect of removing the solid component without affecting the content or quality of the final product galactose.
- the temperature of the heat treatment process is preferably 50 to 80 °C
- the pH adjustment process may be preferably pH 4 to 8.
- the precipitation degree of the solid insoluble material which is not a protein or a carbohydrate (lactose) component increases, and the precipitation degree of the solid insoluble material may increase as the pH is increased. Therefore, as the heat treatment temperature is raised and the pH is raised, precipitation of the solid insoluble substance may be accelerated, and the solid precipitate may increase significantly.
- the solid precipitate removal step may be carried out by warming the temperature of the heat treatment process to 60 to 80 °C, adjust the pH to 5 to 8.
- the protein in the method for producing galactose according to the present invention, can be removed from the solution of the whey membrane permeate or the whey membrane permeate powder from which the solid precipitate is removed.
- the protein removal step is advantageous in that economical protein removal is possible by using activated carbon without using a conventional relatively expensive adsorption method or ion chromatography method.
- the step of removing the protein by treatment with activated charcoal is to treat the dissolved solution of whey membrane permeate or whey membrane permeate powder from which the solid precipitate is removed with activated charcoal and react at 20 to 90 ° C. for 10 minutes to 9 hours.
- the activated carbon may be preferably powdered activated carbon, for example, A to F, but is not limited thereto.
- Activated carbon A specified in the present invention is Norit's DARCOKB-B, B is Norit's NORITCGSP, C is Norit's NORITCASP, D is Norit's NORITCA1, E is Norit's A51, F is Norit's NoritSX plus. More particularly preferably A or B can be used in terms of protein removal efficiency.
- the activated carbon treatment conditions may be preferably reacted for about 3 hours to 8 hours at a temperature of 50 to 80 °C, more particularly preferably about 4 hours to about 7 hours at a temperature of 55 to 75 °C. .
- the method for producing galactose according to the present invention may further include removing ash, salts, or both from the whey membrane permeate from which the protein is removed or the solution of the whey membrane permeate powder.
- the removal of the ash, salt or both may preferably be carried out by electrodialysis.
- the solid precipitate removal step and the protein removal step are performed before the electrodialysis, the degree of contamination of the electrodialysis membrane is minimized, thereby extending the life and improving the salt removal efficiency.
- lactose decomposition is performed in a solution of whey membrane permeate or whey membrane permeate powder before or after any one of the solid precipitate removal step, protein removal step, and ash and / or salt removal step.
- the addition of the enzyme may further comprise the step of producing galactose.
- the step of adding the lactose degrading enzyme may be performed after the solid precipitate is removed and before the protein removal step.
- lactose degrading enzyme can be used without limitation, known enzymes, for example, DSM's Maxilact LX 5000, or Maxilact LG 5000.
- the concentration of the enzyme added in the step of adding lactose degrading enzyme is preferably 0.01 to 5 w / v%, it can be hydrolyzed through the enzyme using a fermenter of 35 to 39 °C.
- the process according to the invention may further comprise ion purification, concentration and chromatographic separation processes after the salt and / or ash removal step.
- ion purification and concentration processes are included to separate, purify and recover galactose using SMB (Simulated Moving Bed) chromatography.
- Cation and anion purification chromatography which typically uses ion removal, may be used, and may also be included before SMB chromatography separation and purification through a concentration process commonly used by those skilled in the art.
- Another aspect of the invention relates to a process for producing tagatose, comprising the step of isomerizing galactose produced by the method described above to obtain tagatose.
- a component analysis in whey membrane permeable powder a by-product generated during the manufacturing process of whey isolate protein, was performed to confirm the content and type of impurities in the raw materials.
- the results of the component analysis in the whey membrane permeable powder are shown in Table 1 below. It has a lactose content of over 80% in whey membrane permeable powder and contains proteins, fats, various inorganic salts and heavy metals in addition to sugars. The remaining components except the sugar component are to be removed using physical and chemical pretreatment.
- Whey membrane permeable powder 4g of Hilmar Corporation was suspended and dissolved ( ⁇ 20%, w / v) in 20 ml of solvent water to prepare a whey membrane permeable powder solution.
- Physical and chemical pretreatment of the DWP solution was intended to remove only impurities by inducing solid insoluble precipitation without changing sugar content and generating reaction byproducts in DWP.
- the prepared whey membrane permeate powder solution was heat-treated at 50-80 ° C. for 1 hour.
- the suspension was titrated to pH 4.0-8.0 with HCl and NaOH, and then treated at room temperature ( ⁇ 25 ° C.) for 1 hour. Centrifugation was performed to recover the supernatant, pH (pH meter), conductivity (conductivity meter), Brix (Brix meter), lactose (HLC composition and quantitative analysis) and protein content (Bradford Protein Assay) Protein content quantitative analysis), the change in the degree of precipitation production was analyzed (Table 2).
- the enzyme was hydrolyzed using a fermenter adjusted to 38 ° C. and 100 rpm after putting the pretreated sample and the enzyme at a concentration of 1% (w / v) in Example 2.
- the corresponding sample was taken at 0, 10, 24, 31, 48 and 58 hours after enzymatic hydrolysis was started to calculate the content of glucose and galactose produced.
- the content of glucose and galactose was quantitatively calculated using an HPLC equipped with a BioRad Aminex HPX-87C column.
- the electrodialysis machine uses a 3-compartment type device, and detailed electrodialysis machine specifications and operating conditions are shown in Table 4 below.
- CMX CMX, AMX, Astom, Japan
- CMX CMX, AMX, Astom, Japan
- CMX Citem Cation Exchange Membrane
- AMX Anion exchange membrane
- ⁇ 1.8 ⁇ 3.8 2.0-3.5 Burt strength ⁇ 0.40 ⁇ 0.30 Thickness (mm) 0.14-0.20 0.12-0.15
- Table 7 shows the results of continuously operating the deproteinated lactose hydrolyzate without chemical cleaning.
- Ion removal rate 100- ⁇ (raw water electrical conductivity value / treated water electrical conductivity value) * 100 ⁇
- the desalination rate of ions was 98% on average and the recovery rate of sugar was 80% on average.
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
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- General Engineering & Computer Science (AREA)
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- Polysaccharides And Polysaccharide Derivatives (AREA)
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Abstract
Description
총 성분 | |
총 탄수화물 | 86.9% |
총 단백질 | 3.6% |
총 지방 | 0.2% |
수분 | - |
회분 | 9.5% |
염 | |
칼슘 이온 | 742.99 mg/100g |
마그네슘 이온 | 135.54 mg/100g |
나트륨 이온 | 562.99 mg/100g |
칼륨 이온 | 2231.12 mg/100g |
철 | 0.22 mg/100g |
인 | 113.1 mg/100g |
아연 | 0.05 mg/100g |
구리 | 0.03 mg/100g |
망간 | 0.01 mg/100g |
셀레늄 | 36.23 ug/100g |
당 | |
유당 | 85.1% |
갈락토스 | 1.6% |
분석항목 | 온도(℃)-60분 반응a | pH(HCl/NaOH로 pH 보정)-상온에서 60분 반응 | |||||||
50 | 60 | 70 | 80 | 4.0 | 5.0 | 6.0 | 7.0 | 8.0 | |
pH | 5.745(5.778)b | 5.712(5.763) | 5.6(5.796) | 5.449(5.781) | 3.9 | 5.0 | 6.1 | 7.0 | 7.7 |
전도도(㎲/cm) | 11980(12040) | 11670(12130) | 11630(12220) | 11850(12200) | 14030 | 12500 | 11720 | 12390 | 12910 |
Brix(%) | 16.82(16.82) | 16.75(16.49) | 16.65(16.61) | 16.76(16.76) | 16.2 | 16.7 | 16.5 | 16.4 | 16.6 |
락토스(g/L) | 159.3(153.1) | 153.7(156.0) | 154.8(153.3) | 155.9(155.5) | 145.8 | 157.5 | 155.4 | 153.1 | 151.5 |
단백질(g/L) | 0.230(0.227) | 0.233(0.227) | 0.229(0.227) | 0.228(0.228) | 0.217 | 0.232 | 0.238 | 0.237 | 0.239 |
반응조건 | 반응시간(hr) | 유당함량(g/L) | 글루코스(g/L) | 갈락토스(g/L) | 총당함량(g/L) | 소화율(%) |
20L DWP 용해액(200g DWP/L 물) | 0 | 227.5 | 227.5 | |||
10 | 28.4 | 97.4 | 78.7 | 204.5 | 77.4 | |
24 | 13.1 | 104.6 | 97.8 | 215.5 | 89.0 | |
31 | 10.5 | 106.3 | 102.3 | 219.1 | 91.7 | |
48 | 7.4 | 108.1 | 107.5 | 223.1 | 94.8 | |
58 | 6.9 | 109.6 | 109.8 | 226.3 | 96.5 |
구분 | 내용 |
장치 | Micro Acilyzer S3 |
총유효막면적 | 0.55 dm2/cell |
카트리지 | AC-220-550 |
전극 | Ti/Pt (Anode)SUS316L(Cathode) |
운전전압 | 9V-12V |
운전온도 | 23℃-32℃ |
샘플액 | 500 ml |
전극액 | 5% Na2SO4 |
항목 | 양이온교환막(CMX) | 음이온교환막(AMX) |
종류 | 강산성 양이온 투과성 | 강염기성 음이온 투과성 |
특징 | 높은 기계강도 (Na-form) | 높은 기계강도 (Cl-form) |
전기 저항(Ω) | 1.8~3.8 | 2.0~3.5 |
브랏(Burat) 강도 | ≥0.40 | ≥0.30 |
두께 (mm) | 0.14~0.20 | 0.12~0.15 |
항목 | 원수 | 처리수 | 제거율(%) |
pH | 6.8 | 6.2 | - |
Brix (%) | 15.8 | 12.6 | 20.0 |
전기 전도도 (㎲/㎝) | 15600 | 300 | 98.10 |
단백 함량 (%) | 0.23 | 0.18 | 21.74 |
조지방 함량 (%) | 0.20 | 0.15 | 25.00 |
연속운전[batch수] | 운전전압[V] | 탈염시간[min] | 당회수율[%] | 이온제거율[%] | 탈염제거속도[LMH] | 에너지소비량[Wh] |
1회 | 9~12 | 56 | 77 | 98.1 | 9.9 | 6.9 |
2회 | 9~12 | 50 | 80 | 97.6 | 11.3 | 4.6 |
3회 | 9~12 | 50 | 79 | 98.0 | 11.2 | 4.3 |
4회 | 9~12 | 50 | 82 | 97.8 | 11.3 | 4.8 |
5회 | 9~12 | 50 | 81 | 98.1 | 11.2 | 4.9 |
Claims (12)
- 유청 막 투과액 또는 유청 막 투과 분말의 용해액으로부터 고형 침전물을 제거하는 단계;상기 고형 침전물이 제거된 유청 막 투과액 또는 유청 막 투과 분말의 용해액으로부터 단백질을 제거하는 단계; 및상기 단백질이 제거된 유청 막 투과액 또는 유청 막 투과 분말의 용해액으로부터 회분, 염 또는 이 둘 다를 제거하는 단계를 포함하는, 유청 막 투과액 또는 유청 막 투과 분말 용해액으로부터 갈락토스를 제조하는 방법.
- 제1항에 있어서, 상기 고형 침전물의 제거 단계가 40 내지 90℃의 열처리 공정, pH 3 내지 9로 조정, 또는 이 둘 다에 의해 유청 막 투과액 또는 유청 막 투과 분말의 용해액으로부터 고형 침전물을 생성시키고 이를 제거하는 단계를 포함하는, 방법.
- 제2항에 있어서, 상기 고형 침전물의 제거 단계가 유청 막 투과액 또는 유청 막 투과 분말의 용해액 중 당 함량의 변화 또는 반응 부산물의 생성 없이 실시되는 것을 특징으로 하는, 방법.
- 제1항에 있어서, 상기 단백질 제거 단계가 활성탄을 처리하고 10분 내지 8시간 동안 20 내지 90℃에서 반응시키는 것을 포함하는, 방법.
- 제4항에 있어서, 상기 단백질 제거 단계에서 추가로 탈색이 이루어지는 것을 특징으로 하는, 방법.
- 제4항에 있어서, 상기 활성탄이 분말 활성탄인, 방법.
- 제1항에 있어서, 상기 회분, 염 또는 이 둘 다의 제거 단계가 전기투석에 의해 수행되는 것을 포함하는, 방법.
- 제1항 내지 제7항 중 어느 하나의 항에 있어서, 유청 막 투과액 또는 유청 막 투과 분말의 용해액에 유당 분해 효소를 첨가하여 갈락토스를 생성시키는 단계를 추가로 포함하는, 방법.
- 제8항에 있어서, 상기 갈락토스 생성 단계의 반응 온도 및 반응 시간이 각각 35 내지 39℃, 및 50 내지 60시간인 방법.
- 제8항에 따른 방법에 의해 제조된 갈락토스를 이성화시켜 타가토스를 수득하는 단계를 포함하는 것을 특징으로 하는, 타가토스의 제조 방법.
- 제1항 내지 제7항 중 어느 하나의 항에 있어서, 상기 회분, 염 또는 이 둘 다를 제거하는 단계 후에 이온 정제, 농축 및 크로마토그래피 분리 과정을 추가로 포함하는, 방법.
- 제1항 내지 제7항 중 어느 하나의 항에 따른 방법에 의해 제조된 갈락토스를 이성화시켜 타가토스를 수득하는 단계를 포함하는 것을 특징으로 하는, 타가토스의 제조 방법.
Priority Applications (8)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
UAA201409069A UA116100C2 (uk) | 2013-05-23 | 2013-05-23 | Метод виробництва d-галактози для використання у виготовленні d-тагатози з фільтрату сироватки або з сухого фільтрату сироватки |
US14/386,771 US10196415B2 (en) | 2013-05-23 | 2013-05-23 | Method of manufacturing D-galactose for use of the production of D-tagatose from whey permeate or dried whey permeate |
NZ628831A NZ628831A (en) | 2013-05-23 | 2013-05-23 | A method of manufacturing d-galactose for use of the production of d-tagatose from whey permeate or dried whey permeate |
AU2013378056A AU2013378056B2 (en) | 2013-05-23 | 2013-05-23 | A method of manufacturing D-galactose for use of the production of D-tagatose from whey permeate or dried whey permeate |
PCT/KR2013/004544 WO2014189163A1 (ko) | 2013-05-23 | 2013-05-23 | 유청 막 투과액 또는 유청 막 투과 분말로부터 타가토스의 제조 원료가 되는 갈락토스를 제조하는 방법 |
CN201380023775.4A CN104321331A (zh) | 2013-05-23 | 2013-05-23 | 从乳清渗透物或干燥乳清渗透物制造用于生产d-塔格糖的d-半乳糖的方法 |
CN201810328579.2A CN108530495A (zh) | 2013-05-23 | 2013-05-23 | 用于生产d-半乳糖和d-塔格糖的方法 |
EP13882627.6A EP3000819B1 (en) | 2013-05-23 | 2013-05-23 | Method for producing galactose constituting a raw material for producing tagatose from whey permeate liquid or whey permeate powder |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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PCT/KR2013/004544 WO2014189163A1 (ko) | 2013-05-23 | 2013-05-23 | 유청 막 투과액 또는 유청 막 투과 분말로부터 타가토스의 제조 원료가 되는 갈락토스를 제조하는 방법 |
Publications (1)
Publication Number | Publication Date |
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WO2014189163A1 true WO2014189163A1 (ko) | 2014-11-27 |
Family
ID=51933707
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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PCT/KR2013/004544 WO2014189163A1 (ko) | 2013-05-23 | 2013-05-23 | 유청 막 투과액 또는 유청 막 투과 분말로부터 타가토스의 제조 원료가 되는 갈락토스를 제조하는 방법 |
Country Status (7)
Country | Link |
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US (1) | US10196415B2 (ko) |
EP (1) | EP3000819B1 (ko) |
CN (2) | CN104321331A (ko) |
AU (1) | AU2013378056B2 (ko) |
NZ (1) | NZ628831A (ko) |
UA (1) | UA116100C2 (ko) |
WO (1) | WO2014189163A1 (ko) |
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US5002612A (en) | 1989-07-19 | 1991-03-26 | Biospherics Incorporated | Process for manufacturing tagatose |
US5078796A (en) | 1989-07-19 | 1992-01-07 | Biospherics Incorporated | Process for manufacturing tagatose |
KR19990038067A (ko) * | 1997-11-03 | 1999-06-05 | 조두업 | 순 자연 발효 응유와 과일 또는 채소를 주원료로한 식품 |
US20040132989A1 (en) * | 2000-12-19 | 2004-07-08 | Lifran Estelle V. | Method for purification of lactose |
US20070134373A1 (en) * | 2003-10-29 | 2007-06-14 | Giovanni Cipoletti | Process for the preparation of galactose |
Family Cites Families (10)
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US1533030A (en) * | 1917-07-26 | 1925-04-07 | Naamlooze Vennootschap Norit W | Purifying and filtering process |
US4202909A (en) * | 1976-11-22 | 1980-05-13 | Patent Technology, Inc. | Treatment of whey |
FR2483748A1 (fr) | 1980-06-06 | 1981-12-11 | Corning Glass Works | Procede d'hydrolyse du lactose contenu dans les lactoserums a l'aide de lactase immobilisee |
AU569612B2 (en) | 1984-04-16 | 1988-02-11 | Fmc Corporation | Process and apparatus to hydrolyse lactose to glucose and galactose |
US6057135A (en) | 1992-01-16 | 2000-05-02 | Kraft Foods, Inc. | Process for manufacturing D-tagatose |
US6991923B2 (en) * | 2001-07-16 | 2006-01-31 | Arla Foods Amba | Process for manufacturing of tagatose |
CN1985624A (zh) * | 2006-11-06 | 2007-06-27 | 广东省食品工业研究所 | 一种塔格糖的生产工艺 |
KR100964091B1 (ko) * | 2008-01-28 | 2010-06-16 | 씨제이제일제당 (주) | 대두 올리고당을 이용한 타가토스의 제조 방법 |
RU2409965C2 (ru) | 2009-04-23 | 2011-01-27 | Государственное образовательное учреждение высшего профессионального образования "Воронежская государственная технологическая академия" | Способ получения тагатозосодержащей добавки подсластителя из молочной сыворотки |
WO2011139683A1 (en) | 2010-05-05 | 2011-11-10 | Pepsico, Inc. | Use of whey for the manufacture of erythritol |
-
2013
- 2013-05-23 NZ NZ628831A patent/NZ628831A/en unknown
- 2013-05-23 EP EP13882627.6A patent/EP3000819B1/en not_active Revoked
- 2013-05-23 CN CN201380023775.4A patent/CN104321331A/zh active Pending
- 2013-05-23 UA UAA201409069A patent/UA116100C2/uk unknown
- 2013-05-23 AU AU2013378056A patent/AU2013378056B2/en active Active
- 2013-05-23 US US14/386,771 patent/US10196415B2/en active Active
- 2013-05-23 WO PCT/KR2013/004544 patent/WO2014189163A1/ko active Application Filing
- 2013-05-23 CN CN201810328579.2A patent/CN108530495A/zh active Pending
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US5002612A (en) | 1989-07-19 | 1991-03-26 | Biospherics Incorporated | Process for manufacturing tagatose |
US5078796A (en) | 1989-07-19 | 1992-01-07 | Biospherics Incorporated | Process for manufacturing tagatose |
KR100190671B1 (ko) * | 1989-07-19 | 1999-06-01 | 길버트 브이 레빈 | 타가토스의제조방법 |
KR19990038067A (ko) * | 1997-11-03 | 1999-06-05 | 조두업 | 순 자연 발효 응유와 과일 또는 채소를 주원료로한 식품 |
US20040132989A1 (en) * | 2000-12-19 | 2004-07-08 | Lifran Estelle V. | Method for purification of lactose |
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See also references of EP3000819A4 |
Also Published As
Publication number | Publication date |
---|---|
UA116100C2 (uk) | 2018-02-12 |
NZ628831A (en) | 2016-08-26 |
CN104321331A (zh) | 2015-01-28 |
US10196415B2 (en) | 2019-02-05 |
AU2013378056A1 (en) | 2014-12-11 |
CN108530495A (zh) | 2018-09-14 |
EP3000819B1 (en) | 2021-09-22 |
US20160152652A1 (en) | 2016-06-02 |
EP3000819A1 (en) | 2016-03-30 |
AU2013378056B2 (en) | 2016-07-07 |
EP3000819A4 (en) | 2017-01-18 |
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