CN106636254A - Process for preparing high-purity xylooligosaccharide - Google Patents
Process for preparing high-purity xylooligosaccharide Download PDFInfo
- Publication number
- CN106636254A CN106636254A CN201611235027.4A CN201611235027A CN106636254A CN 106636254 A CN106636254 A CN 106636254A CN 201611235027 A CN201611235027 A CN 201611235027A CN 106636254 A CN106636254 A CN 106636254A
- Authority
- CN
- China
- Prior art keywords
- xylo
- oligosaccharide
- content
- acid
- production method
- 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.)
- Granted
Links
- HEBKCHPVOIAQTA-NGQZWQHPSA-N d-xylitol Chemical compound OC[C@H](O)C(O)[C@H](O)CO HEBKCHPVOIAQTA-NGQZWQHPSA-N 0.000 title claims abstract description 49
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 23
- 238000000855 fermentation Methods 0.000 claims abstract description 19
- 230000004151 fermentation Effects 0.000 claims abstract description 18
- 238000005516 engineering process Methods 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 9
- 150000002772 monosaccharides Chemical class 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 229920002488 Hemicellulose Polymers 0.000 claims abstract description 5
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Chemical compound OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 30
- 239000007788 liquid Substances 0.000 claims description 20
- 108090000790 Enzymes Proteins 0.000 claims description 17
- 102000004190 Enzymes Human genes 0.000 claims description 17
- 241000222120 Candida <Saccharomycetales> Species 0.000 claims description 15
- 241000222173 Candida parapsilosis Species 0.000 claims description 15
- 229940055022 candida parapsilosis Drugs 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 15
- 241000235060 Scheffersomyces stipitis Species 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 14
- 239000002054 inoculum Substances 0.000 claims description 14
- 239000002609 medium Substances 0.000 claims description 13
- 150000004823 xylans Chemical class 0.000 claims description 13
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 230000000694 effects Effects 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 238000011081 inoculation Methods 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- 238000009835 boiling Methods 0.000 claims description 9
- 238000000746 purification Methods 0.000 claims description 9
- 238000011218 seed culture Methods 0.000 claims description 9
- 229920001221 xylan Polymers 0.000 claims description 9
- 238000010411 cooking Methods 0.000 claims description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- LGQKSQQRKHFMLI-SJYYZXOBSA-N (2s,3r,4s,5r)-2-[(3r,4r,5r,6r)-4,5,6-trihydroxyoxan-3-yl]oxyoxane-3,4,5-triol Chemical compound O[C@@H]1[C@@H](O)[C@H](O)CO[C@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O)OC1 LGQKSQQRKHFMLI-SJYYZXOBSA-N 0.000 claims description 6
- JCSJTDYCNQHPRJ-UHFFFAOYSA-N 20-hydroxyecdysone 2,3-acetonide Natural products OC1C(O)C(O)COC1OC1C(O)C(O)C(OC2C(C(O)C(O)OC2)O)OC1 JCSJTDYCNQHPRJ-UHFFFAOYSA-N 0.000 claims description 6
- LGQKSQQRKHFMLI-UHFFFAOYSA-N 4-O-beta-D-xylopyranosyl-beta-D-xylopyranose Natural products OC1C(O)C(O)COC1OC1C(O)C(O)C(O)OC1 LGQKSQQRKHFMLI-UHFFFAOYSA-N 0.000 claims description 6
- SQNRKWHRVIAKLP-UHFFFAOYSA-N D-xylobiose Natural products O=CC(O)C(O)C(CO)OC1OCC(O)C(O)C1O SQNRKWHRVIAKLP-UHFFFAOYSA-N 0.000 claims description 6
- 108010001682 Dextranase Proteins 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- JCSJTDYCNQHPRJ-FDVJSPBESA-N beta-D-Xylp-(1->4)-beta-D-Xylp-(1->4)-D-Xylp Chemical compound O[C@@H]1[C@@H](O)[C@H](O)CO[C@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O)C(O)OC2)O)OC1 JCSJTDYCNQHPRJ-FDVJSPBESA-N 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 238000007654 immersion Methods 0.000 claims description 6
- ABKNGTPZXRUSOI-UHFFFAOYSA-N xylotriose Natural products OCC(OC1OCC(OC2OCC(O)C(O)C2O)C(O)C1O)C(O)C(O)C=O ABKNGTPZXRUSOI-UHFFFAOYSA-N 0.000 claims description 6
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 5
- 239000001963 growth medium Substances 0.000 claims description 5
- 239000003456 ion exchange resin Substances 0.000 claims description 5
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 238000010564 aerobic fermentation Methods 0.000 claims description 4
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 2
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 2
- 229920000742 Cotton Polymers 0.000 claims description 2
- 244000082204 Phyllostachys viridis Species 0.000 claims description 2
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 2
- JVZHSOSUTPAVII-UHFFFAOYSA-N Xylotetraose Natural products OCC(OC1OCC(OC2OCC(OC3OCC(O)C(O)C3O)C(O)C2O)C(O)C1O)C(O)C(O)C=O JVZHSOSUTPAVII-UHFFFAOYSA-N 0.000 claims description 2
- 230000004913 activation Effects 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 239000011425 bamboo Substances 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 239000004310 lactic acid Substances 0.000 claims description 2
- 235000014655 lactic acid Nutrition 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 240000004928 Paspalum scrobiculatum Species 0.000 claims 1
- 235000003675 Paspalum scrobiculatum Nutrition 0.000 claims 1
- 238000001816 cooling Methods 0.000 claims 1
- 238000007790 scraping Methods 0.000 claims 1
- 206010012601 diabetes mellitus Diseases 0.000 abstract description 4
- 230000006196 deacetylation Effects 0.000 abstract description 2
- 238000003381 deacetylation reaction Methods 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000003344 environmental pollutant Substances 0.000 abstract description 2
- 201000001421 hyperglycemia Diseases 0.000 abstract description 2
- 231100000719 pollutant Toxicity 0.000 abstract description 2
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 abstract 1
- 230000009466 transformation Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 26
- 239000008103 glucose Substances 0.000 description 23
- 229960003487 xylose Drugs 0.000 description 18
- SRBFZHDQGSBBOR-LECHCGJUSA-N alpha-D-xylose Chemical compound O[C@@H]1CO[C@H](O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-LECHCGJUSA-N 0.000 description 15
- 230000001954 sterilising effect Effects 0.000 description 12
- 239000000470 constituent Substances 0.000 description 11
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 description 9
- 239000001888 Peptone Substances 0.000 description 8
- 108010080698 Peptones Proteins 0.000 description 8
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 description 8
- 229940041514 candida albicans extract Drugs 0.000 description 8
- 235000019319 peptone Nutrition 0.000 description 8
- 238000002203 pretreatment Methods 0.000 description 8
- 239000012138 yeast extract Substances 0.000 description 8
- LPQOADBMXVRBNX-UHFFFAOYSA-N ac1ldcw0 Chemical compound Cl.C1CN(C)CCN1C1=C(F)C=C2C(=O)C(C(O)=O)=CN3CCSC1=C32 LPQOADBMXVRBNX-UHFFFAOYSA-N 0.000 description 7
- 125000002777 acetyl group Chemical group [H]C([H])([H])C(*)=O 0.000 description 7
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 description 6
- 238000002835 absorbance Methods 0.000 description 6
- 239000002585 base Substances 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- 230000002255 enzymatic effect Effects 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- PYMYPHUHKUWMLA-WDCZJNDASA-N arabinose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)C=O PYMYPHUHKUWMLA-WDCZJNDASA-N 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 4
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 4
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 4
- 235000011130 ammonium sulphate Nutrition 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 235000013305 food Nutrition 0.000 description 4
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000010792 warming Methods 0.000 description 4
- 229920001817 Agar Polymers 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 3
- 101710121765 Endo-1,4-beta-xylanase Proteins 0.000 description 3
- 239000008272 agar Substances 0.000 description 3
- 230000001580 bacterial effect Effects 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
- 238000001514 detection method Methods 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 235000013406 prebiotics Nutrition 0.000 description 3
- 239000002023 wood Substances 0.000 description 3
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 2
- 229930006000 Sucrose Natural products 0.000 description 2
- 240000008042 Zea mays Species 0.000 description 2
- 235000016383 Zea mays subsp huehuetenangensis Nutrition 0.000 description 2
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 239000013505 freshwater Substances 0.000 description 2
- 150000004676 glycans Chemical class 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 229920005610 lignin Polymers 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- 235000009973 maize Nutrition 0.000 description 2
- 235000012054 meals Nutrition 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920001542 oligosaccharide Polymers 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000007781 pre-processing Methods 0.000 description 2
- MUPFEKGTMRGPLJ-ZQSKZDJDSA-N raffinose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO[C@@H]2[C@@H]([C@@H](O)[C@@H](O)[C@@H](CO)O2)O)O1 MUPFEKGTMRGPLJ-ZQSKZDJDSA-N 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- -1 stalk Substances 0.000 description 2
- 239000005720 sucrose Substances 0.000 description 2
- 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 1
- QWIZNVHXZXRPDR-UHFFFAOYSA-N D-melezitose Natural products O1C(CO)C(O)C(O)C(O)C1OC1C(O)C(CO)OC1(CO)OC1OC(CO)C(O)C(O)C1O QWIZNVHXZXRPDR-UHFFFAOYSA-N 0.000 description 1
- SRBFZHDQGSBBOR-HWQSCIPKSA-N L-arabinopyranose Chemical compound O[C@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-HWQSCIPKSA-N 0.000 description 1
- 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 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 208000008589 Obesity Diseases 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 description 1
- DLRVVLDZNNYCBX-ZZFZYMBESA-N beta-melibiose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@@H]1OC[C@@H]1[C@@H](O)[C@H](O)[C@@H](O)[C@H](O)O1 DLRVVLDZNNYCBX-ZZFZYMBESA-N 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 108010089934 carbohydrase Proteins 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000013375 chromatographic separation Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000009514 concussion Effects 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000001976 enzyme digestion Methods 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 229930182478 glucoside Natural products 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000003345 hyperglycaemic effect Effects 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000010977 jade Substances 0.000 description 1
- 239000008101 lactose Substances 0.000 description 1
- QWIZNVHXZXRPDR-WSCXOGSTSA-N melezitose Chemical compound O([C@@]1(O[C@@H]([C@H]([C@@H]1O[C@@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)O)CO)CO)[C@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O QWIZNVHXZXRPDR-WSCXOGSTSA-N 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000001728 nano-filtration Methods 0.000 description 1
- 235000015816 nutrient absorption Nutrition 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 230000001175 peptic effect Effects 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 150000005846 sugar alcohols Chemical class 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012549 training Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C12P19/04—Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
-
- 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
-
- 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
-
- 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
- C12P2203/00—Fermentation products obtained from optionally pretreated or hydrolyzed cellulosic or lignocellulosic material as the carbon source
Abstract
The invention discloses a process for preparing high-purity xylooligosaccharide. The process comprises the following steps: firstly, removing acetyl and monosaccharide of the side chain in a hemicellulose raw material through deacetylation; performing pretreatment, enzymolysis and fermentation to enable the purity of xylooligosaccharide to be more than or equal to 90 percent. An xylooligosaccharide product prepared by the method has light color and stable pH value. The process can be used for greatly reducing energy consumption, improving product yield and reducing pollutant emission, is more friendly to the environment, can be widely taken by diabetic patients and hyperglycemia patients, and is a novel technology for preparing xylooligosaccharide with high-value transformation.
Description
Technical field
The present invention relates to food processing field, is related to a kind of xylo-oligosaccharide preparation technology, belong to functional sugar alcohol production technology
Field.
Background technology
Xylo-oligosaccharide is one kind of compound sugar, be by β-Isosorbide-5-Nitrae-endo-xylanase with xylan as substrate, hydrolysis β-Isosorbide-5-Nitrae
It is principle active component that the degree of polymerization of glucosides bond formed is the compound sugar of 2-7, wherein xylobiose and xylotriose.Due to xylo-oligosaccharide
Organism (humans and animals) archenteric flora balance can be improved, promote the growth of alimentary canal beneficial bacteria, suppress to be harmful to micro- life
The breeding of thing, promotes nutrient absorption, improves immunity of organisms, and food, health products and field of fodder are widely used at present.No
Only thus, xylo-oligosaccharide sugariness is low, low in calories, it is difficult to entered enteron aisle by peptic digest, substantially do not increase blood pressure and blood lipoid, can be with
Play a role in low-energy food, the requirement that those confectioneries worry the person of getting fat again is met to greatest extent, can also provide
Diabetes patient, adiposis patient and hyperglycemia patient are used.
Xylo-oligosaccharide preparation technology disclosed xylo-oligosaccharide its preparation process 200410023875.X and
200410013840.8, xylo-oligosaccharide content 70%～76% in the two difference enzymolysis liquid, equal Jing NF membranes circulation purification is obtained
Xylo-oligosaccharide content ＞ more than 90%, wherein containing 2%～5% monose, the seven of 1%～5% sugar or seven sugared above macromolecular complex
Matter；Patent 201210136672.6 realized using chromatographic separation technology xylo-oligosaccharide, wood sugar, three kinds of components of arabinose point
From although lower than nanofiltration water consumption and whole energy consumption in whole production process, whole process still needs investment new equipment, so
And xylo-oligosaccharide yield is only 80% in purification process, remainder is separated into Xylose, directly reduces product yield.
The content of the invention
Present invention is that, for the difficult point in existing production technology, novelty provides a kind of system of high-purity oligoxylose
Preparation Method.It is an advantage of the current invention that remove the acetyl group and monose of side chain in hemicellulosic material by deacetylation first,
Then by pretreatment, enzymolysis, fermentation, xylo-oligosaccharide purity is made up to more than 90%, xylo-oligosaccharide component XOS before and after fermentation2-7Contain
Amount is not changed in, at the same the method prepare xylo-oligosaccharide product color is shallow, pH is stable.The present invention can not only be greatly lowered energy
Source consumes, and improves product yield, reduces pollutant emission, more friendly to environment, and product can extensively by patient of diabetes
Person and hyperglycemic patients are edible, are the technologies that a kind of novel green high level conversion prepares xylo-oligosaccharide.
For achieving the above object, the present invention adopts following technical proposals：
A kind of high-purity oligoxylose production method, concrete steps include：
(1) hemicellulosic material is immersed in the aqueous solution of pH8-10, is soaked, then filtered, filtrate is capable of circulation repeatedly
Use；
(2) the hemicellulose residue after filtration is added into acid, adjusts pH to 2～4, then carry out boiling；
(3) material after processing in step (2) adds zytase and dextranase, enzyme activity ratio 20～5:1, wood is poly-
Carbohydrase addition is 5-50IU/g, 40～60 DEG C of enzymolysis 2-10h；
(4) digest after, inoculation pichia stipitis, Torulopsis candida, one or more of Candida parapsilosis, carry out
Aerobic fermentation, total monosaccharide content accounts for total sugar content less than 10%, and heat up the enzyme that goes out；
(5) go out to filter after enzyme and obtain xylo-oligosaccharide enzymolysis liquid, then carry out activated carbon decolorizing and ion exchange resin removal of impurities；
(6) xylo-oligosaccharide liquid glucose after purification is concentrated into concentration for 40%～75% by 5～10% mass concentration；
(7) the xylo-oligosaccharide liquid glucose after concentration is carried out into vacuum belt type drying, obtains high-purity oligoxylose powder.
The high-purity of of the present invention kind of high-purity oligoxylose production method refers to that purity is equal to more than 90%, or
Equal to more than 93%, or equal to more than 96%, or equal to more than 99%, preferably equal to 93.22%, 94.76%,
96.14%th, 97.95%.
In step (1), from for the purity of the xylo-oligosaccharide for obtaining, the hemicellulosic material be corncob, cotton seed hulls,
Straw, stalk, bamboo etc. are rich in hemicellulosic material, preferred corncob.
Present invention employs the weak alkaline aqueous solution of pH8-10 has carried out pre-treatment to raw material, can gather in the wood in raw material
Acetyl group, glucosyl group, aralino on sugar backbone is removed so that product contents of monosaccharides is greatly lowered, and is conducive to carrying
High product glycan proportion.Based on acetyl group, glucosyl group, the Arab that can farthest remove in xylan backbone
Glycosyl, the present invention selects pH for the weak alkaline aqueous solution of 8-10.If alkalescence is too high, the structure of xylan can be destroyed, be reduced low
Xylan yield, if alkalescence is too low, does not have the effect for removing miscellaneous sugar chain, acetyl group and a small amount of lignin and colloid.
The aqueous solution of the pH8-10 can be adjusted using highly basic or weak base, can be liquid base can also be solid
Alkali, wherein it is preferred that NaOH, potassium hydroxide and ammoniacal liquor.
From for pre-treatment effect, the soaking conditionses are：0.5～24h is soaked under the conditions of 10～100 DEG C；Preferably,
The temperature is 50～60 DEG C.
From for immersion effect, it is preferred that the ratio (solid-to-liquid ratio) of hemicellulosic material and the aqueous solution is 1：5～10 (g/mL).
In step (2), the step advantage of this is that using the boiling stage is directly entered after acid adding：Steamed using acid system
Boiling can realize the stripping of hemicellulose and cellulose, hemicellulose with the dissolution of xylan form in the solution.PH is adjusted to 2
～4 the reason for is to realize that xylan degrading accounts for more than 60% for molecular weight more than more than 800 ratios by boiling under the conditions of this, point
Son amount accounts for more than 90% more than more than 250, if pH>2, xylan is further reduced to the product of low-molecular-weight, while monose contains
Amount is raised；If pH>4, xylan dissolution rate is too low.
Preferably, to obtain more preferable cooking effect, acid adding conditions of cooking is：0.4～1.0MPa, 5～120min of boiling.
Acid described in the regulation pH to 2.0～4.0, can be strong acid, or weak acid, preferably hydrochloric acid, sulfuric acid,
Acetic acid, citric acid, lactic acid.
In step (3), the zytase can be middle temperature zytase or high-temperature xylanase, wherein in order that
XOS2-4>65%, preferred fire resistant xylanase.
Zytase addition is 5-50IU/g, refers to that the material after processing in every 1g steps (2) adds 5-50IU active
Zytase.
The present invention obtains suitable zytase and dextranase enzyme addition and its enzymatic activity ratio by screening and optimizing,
The xylobiose containing high level and xylotriose in the product for obtaining are made, prebiotic cultivation effect is obvious.
In step (4), fermentation condition is preferably：30～37 DEG C of 6～90h of aerobic fermentation.
According to the enzymolysis liquid in step (3), the present invention selects inoculation pichia stipitis CICC1960 through screening and optimizing
Or Torulopsis candida CICC31239, one or more of Candida parapsilosis CICC1257.
The feature of pichia stipitis CICC1960 is：Using xylose fermentation for producing alcohol.
The feature of Torulopsis candida CICC31239 is：Any carbohydrate of azymic；Assimilation glucose sugar, maltose, gala
Sugar, sucrose, gossypose, L-arabinose, ethanol.
The feature of Candida parapsilosis CICC1257 is：Glucose fermentation, sucrose, maltose, gossypose, marine alga
Sugar；Azymic galactolipin, lactose, melibiose, melezitose；Wood sugar, sorbierite, glycerine can be assimilated；Arabinose is not assimilated.
Preferably, according to the fermentation character of above-mentioned three kinds of bacterial classifications, select from for the utilizing status of monose, the present invention is preferential
Select the compound addition of three kinds of bacterial classifications, order of addition is pichia stipitis CICC1960, Candida parapsilosis CICC1257, is connect
The amount of kind is 1～3%, and inoculum concentration ratio is 1～2：2～1, add inoculum concentration to be 1～2% Torulopsis candida after 16～24h of fermentation
CICC31239 continues the 18～24h that ferments.
Before fermentation, pichia stipitis, Candida parapsilosis or Torulopsis candida activation method are to scrape a ring respectively oblique
The bacterial classification (first class inoculum) of face culture is transferred in level liquid seed culture medium, and secondary seed inoculum concentration is 2～8% (v/v).
Preferably, first order seed and secondary seed training method are 25～37 DEG C, 50～300rpm/min, 6～36h of concussion and cultivate.
Preferably, first order seed is cultivated 16～24h and is transferred in secondary seed culture in 30 ± 5 DEG C, 100～200rpm/min
In base, 30 ± 5 DEG C, 100～200rpm/min cultivate 18～36h after, according to 2～5% inoculum concentrations (v/v) inoculation enzymolysis liquid in.
Preferably, the slant medium is YPD culture mediums, wherein glucose 1%, dusty yeast 2%, peptone 1%, fine jade
Fat 2%, pH5.0-6.0,121 DEG C sterilizing 15min.
Preferably, in primary-seed medium, 2～10g/L of yeast extract, 5～20g/L of peptone, 2～10g/ of glucose
L, 2～20g/L of wood sugar, pH5.0～7.5,115 DEG C of sterilizing 20min.
Preferably, in secondary seed medium, 0.5～4g/L of yeast extract, 0.2～2g/L of ammonium sulfate, glucose 2～
10g/L, 2～20g/L of wood sugar, pH5.0～7.5,115 DEG C of sterilizing 20min.
The present invention removes monose using fermentation method, and does not utilize xylo-oligosaccharide, product free of losses in purification process.
Preferably, when concentration of glucose is 0.5%, total monosaccharide content accounts for total sugar content less than 10%, and heat up the enzyme that goes out.
Preferably, enzyme condition of going out is：It is warming up to 80～100 DEG C of enzymes that go out.
In step (6), mechanical steam recompression evaporimeter (MVR) is adopted during concentration.
Suitable cycles of concentration is have selected in the step, cycles of concentration is too high to cause color depth, cycles of concentration to be less than
40%, the big rate of drying of mobility is slow, easily produces bubble.
In step (7), using vacuum belt type drying equipment, specific process parameter is：Vacuum be -80～-120KPa, one
Section 95～130 DEG C of heating-up temperature, the time be 15～30min, two sections of 80～110 DEG C of heating-up temperatures, the time be 20～60min, three
Section heating-up temperature is 60～90 DEG C, and the time is 30～120min；Chilling temperature is 20～40 DEG C.
Vacuum belt type drying can reduce material through high temperature using one section, two sections and three sections heating-up temperature of control and time
Caused color and luster is partially deep, while avoiding foaming caused by long-time serious and causing the little difficult problem of density.
The present invention also protects the xylo-oligosaccharide product prepared using said method, and it is powder, wherein, oligomeric wood
The content of sugar is more than 93%, and the content of xylobiose is 38～42%, and the content of xylotriose is 32～38%, in terms of butt.
Further, the content of Xylotetrose is 4～12%, and the content of wooden pentasaccharides is 4～6%, the content of wooden six sugar is 2～
5%, the content of wooden seven sugar is 0～2%.
Xylo-oligosaccharide in the present invention refers to the xylo-oligosaccharide that the degree of polymerization is 2-7.
The purity of xylo-oligosaccharide product obtained using the preparation method of the present invention is high, especially xylobiose and xylotriose
Content is higher；Product color is shallow, pH is stable；Good product mobility, dissolution velocity is fast, and anti-moisture absorption can be good.
The present invention makes xylo-oligosaccharide high purity by the optimal control of the process conditions to each step and parameter
While more than 90%, also cause xylobiose therein and xylotriose content higher, it is ensured that the health-care effect of xylo-oligosaccharide；
The color and luster of the xylo-oligosaccharide product for arriving is shallower, and pH is stable.In addition, using the process step of the invention, energy can be greatly lowered
Source consumes, and industrial mass production is more suitable for, beneficial to popularization and application.
Above-mentioned technical proposal has the advantages that：
(1) the base extraction material using pH8～10 before pretreatment can be by the acetyl in xylan backbone in raw material
Base, glucosyl group, aralino are removed so that product contents of monosaccharides is greatly lowered, and are conducive to improving shared by product glycan
Ratio；A small amount of soluble lignin and pectin can be removed simultaneously, product color is reduced, and reduce ion-exchange purification load.
(2) three big key points, XOS in control prebiotics are digested by pre-treatment, pretreatment coupling2-4Content ＞ 65%, benefit
Raw bacterium cultivation effect is obvious.
(3) monose such as glucose, wood sugar are removed by fermentation process in enzymolysis process, improves xylo-oligosaccharide prebiotic
First content, high income not only reduces equipment investment, reduces production cost, and improves product quality, and diabetes patient can
To use.
(4) by the good product mobility of belt drying, dissolution velocity is fast, and because contents of monosaccharides is low, anti-moisture absorption can be good,
In can be widely applied to food and health products.
Specific embodiment
With reference to embodiment, the present invention is further described.
Embodiment 1
Maize cob meal is broken into 20 mesh or so, according to 1:10 solid-to-liquid ratios are sized mixing, and lead to NH3To 50 DEG C of immersion 24h of pH9.0, pipe
Road filter screen draining, filtrate is used to soak next batch materials, adds phosphorus acid for adjusting pH to after 3.5, and direct feeding enters transverse tube even steam
Device, after 0.55MPa boiling 90min, release is spurted into enzymatic vessel.Treat that temperature is reduced to 60～65 DEG C of addition xylans after spurting
Enzyme, dextranase compound, enzyme activity ratio 20～5:1, zytase addition is 5IU/g, is reduced after 40～60 DEG C of enzymolysis 4h
Temperature to 37 DEG C, inoculation pichia stipitis CICC1960 fermentation 36h, when concentration of glucose is less than 0.5%, be warming up to 80～
100 DEG C of enzymes that go out.Conventionally include activated carbon decolorizing and ion exchange resin removal of impurities, will after purification xylo-oligosaccharide liquid glucose by
5～10% concentration is concentrated into 50% using MVR concentrators, into vacuum belt type drying.
Vacuum belt concentration parameter be vacuum be -80KPa, one section of 95 DEG C of heating-up temperature, the time is 15min；Two sections add
110 DEG C of hot temperature, the time is 20min；Three sections of heating-up temperatures are 60 DEG C, and the time is 30min；Chilling temperature is 25 DEG C.
Seed culture method：The pichia stipitis CICC1960 strain transfers of a ring YPD inclined-plane cultures are scraped in one-level liquid
In body seed culture medium, secondary seed inoculum concentration is 6%, and the inoculum concentration being inoculated in enzymatic vessel is 3%.
Above-mentioned slant medium is YPD culture mediums, wherein glucose 1%, dusty yeast 2%, peptone 1%, agar 2%,
PH5.0-6.0,121 DEG C of sterilizing 15min.
In primary-seed medium, yeast extract 10g/L, peptone 20g/L, glucose 10g/L, wood sugar 10g/L,
PH5.0～7.5,115 DEG C of sterilizing 20min.
Secondary seed medium each component content, yeast extract 2g/L, ammonium sulfate 2g/L, glucose 10g/L, wood sugar 10g/
L, pH5.0～7.5,115 DEG C of sterilizing 20min.
It is as described in Table 1 using pretreatment steaming boil liquid component after pre-treatment.
Table 1:Constituent content table in cooking liquor in embodiment 1
Xylo-oligosaccharide constituent content is determined using KS802 posts as described in Table 2.
Table 2:Xylo-oligosaccharide constituent content table in embodiment 1
| Project | XOS2-7 | X7 | X6 | X5 | X4 | X3 | X2 | Glucose G | Wood sugar X | Arabinose A |
| Each sugared content (%) | 96.14 | 1.73 | 2.04 | 4.43 | 16.33 | 32.61 | 39.00 | 0.41 | 2.16 | 1.29 |
The absorbance detection of 5cm cuvettes, XOS finished products is diluted under 37.5%, 420nm and detects that absorbance is 0.017.
Embodiment 2
After taking corncob crushing, with the sodium hydroxide solution that mass concentration is 0.05% by 1:7 mass ratio mix to
PH10, is warming up to 60 degrees Celsius of insulation 30min, filters liquid；One time is washed to pH value neutrality；1 is pressed with fresh water (FW):3 quality
Than mixing, the acetic acid of corncob dry weight percentage 0.7%, Steam explosion treatment, processing pressure 1.5MPa, time 120s are added；
Xylose Content in steam explosion liquid is 5.85%, treats that temperature is reduced to 60～65 DEG C and adds zytase, dextranase compound, enzyme
Ratio 20～5 living:1, zytase dosage zytase 8IU/g, temperature is reduced to 37 DEG C after 40～60 DEG C of enzymolysis 4h, and inoculation is white
Torulopsis (CICC31239) or Candida parapsilosis CICC31239 fermentation 72h, when concentration of glucose≤0.5%, rise
Temperature is to 80～100 DEG C of enzymes that go out.0.8g Xylanase Compositions are added to cooking liquor, enzyme digestion reaction temperature is 60 DEG C, enzymolysis time
For 8h, include activated carbon decolorizing and ion exchange resin removal of impurities according to conventional, by xylo-oligosaccharide liquid glucose after purification by 5～10%
Concentration is concentrated into 50% using MVR concentrators, into vacuum belt type drying.
Vacuum belt concentration parameter be vacuum be -100KPa, one section of 130 DEG C of heating-up temperature, the time is 20min；Two sections
95 DEG C of heating-up temperature, the time is 30min；Three sections of heating-up temperatures are 80 DEG C, and the time is 60min；Chilling temperature is 40 DEG C.
Seed culture method：Scrape the Torulopsis candida (CICC31239) or Candida parapsilosis of a ring YPD inclined-plane cultures
CICC31239 transfers in level liquid seed culture medium, and secondary seed inoculum concentration is 5%, the inoculation being inoculated in enzymatic vessel
Measure as 4%.
Above-mentioned slant medium is YPD culture mediums, wherein glucose 1%, dusty yeast 2%, peptone 1%, agar 2%,
PH5.0-6.0,121 DEG C of sterilizing 15min.
In primary-seed medium, yeast extract 10g/L, peptone 20g/L, glucose 10g/L, wood sugar 15g/L,
PH5.0～7.5,115 DEG C of sterilizing 20min.
Secondary seed medium each component content, yeast extract 3g/L, ammonium sulfate 2g/L, glucose 10g/L, wood sugar 15g/
L, pH5.0～7.5,115 DEG C of sterilizing 20min.
Table 3:Torulopsis candida CICC31239 xylo-oligosaccharides constituent content table in embodiment 2
| Project | XOS2-7 | X7 | X6 | X5 | X4 | X3 | X2 | G | X | A |
| Each sugared content (%) | 93.22 | 0 | 4.37 | 5.04 | 11.68 | 32.6 | 39.53 | 0.05 | 6.13 | 0.6 |
The absorbance detection of 5cm cuvettes, by XOS be dissolved into finished product be diluted under 37.5%, 420nm detect absorbance be
0.033。
Table 4:Candida parapsilosis CICC31239 xylo-oligosaccharides constituent content table in embodiment 2
| Project | XOS2-7 | X7 | X6 | X5 | X4 | X3 | X2 | G | X | A |
| Each sugared content (%) | 94.76 | 0.13 | 2.37 | 4.55 | 11.58 | 35.6 | 40.53 | 0.12 | 3.32 | 1.8 |
The absorbance detection of 5cm cuvettes, XOS finished products is diluted under 37.5%, 420nm and detects that absorbance is 0.021.
Embodiment 3
Maize cob meal is broken into 20 mesh or so, according to 1:10 solid-to-liquid ratios are sized mixing, and lead to NH3To 50 DEG C of immersion 24h of pH9.0, pipe
Road filter screen draining, filtrate is used to soak next batch materials, adds phosphorus acid for adjusting pH to after 3.5, and direct feeding enters transverse tube even steam
Device, after 0.55MPa boiling 90min, release is spurted into enzymatic vessel.Treat that temperature is reduced to 60～65 DEG C of addition xylans after spurting
Enzyme, dextranase compound, enzyme activity ratio 20～5:1, zytase addition is 5IU/g, is reduced after 40～60 DEG C of enzymolysis 4h
Temperature is inoculated with pichia stipitis CICC1960 and Candida parapsilosis CICC1257 to 37 DEG C, and inoculum concentration is respectively 1% (v/
V), the Torulopsis candida CICC31239 fermentation 20h of 1% (v/v) are inoculated with after fermentation 16h, when concentration of glucose is less than 0.5%,
It is warming up to 80～100 DEG C of enzymes that go out.Conventionally include activated carbon decolorizing and ion exchange resin removal of impurities, will be oligomeric after purification
Wood sugar liquid glucose is concentrated into 50% by 5～10% concentration using MVR concentrators, into vacuum belt type drying.
Vacuum belt concentration parameter be vacuum be -80KPa, one section of 95 DEG C of heating-up temperature, two sections of 120 DEG C of heating-up temperatures,
Three sections of heating-up temperatures are 60 DEG C, and chilling temperature is 25 DEG C；Scraper plate be concentrated by evaporation parameter be temperature control at 120 DEG C, evaporating pressure
For -0.08MPa, at 105 DEG C, in 3m/s, chilling temperature is 25 DEG C to the control of scraper plate rotating speed for drop temperature control.
Seed culture method：Pichia stipitis CICC1960, the Torulopsis candida of a ring YPD inclined-plane cultures are scraped respectively
In level liquid seed culture medium, secondary seed is inoculated with for CICC31239 and Candida parapsilosis CICC1257 strain transfers
Measure as 6%.It is 3% to be inoculated in inoculum concentration total in enzymatic vessel, pichia stipitis CICC1960, Candida parapsilosis
The inoculum concentration of CICC1257 and Torulopsis candida CICC31239 is respectively 1%.
Above-mentioned slant medium is YPD culture mediums, wherein glucose 1%, dusty yeast 2%, peptone 1%, agar 2%,
PH5.0-6.0,121 DEG C of sterilizing 15min.
In primary-seed medium, yeast extract 10g/L, peptone 20g/L, glucose 10g/L, wood sugar 10g/L,
PH5.0～7.5,115 DEG C of sterilizing 20min.
Secondary seed medium each component content, yeast extract 2g/L, ammonium sulfate 2g/L, glucose 10g/L, wood sugar 10g/
L, pH5.0～7.5,115 DEG C of sterilizing 20min.
Xylo-oligosaccharide constituent content is determined using KS802 posts as described in Table 5.
Table 5:Xylo-oligosaccharide constituent content table in embodiment 3
| Project | XOS2-7 | X7 | X6 | X5 | X4 | X3 | X2 | Glucose G | Wood sugar X | Arabinose A |
| Each sugared content (%) | 97.95 | 0.13 | 2.40 | 4.70 | 12.00 | 36.81 | 41.91 | 0.03 | 1.71 | 0.31 |
Tests prove that, fermented using composite bacteria, the effect for removing monose is more preferable so that xylo-oligosaccharide product
Purity is higher.
Comparative example 1
It is with the difference in embodiment 1：Logical NH3To 50 DEG C of immersion 24h of pH11, other process conditions and method and enforcement
Example 1 is identical.
Xylo-oligosaccharide constituent content is determined using KS802 posts as described in Table 6.
Table 6:Cooking liquor constituent content table after pre-processing in comparative example 1
It can be seen that, the impurities affect of xylo-oligosaccharide products of the pH of the aqueous solution to finally giving is larger in pre-treatment, in order to more
The good acetyl group, glucosyl group, the aralino that reduce in raw material in xylan backbone, it is proposed that the pH of the aqueous solution in pre-treatment
Adjust to 8～10.
Comparative example 2
It is with the difference in embodiment 1：Logical NH3To 50 DEG C of immersion 24h of pH7.5, other process conditions and method and enforcement
Example 1 is identical.
Xylo-oligosaccharide constituent content is determined using KS802 posts as described in Table 7.
Table 7:Cooking liquor constituent content table after pre-processing in comparative example 1
| Project | X>7 | X7 | X6 | X5 | X4 | X3 | X2 | Glucose G | Wood sugar X | Arabinose A |
| Each sugared content (%) | 48.92 | 4.59 | 5.14 | 5.2 | 6.41 | 6.44 | 6.87 | 7.3 | 5.87 | 3.26 |
It can be seen that, the pH of the aqueous solution is too high or too low in pre-treatment affects big to contents of monosaccharides in cooking liquor, to finally giving
Xylo-oligosaccharide product impurities affect it is larger, in order to preferably reduce acetyl group, glucose in raw material in xylan backbone
Base, aralino, it is proposed that the pH of the aqueous solution is adjusted to 8～10 in pre-treatment.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention not by above-described embodiment
Limit, other any Spirit Essences without departing from the present invention and the change, modification, replacement made under principle, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of high-purity oligoxylose production method, is characterized in that, step is as follows：
（1）Hemicellulosic material is immersed in the aqueous solution of pH8-10, under the conditions of 10-100 DEG C, then immersion filters, and filters
Liquid Reusability capable of circulation；
（2）Hemicellulose residue after filtration is added into acid, pH to 3.0 ~ 3.5 is adjusted, boiling is then carried out；
（3）To step（2）Material after middle process adds zytase and dextranase, enzyme activity ratio 20 ~ 5:1, zytase
Addition is 5-50IU/g, 40 ~ 60 DEG C of enzymolysis 2-10h；
（4）After enzymolysis, inoculation pichia stipitis, Torulopsis candida, one or more of Candida parapsilosis, carry out aerobic
Fermentation, treats that total monosaccharide content accounts for total sugar content less than 10%, and heat up the enzyme that goes out；
（5）Go out to filter after enzyme and obtain xylo-oligosaccharide enzymolysis liquid, then carry out activated carbon decolorizing and ion exchange resin removal of impurities；
（6）Xylo-oligosaccharide liquid glucose after purification is concentrated into 40 ~ 75% by 5 ~ 10% mass concentration；
（7）Xylo-oligosaccharide liquid glucose after concentration is carried out into vacuum belt type drying, high-purity oligoxylose powder is obtained.
2. production method as claimed in claim 1, is characterized in that：Step（1）In, the raw material is corncob, cotton seed hulls, rice
Grass, stalk, bamboo are rich in hemicellulosic material, preferred corncob；
The ratio of hemicellulosic material and the aqueous solution is 1：5~10（g/mL）；
The soaking conditionses are：0.5 ~ 24h is soaked under the conditions of 10 ~ 100 DEG C；Preferably, temperature is 50 ~ 60 DEG C；
The aqueous solution of the pH8-10 is adjusted using highly basic or weak base, including liquid base and solid base, preferably hydroxide
Sodium, potassium hydroxide and ammoniacal liquor.
3. production method as claimed in claim 1, is characterized in that：Step（2）In, described in the regulation pH to 3.0 ~ 3.5
Acid, including strong acid and weak acid, preferably hydrochloric acid, sulfuric acid, acetic acid, citric acid, lactic acid；
Acid adding conditions of cooking is：0.4 ~ 1.0MPa, 5 ~ 120min of boiling.
4. production method as claimed in claim 1, is characterized in that：Step（3）In, inoculation pichia stipitis CICC1960 or
One or more of Torulopsis candida CICC31239, Candida parapsilosis CICC1257；
Fermentation condition is：30 ~ 37 DEG C of 6 ~ 90h of aerobic fermentation；
Preferably, during fermentation, order of addition is pichia stipitis CICC1960 and Candida parapsilosis CICC1257, is inoculated with
Measure as 1 ~ 3%, inoculum concentration ratio is 1 ~ 2：2 ~ 1, add inoculum concentration to be 1 ~ 2% Torulopsis candida CICC31239 after 16 ~ 24h of fermentation
Continue the 18 ~ 24h that ferments.
5. production method as claimed in claim 4, is characterized in that：Before fermentation, pichia stipitis, Candida parapsilosis or
Torulopsis candida activation method be the strain transfer for scraping a ring inclined-plane culture in level liquid seed culture medium, secondary seed
Inoculum concentration is 2 ~ 8%.
6. production method as claimed in claim 5, is characterized in that：First order seed is cultivated in 30 ± 5 DEG C, 100 ~ 200rpm/min
16 ~ 24h transfers in secondary seed medium, 30 ± 5 DEG C, 100 ~ 200rpm/min cultivate 18 ~ 36h after, according to 2 ~ 5% inoculation
In amount inoculation enzymolysis liquid.
7. production method as claimed in claim 1, is characterized in that：Step（6）In, mechanical steam recompression is adopted during concentration
Evaporimeter.
8. production method as claimed in claim 1, is characterized in that：Step（7）In, dense employing vacuum belt type drying equipment, tool
Body technology parameter is：Vacuum is -80～-120KPa, and one section of 95～130 DEG C of heating-up temperature, the time is 15 ~ 30min, and two sections add
80～110 DEG C of hot temperature, the time is 20 ~ 60min, and three sections of heating-up temperatures are 60～90 DEG C, and the time is 30 ~ 120min；Cooling temperature
Spend for 20～40 DEG C.
9. the xylo-oligosaccharide product for being prepared using the method any one of claim 1 ~ 8, is characterized in that：It is described low
Xylan product is powder, wherein, the content of xylo-oligosaccharide is more than 93%, and the content of xylobiose is 38 ~ 42%, xylotriose
Content is 32 ~ 38%, in terms of butt.
10. xylo-oligosaccharide product as claimed in claim 9, is characterized in that：The content of Xylotetrose is 4 ~ 12%, and wooden pentasaccharides contains
Measure as 4 ~ 6%, the content of wooden six sugar is 2 ~ 5%, the content of wooden seven sugar is 0 ~ 2%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611235027.4A CN106636254B (en) | 2016-12-28 | 2016-12-28 | Preparation process of high-purity xylo-oligosaccharide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611235027.4A CN106636254B (en) | 2016-12-28 | 2016-12-28 | Preparation process of high-purity xylo-oligosaccharide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106636254A true CN106636254A (en) | 2017-05-10 |
| CN106636254B CN106636254B (en) | 2024-03-08 |
Family
ID=58832193
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611235027.4A Active CN106636254B (en) | 2016-12-28 | 2016-12-28 | Preparation process of high-purity xylo-oligosaccharide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106636254B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107912758A (en) * | 2017-12-08 | 2018-04-17 | 厦门大学 | A kind of preparation method for the composite functional Xylo-oligosaccharide composition for promoting dry anti-moisture absorption |
| CN111148749A (en) * | 2016-08-31 | 2020-05-12 | 王子控股株式会社 | Production method of acidic xylo-oligosaccharide and acidic xylo-oligosaccharide |
| CN111493306A (en) * | 2020-06-05 | 2020-08-07 | 山东肥城精制盐厂有限公司 | Xylo-oligosaccharide edible salt capable of effectively improving moisture resistance |
| CN114250257A (en) * | 2021-12-22 | 2022-03-29 | 山东君恒营养技术研究有限公司 | Preparation of oligosaccharide and high-value clean utilization method of non-grain biomass resources |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101434977A (en) * | 2008-12-23 | 2009-05-20 | 中国石油化工股份有限公司 | Novel method for saccharification of ligno-cellulose |
| CN102061323A (en) * | 2010-11-10 | 2011-05-18 | 山东龙力生物科技股份有限公司 | Comprehensive utilization process of wood cellulose |
| CN102660606A (en) * | 2012-05-04 | 2012-09-12 | 山东龙力生物科技股份有限公司 | Bio-preparation method for production of high-purity xylo-oligosaccharide and coproduction of arabinose and xylose |
| CN103333932A (en) * | 2012-12-29 | 2013-10-02 | 青岛蔚蓝生物集团有限公司 | A method for preparing xylooligosaccharide |
| CN104593446A (en) * | 2014-12-25 | 2015-05-06 | 山东龙力生物科技股份有限公司 | Preparation method of pure xylooligosaccharide powder |
| CN105255965A (en) * | 2015-10-14 | 2016-01-20 | 山东龙力生物科技股份有限公司 | Method for preparing high-purity xylo-oligosaccarides by taking cottonseed hulls as raw materials |
-
2016
- 2016-12-28 CN CN201611235027.4A patent/CN106636254B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101434977A (en) * | 2008-12-23 | 2009-05-20 | 中国石油化工股份有限公司 | Novel method for saccharification of ligno-cellulose |
| CN102061323A (en) * | 2010-11-10 | 2011-05-18 | 山东龙力生物科技股份有限公司 | Comprehensive utilization process of wood cellulose |
| CN102660606A (en) * | 2012-05-04 | 2012-09-12 | 山东龙力生物科技股份有限公司 | Bio-preparation method for production of high-purity xylo-oligosaccharide and coproduction of arabinose and xylose |
| CN103333932A (en) * | 2012-12-29 | 2013-10-02 | 青岛蔚蓝生物集团有限公司 | A method for preparing xylooligosaccharide |
| CN104593446A (en) * | 2014-12-25 | 2015-05-06 | 山东龙力生物科技股份有限公司 | Preparation method of pure xylooligosaccharide powder |
| CN105255965A (en) * | 2015-10-14 | 2016-01-20 | 山东龙力生物科技股份有限公司 | Method for preparing high-purity xylo-oligosaccarides by taking cottonseed hulls as raw materials |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111148749A (en) * | 2016-08-31 | 2020-05-12 | 王子控股株式会社 | Production method of acidic xylo-oligosaccharide and acidic xylo-oligosaccharide |
| CN107912758A (en) * | 2017-12-08 | 2018-04-17 | 厦门大学 | A kind of preparation method for the composite functional Xylo-oligosaccharide composition for promoting dry anti-moisture absorption |
| CN111493306A (en) * | 2020-06-05 | 2020-08-07 | 山东肥城精制盐厂有限公司 | Xylo-oligosaccharide edible salt capable of effectively improving moisture resistance |
| CN114250257A (en) * | 2021-12-22 | 2022-03-29 | 山东君恒营养技术研究有限公司 | Preparation of oligosaccharide and high-value clean utilization method of non-grain biomass resources |
| CN114250257B (en) * | 2021-12-22 | 2023-09-12 | 山东君恒营养技术研究有限公司 | Preparation of oligosaccharide and non-grain biomass resource high-value clean utilization method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106636254B (en) | 2024-03-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP4675139B2 (en) | High purity xylooligosaccharide composition | |
| JP5633839B2 (en) | Method for converting lignocellulosic biomass | |
| CN106636256B (en) | Xylo-oligosaccharide with low polymerization degree and preparation method and application thereof | |
| CN103005147B (en) | Biological feed based on vinasse | |
| CN101643795B (en) | Method for preparing xylose and xylitol by using bamboo | |
| CN106636254A (en) | Process for preparing high-purity xylooligosaccharide | |
| CN102517403B (en) | Method for preparing hemicellulose oligosaccharide by high-temperature liquid water | |
| KR102117175B1 (en) | Soluble dietary fiber and method for its preparation | |
| CN106387923A (en) | Soluble dietary fibers rich in galactomannan and preparation method of soluble dietary fibers | |
| CN101914589A (en) | New method for producing low polyxylose by utilizing microorganism | |
| CN1186461C (en) | Prepn of oligoxylose | |
| CN109576324A (en) | A kind of astragalus polyose and its biological extraction method | |
| JP4078778B2 (en) | Xylooligosaccharide composition | |
| CN101624584A (en) | Preparation method of internal cutting type xylanase | |
| CN106755193B (en) | Method for producing xylo-oligosaccharide by using viscose fiber squeezed liquid as raw material | |
| CN101565468B (en) | Method for producing xylo-oligosaccharide by utilizing cotton seed hulls | |
| Wu et al. | L-Arabinose and oligosaccharides production from sugar beet pulp by xylanase and acid hydrolysis | |
| CN107384733A (en) | A kind of method that spontaneous fermentation prepares sugarcane vinegar | |
| CN105166673B (en) | A kind of production method of the processing method and rice bran rice cake of rice bran | |
| CN109105738A (en) | A kind of method of enzymatic conversion glutinous rice preparation Pengxi ginger cake | |
| CN1274702C (en) | Process for preparing xylo-oligosaccharide through high temperature degradation of xylan | |
| CN110964706A (en) | Preparation method of cellulase, xylanase and pectinase | |
| CN109567202A (en) | A kind of extracting method of barley green | |
| CN111349668A (en) | Method for producing high-quality reducing sugar by using straws as raw materials | |
| CN104855777A (en) | Method for preparing flavor Natta sugar with astringent persimmons |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |