CN113397169A - Method for continuously extracting and separating multiple natural active ingredients from mulberries - Google Patents
Method for continuously extracting and separating multiple natural active ingredients from mulberries Download PDFInfo
- Publication number
- CN113397169A CN113397169A CN202110732680.6A CN202110732680A CN113397169A CN 113397169 A CN113397169 A CN 113397169A CN 202110732680 A CN202110732680 A CN 202110732680A CN 113397169 A CN113397169 A CN 113397169A
- Authority
- CN
- China
- Prior art keywords
- mulberry
- exchange resin
- resin column
- column
- cation exchange
- 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.)
- Pending
Links
- 235000008708 Morus alba Nutrition 0.000 title claims abstract description 150
- 238000000034 method Methods 0.000 title claims abstract description 41
- 239000004480 active ingredient Substances 0.000 title claims abstract description 27
- 241000218231 Moraceae Species 0.000 title claims abstract description 14
- 240000000249 Morus alba Species 0.000 claims abstract description 136
- 239000011347 resin Substances 0.000 claims abstract description 82
- 229920005989 resin Polymers 0.000 claims abstract description 82
- 235000010208 anthocyanin Nutrition 0.000 claims abstract description 76
- 229930002877 anthocyanin Natural products 0.000 claims abstract description 76
- 239000004410 anthocyanin Substances 0.000 claims abstract description 76
- 150000004636 anthocyanins Chemical class 0.000 claims abstract description 76
- 238000001179 sorption measurement Methods 0.000 claims abstract description 74
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 73
- 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 abstract description 49
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000003729 cation exchange resin Substances 0.000 claims abstract description 48
- 239000003957 anion exchange resin Substances 0.000 claims abstract description 43
- 150000008442 polyphenolic compounds Chemical class 0.000 claims abstract description 42
- 235000013824 polyphenols Nutrition 0.000 claims abstract description 42
- 150000001413 amino acids Chemical class 0.000 claims abstract description 41
- 239000002994 raw material Substances 0.000 claims abstract description 36
- 238000002386 leaching Methods 0.000 claims abstract description 30
- 238000000926 separation method Methods 0.000 claims abstract description 21
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 19
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 19
- 238000011033 desalting Methods 0.000 claims abstract description 8
- 239000000047 product Substances 0.000 claims description 42
- 238000010828 elution Methods 0.000 claims description 23
- 239000003480 eluent Substances 0.000 claims description 22
- 239000007788 liquid Substances 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 15
- 230000002378 acidificating effect Effects 0.000 claims description 13
- 238000000605 extraction Methods 0.000 claims description 13
- 239000000706 filtrate Substances 0.000 claims description 13
- 238000001914 filtration Methods 0.000 claims description 13
- 239000003223 protective agent Substances 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 8
- 235000000346 sugar Nutrition 0.000 claims description 8
- 238000005119 centrifugation Methods 0.000 claims description 7
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 5
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 5
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 4
- 235000021581 juice product Nutrition 0.000 claims description 4
- 238000004062 sedimentation Methods 0.000 claims description 4
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical group OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 3
- LVGQIQHJMRUCRM-UHFFFAOYSA-L calcium bisulfite Chemical compound [Ca+2].OS([O-])=O.OS([O-])=O LVGQIQHJMRUCRM-UHFFFAOYSA-L 0.000 claims description 3
- 235000010260 calcium hydrogen sulphite Nutrition 0.000 claims description 3
- DJEHXEMURTVAOE-UHFFFAOYSA-M potassium bisulfite Chemical compound [K+].OS([O-])=O DJEHXEMURTVAOE-UHFFFAOYSA-M 0.000 claims description 3
- 229940099427 potassium bisulfite Drugs 0.000 claims description 3
- 235000010259 potassium hydrogen sulphite Nutrition 0.000 claims description 3
- AOSFMYBATFLTAQ-UHFFFAOYSA-N 1-amino-3-(benzimidazol-1-yl)propan-2-ol Chemical compound C1=CC=C2N(CC(O)CN)C=NC2=C1 AOSFMYBATFLTAQ-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000009776 industrial production Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 229940024606 amino acid Drugs 0.000 description 38
- 239000000243 solution Substances 0.000 description 9
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 7
- 239000002699 waste material Substances 0.000 description 7
- OHZCFWMJMWFNFP-ZVGUSBNCSA-L (2r,3r)-2,3-dihydroxybutanedioate;iron(2+) Chemical compound [Fe+2].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O OHZCFWMJMWFNFP-ZVGUSBNCSA-L 0.000 description 6
- 238000004737 colorimetric analysis Methods 0.000 description 6
- 238000011161 development Methods 0.000 description 6
- 238000010812 external standard method Methods 0.000 description 6
- 229940057006 ferrous tartrate Drugs 0.000 description 6
- 238000004128 high performance liquid chromatography Methods 0.000 description 6
- FEMOMIGRRWSMCU-UHFFFAOYSA-N ninhydrin Chemical compound C1=CC=C2C(=O)C(O)(O)C(=O)C2=C1 FEMOMIGRRWSMCU-UHFFFAOYSA-N 0.000 description 6
- 238000001694 spray drying Methods 0.000 description 6
- 239000003463 adsorbent Substances 0.000 description 4
- 229930014669 anthocyanidin Natural products 0.000 description 4
- 150000001452 anthocyanidin derivatives Chemical class 0.000 description 4
- 235000008758 anthocyanidins Nutrition 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 235000013399 edible fruits Nutrition 0.000 description 4
- 238000011068 loading method Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000011782 vitamin Substances 0.000 description 4
- 229930003231 vitamin Natural products 0.000 description 4
- 235000013343 vitamin Nutrition 0.000 description 4
- 229940088594 vitamin Drugs 0.000 description 4
- YQUVCSBJEUQKSH-UHFFFAOYSA-N 3,4-dihydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C(O)=C1 YQUVCSBJEUQKSH-UHFFFAOYSA-N 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 229930091371 Fructose Natural products 0.000 description 3
- 239000005715 Fructose Substances 0.000 description 3
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 description 3
- 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 3
- 229930006000 Sucrose Natural products 0.000 description 3
- 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 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000002253 acid Substances 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
- 238000005189 flocculation Methods 0.000 description 3
- 239000008103 glucose Substances 0.000 description 3
- 150000004676 glycans Chemical class 0.000 description 3
- 229920001282 polysaccharide Polymers 0.000 description 3
- 239000005017 polysaccharide Substances 0.000 description 3
- 239000005720 sucrose Substances 0.000 description 3
- RKWHWFONKJEUEF-GQUPQBGVSA-O Cyanidin 3-O-glucoside Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC2=C(O)C=C(O)C=C2[O+]=C1C1=CC=C(O)C(O)=C1 RKWHWFONKJEUEF-GQUPQBGVSA-O 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 2
- YTMNONATNXDQJF-UBNZBFALSA-N chrysanthemin Chemical compound [Cl-].O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC2=C(O)C=C(O)C=C2[O+]=C1C1=CC=C(O)C(O)=C1 YTMNONATNXDQJF-UBNZBFALSA-N 0.000 description 2
- 235000009508 confectionery Nutrition 0.000 description 2
- USNPULRDBDVJAO-FXCAAIILSA-N cyanidin 3-O-rutinoside betaine Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1OC[C@@H]1[C@@H](O)[C@H](O)[C@@H](O)[C@H](OC=2C(=[O+]C3=CC(O)=CC([O-])=C3C=2)C=2C=C(O)C(O)=CC=2)O1 USNPULRDBDVJAO-FXCAAIILSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 2
- 229960001331 keracyanin Drugs 0.000 description 2
- ABVCUBUIXWJYSE-GQUPQBGVSA-O pelargonidin 3-O-beta-D-glucoside Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC2=C(O)C=C(O)C=C2[O+]=C1C1=CC=C(O)C=C1 ABVCUBUIXWJYSE-GQUPQBGVSA-O 0.000 description 2
- IFYOHQQBIKDHFT-ASZXTAQUSA-N pelargonidin 3-O-rutinoside betaine Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1OC[C@@H]1[C@@H](O)[C@H](O)[C@@H](O)[C@H](OC=2C(=[O+]C3=CC(O)=CC([O-])=C3C=2)C=2C=CC(O)=CC=2)O1 IFYOHQQBIKDHFT-ASZXTAQUSA-N 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- JMSVCTWVEWCHDZ-UHFFFAOYSA-N syringic acid Chemical compound COC1=CC(C(O)=O)=CC(OC)=C1O JMSVCTWVEWCHDZ-UHFFFAOYSA-N 0.000 description 2
- QAIPRVGONGVQAS-DUXPYHPUSA-N trans-caffeic acid Chemical compound OC(=O)\C=C\C1=CC=C(O)C(O)=C1 QAIPRVGONGVQAS-DUXPYHPUSA-N 0.000 description 2
- ACEAELOMUCBPJP-UHFFFAOYSA-N (E)-3,4,5-trihydroxycinnamic acid Natural products OC(=O)C=CC1=CC(O)=C(O)C(O)=C1 ACEAELOMUCBPJP-UHFFFAOYSA-N 0.000 description 1
- KSEBMYQBYZTDHS-HWKANZROSA-M (E)-Ferulic acid Natural products COC1=CC(\C=C\C([O-])=O)=CC=C1O KSEBMYQBYZTDHS-HWKANZROSA-M 0.000 description 1
- WBYWAXJHAXSJNI-VOTSOKGWSA-M .beta-Phenylacrylic acid Natural products [O-]C(=O)\C=C\C1=CC=CC=C1 WBYWAXJHAXSJNI-VOTSOKGWSA-M 0.000 description 1
- 206010003210 Arteriosclerosis Diseases 0.000 description 1
- 241000255789 Bombyx mori Species 0.000 description 1
- 108010059892 Cellulase Proteins 0.000 description 1
- WBYWAXJHAXSJNI-SREVYHEPSA-N Cinnamic acid Chemical compound OC(=O)\C=C/C1=CC=CC=C1 WBYWAXJHAXSJNI-SREVYHEPSA-N 0.000 description 1
- 241000371652 Curvularia clavata Species 0.000 description 1
- 240000000950 Hippophae rhamnoides Species 0.000 description 1
- 235000003145 Hippophae rhamnoides Nutrition 0.000 description 1
- AGPKZVBTJJNPAG-WHFBIAKZSA-N L-isoleucine Chemical compound CC[C@H](C)[C@H](N)C(O)=O AGPKZVBTJJNPAG-WHFBIAKZSA-N 0.000 description 1
- KDXKERNSBIXSRK-YFKPBYRVSA-N L-lysine Chemical compound NCCCC[C@H](N)C(O)=O KDXKERNSBIXSRK-YFKPBYRVSA-N 0.000 description 1
- FFEARJCKVFRZRR-BYPYZUCNSA-N L-methionine Chemical compound CSCC[C@H](N)C(O)=O FFEARJCKVFRZRR-BYPYZUCNSA-N 0.000 description 1
- AYFVYJQAPQTCCC-GBXIJSLDSA-N L-threonine Chemical compound C[C@@H](O)[C@H](N)C(O)=O AYFVYJQAPQTCCC-GBXIJSLDSA-N 0.000 description 1
- QIVBCDIJIAJPQS-VIFPVBQESA-N L-tryptophane Chemical compound C1=CC=C2C(C[C@H](N)C(O)=O)=CNC2=C1 QIVBCDIJIAJPQS-VIFPVBQESA-N 0.000 description 1
- KZSNJWFQEVHDMF-BYPYZUCNSA-N L-valine Chemical compound CC(C)[C@H](N)C(O)=O KZSNJWFQEVHDMF-BYPYZUCNSA-N 0.000 description 1
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 description 1
- 239000004472 Lysine Substances 0.000 description 1
- 235000016357 Mirtillo rosso Nutrition 0.000 description 1
- 240000008790 Musa x paradisiaca Species 0.000 description 1
- 108010059820 Polygalacturonase Proteins 0.000 description 1
- 241000220324 Pyrus Species 0.000 description 1
- 240000001890 Ribes hudsonianum Species 0.000 description 1
- 235000016954 Ribes hudsonianum Nutrition 0.000 description 1
- 235000001466 Ribes nigrum Nutrition 0.000 description 1
- 235000011034 Rubus glaucus Nutrition 0.000 description 1
- 244000235659 Rubus idaeus Species 0.000 description 1
- 235000009122 Rubus idaeus Nutrition 0.000 description 1
- AYFVYJQAPQTCCC-UHFFFAOYSA-N Threonine Natural products CC(O)C(N)C(O)=O AYFVYJQAPQTCCC-UHFFFAOYSA-N 0.000 description 1
- 239000004473 Threonine Substances 0.000 description 1
- QIVBCDIJIAJPQS-UHFFFAOYSA-N Tryptophan Natural products C1=CC=C2C(CC(N)C(O)=O)=CNC2=C1 QIVBCDIJIAJPQS-UHFFFAOYSA-N 0.000 description 1
- -1 VB1 Natural products 0.000 description 1
- 240000000851 Vaccinium corymbosum Species 0.000 description 1
- 235000003095 Vaccinium corymbosum Nutrition 0.000 description 1
- 235000017537 Vaccinium myrtillus Nutrition 0.000 description 1
- 244000077923 Vaccinium vitis idaea Species 0.000 description 1
- 235000017606 Vaccinium vitis idaea Nutrition 0.000 description 1
- KZSNJWFQEVHDMF-UHFFFAOYSA-N Valine Natural products CC(C)C(N)C(O)=O KZSNJWFQEVHDMF-UHFFFAOYSA-N 0.000 description 1
- 241000219094 Vitaceae Species 0.000 description 1
- 241001247821 Ziziphus Species 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 208000011775 arteriosclerosis disease Diseases 0.000 description 1
- 235000021015 bananas Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000021028 berry Nutrition 0.000 description 1
- 235000021014 blueberries Nutrition 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
- 235000004883 caffeic acid Nutrition 0.000 description 1
- 229940074360 caffeic acid Drugs 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 229940106157 cellulase Drugs 0.000 description 1
- 235000012000 cholesterol Nutrition 0.000 description 1
- 235000013985 cinnamic acid Nutrition 0.000 description 1
- 229930016911 cinnamic acid Natural products 0.000 description 1
- QAIPRVGONGVQAS-UHFFFAOYSA-N cis-caffeic acid Natural products OC(=O)C=CC1=CC=C(O)C(O)=C1 QAIPRVGONGVQAS-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- GRWZHXKQBITJKP-UHFFFAOYSA-L dithionite(2-) Chemical group [O-]S(=O)S([O-])=O GRWZHXKQBITJKP-UHFFFAOYSA-L 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000020774 essential nutrients Nutrition 0.000 description 1
- 108010093305 exopolygalacturonase Proteins 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 235000019197 fats Nutrition 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- KSEBMYQBYZTDHS-HWKANZROSA-N ferulic acid Chemical compound COC1=CC(\C=C\C(O)=O)=CC=C1O KSEBMYQBYZTDHS-HWKANZROSA-N 0.000 description 1
- 235000001785 ferulic acid Nutrition 0.000 description 1
- 229940114124 ferulic acid Drugs 0.000 description 1
- KSEBMYQBYZTDHS-UHFFFAOYSA-N ferulic acid Natural products COC1=CC(C=CC(O)=O)=CC=C1O KSEBMYQBYZTDHS-UHFFFAOYSA-N 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 229940074391 gallic acid Drugs 0.000 description 1
- 235000004515 gallic acid Nutrition 0.000 description 1
- 235000021021 grapes Nutrition 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 229960000310 isoleucine Drugs 0.000 description 1
- AGPKZVBTJJNPAG-UHFFFAOYSA-N isoleucine Natural products CCC(C)C(N)C(O)=O AGPKZVBTJJNPAG-UHFFFAOYSA-N 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 229930182817 methionine Natural products 0.000 description 1
- WBYWAXJHAXSJNI-UHFFFAOYSA-N methyl p-hydroxycinnamate Natural products OC(=O)C=CC1=CC=CC=C1 WBYWAXJHAXSJNI-UHFFFAOYSA-N 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001728 nano-filtration Methods 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 235000021017 pears Nutrition 0.000 description 1
- 238000004094 preconcentration Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
- YIBXWXOYFGZLRU-UHFFFAOYSA-N syringic aldehyde Natural products CC12CCC(C3(CCC(=O)C(C)(C)C3CC=3)C)C=3C1(C)CCC2C1COC(C)(C)C(O)C(O)C1 YIBXWXOYFGZLRU-UHFFFAOYSA-N 0.000 description 1
- QURCVMIEKCOAJU-UHFFFAOYSA-N trans-isoferulic acid Natural products COC1=CC=C(C=CC(O)=O)C=C1O QURCVMIEKCOAJU-UHFFFAOYSA-N 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 239000004474 valine Substances 0.000 description 1
- WKOLLVMJNQIZCI-UHFFFAOYSA-N vanillic acid Chemical compound COC1=CC(C(O)=O)=CC=C1O WKOLLVMJNQIZCI-UHFFFAOYSA-N 0.000 description 1
- TUUBOHWZSQXCSW-UHFFFAOYSA-N vanillic acid Natural products COC1=CC(O)=CC(C(O)=O)=C1 TUUBOHWZSQXCSW-UHFFFAOYSA-N 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/02—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation containing fruit or vegetable juices
- A23L2/04—Extraction of juices
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/70—Clarifying or fining of non-alcoholic beverages; Removing unwanted matter
- A23L2/80—Clarifying or fining of non-alcoholic beverages; Removing unwanted matter by adsorption
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
- C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G99/00—Subject matter not provided for in other groups of this subclass
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Botany (AREA)
- Mycology (AREA)
- Medicines Containing Plant Substances (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The method for continuously extracting and separating various natural active ingredients from the mulberries comprises the following steps: (1) crushing raw materials and leaching with cold water; (2) centrifuging; (3) adsorbing by macroporous adsorption resin; (4) and (3) separating anthocyanin: eluting with low alcohol; (5) and (3) separation of polyphenol: eluting with high ethanol; (6) desalting and decoloring: passing through a series of cation-anion exchange resin columns; (7) separation of total amino acids: eluting the cation exchange resin column with dilute ammonia water. The method can realize the comprehensive utilization of mulberry resources, and has the advantages of high product yield, high active ingredient content, simple process, strong operability, low equipment requirement, low production cost, safety, greenness, environmental protection and suitability for industrial production.
Description
Technical Field
The invention relates to a method for extracting and separating natural active ingredients of mulberries, in particular to a method for continuously extracting and separating various natural active ingredients from mulberries.
Background
Mulberries, also known as jujubes, mulberries, mulberry seeds, mulberries and the like, are polymeric succulent berries born by perennial woody plants, are cylindrical, have a length of 1-2cm and a diameter of 0.5-0.8cm, and are ripe in about 4-6 months per year. The ripe mulberry fruit is mellow, sour and sweet, and is preferably large, thick in flesh, purplish red in color and rich in sugar. The mulberry juice is thick and honey-like, sweet and sour, fragrant and rich in nutrient components, is listed as one of 'medicinal and edible' agricultural products which are both food and medicines by the national ministry of health, and is praised as 'third generation fruit' together with sea buckthorn and raspberry.
Anthocyanidin is also called anthocyanidin, is a main color substance in plant flowers and fruits, is known as the 7 th most essential nutrient of human body after water, protein, fat, sugar, vitamin and mineral substances, and becomes the pigment with the most development prospect in natural pigments. The mulberry anthocyanin has been listed as a food additive variety which is approved by public notice of the health department due to the characteristics of high extraction rate, stable structure and the like, and is widely applied to the fields of food and health care products. The mulberry anthocyanin mainly comprises: cyanidin-3-O-glucoside, cyanidin-3-O-rutinoside, pelargonidin-3-O-glucoside, pelargonidin-3-O-rutinoside, etc.
In addition, the mulberry contains polyphenols such as gallic acid, protocatechuic acid, caffeic acid, syringic acid, cinnamic acid, ferulic acid, vanillic acid and coumaric acid, and these compounds have the effects of resisting arteriosclerosis, reducing cholesterol, resisting oxidation and resisting radiation.
The mulberry also contains various amino acids, wherein 6 amino acids such as threonine, lysine, valine, methionine, tryptophan, isoleucine and the like are necessary amino acids for human bodies, and the content of the total amino acids of the mulberry is 6-8 times higher than that of grapes, bananas, pears and oranges. The mulberry contains multiple vitamins such as VB1, VB2, VB3, VB5, VB6, VC, VE and the like, wherein the content of VC is the highest. Besides polysaccharides, the saccharide components in mulberry include fructose, glucose and sucrose, which are easily absorbed by human body.
China is the earliest country for breeding mulberry silkworms in the world, the cultivation of mulberry has a history of more than four thousand years, and the variety, variety and yield of mulberry are the top of the world. The mulberry resources in China are rich, and a plurality of methods for extracting anthocyanin from mulberries are provided. However, anthocyanin is only one of the active ingredients with economic value in mulberries, and if anthocyanin in mulberries is extracted and separated, and other ingredients are discarded as waste residues and waste materials, huge waste of resources is undoubtedly caused, so that environmental pollution is increased, and the production and processing cost is high. Therefore, the comprehensive utilization of mulberry resources should be solved early.
CN102212053A discloses a mulberry anthocyanin extraction method, which takes mulberry as a raw material, and comprises the steps of enzymolysis of cellulase and pectinase by ultrasound, extraction of deoxyhydrochloric acid aqueous solution at 75 ℃, flocculation of polymeric ferric sulfate, filtration, macroporous resin adsorption, nanofiltration membrane filtration of eluent and the like, thus obtaining the anthocyanin product with the highest product purity of 32%. In the method, whether the ultrasonic wave has promotion effect on the enzymolysis of the mulberry under the condition is uncertain, the anthocyanin is degraded due to overhigh extraction temperature, and partial anthocyanin is likely to be precipitated in the flocculation process of polymeric ferric sulfate, so that the yield of the mulberry anthocyanin obtained by the method is low.
CN102659743A discloses a method for extracting and refining anthocyanin from mulberry, which comprises the steps of taking fresh mulberry as a raw material, carrying out heat preservation extraction by acid water or acidic alcohol water solution, filtering, carrying out reduced pressure concentration, carrying out adsorption by macroporous adsorption resin, resolving aqueous alcohol solution, concentrating, carrying out spray drying and the like to obtain a mixture of anthocyanin and procyanidine. The method adopts spray drying mode, and can cause anthocyanin to degrade due to overhigh temperature.
CN104961783A discloses a method for effectively extracting anthocyanin and anthocyanin, which comprises the steps of taking cowberry, blackcurrant, blueberry, mulberry and black rice as raw materials, stirring and extracting by using an ethanol solution, concentrating under reduced pressure, refining by using macroporous adsorption resin, eluting by using ethanol, concentrating, spray drying and the like to obtain an extract containing anthocyanin and anthocyanin. The method adopts spray drying mode, and can cause anthocyanin to degrade due to overhigh temperature.
CN105524035A discloses a method for preparing mulberry anthocyanin, which comprises the steps of taking mulberries as raw materials, extracting with an alkaline aqueous solution containing a natural antioxidant, acidifying, flocculating, adsorbing by cation exchange resin, eluting with an acidic solution, concentrating under reduced pressure, spray drying and the like to obtain a mulberry anthocyanin product. Anthocyanins are extremely unstable in alkaline environments and flocculation and spray drying can lead to degradation of anthocyanins.
CN105949164A discloses a mulberry anthocyanin extraction method, which comprises the steps of pulping fresh mulberries as a raw material, acidifying with hydrochloric acid and stirring and leaching with ethanol, centrifuging, concentrating, extracting with ethyl acetate, carrying out macroporous resin adsorption column chromatography, eluting with ethanol, carrying out reduced pressure concentration and the like to obtain the mulberry anthocyanin. The method uses too much inflammable and explosive organic solvent, and is not suitable for industrial production.
CN106954773A discloses a processing method for comprehensively utilizing mulberry juice, which takes fresh mulberry fruits as raw materials, and the anthocyanin and concentrated, fermented and decolored mulberry juice are obtained through the steps of sorting, cleaning, squeezing, rough filtering, sterilization, enzymolysis, centrifugation, ultrafiltration, preconcentration, resin adsorption, water washing, anthocyanin elution, vacuum concentration, freeze drying, fermentation and the like. The method has low extraction rate of anthocyanidin.
The methods all have a common defect that only anthocyanin or anthocyanin active ingredients in the mulberry can be obtained, other natural active ingredients in the mulberry are not extracted and utilized, and the comprehensive and full utilization of natural resources is not realized.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects in the prior art and provide the method for continuously extracting and separating the natural active ingredients from the mulberry, which has the advantages of high product yield, high active ingredient content and simple process and can continuously extract the natural active ingredients.
The technical scheme for solving the technical problems is that the method for continuously extracting and separating various natural active ingredients from the mulberry comprises the following steps:
(1) crushing raw materials, and leaching in cold water: crushing a mulberry raw material by using a crusher, adding cold water containing an anthocyanin protective agent, stirring, leaching, filtering, and collecting filtrate; obtaining cold water leaching liquor;
(2) centrifuging: centrifuging the cold water leaching liquor obtained in the step (1), and collecting a centrifugate;
(3) adsorption by macroporous adsorption resin: passing the centrifugate obtained in the step (2) through a macroporous adsorption resin column, and collecting effluent liquid on the column on the macroporous adsorption resin column for later use; after the column is loaded, washing the macroporous adsorption resin column to be slightly acidic by using pure water;
(4) and (3) separating anthocyanin: eluting the macroporous adsorption resin column which is washed to be slightly acidic in the step (3) by using low-alcohol to obtain low-alcohol eluent; concentrating the low-alcohol eluent under reduced pressure, and performing microwave drying to obtain an anthocyanin product;
(5) and (3) separation of polyphenol: eluting the macroporous adsorption resin column in the step (4) by using high ethanol to obtain high ethanol eluent; concentrating the high-alcohol eluent under reduced pressure, and performing microwave drying to obtain polyphenol products;
(6) desalting and decoloring: enabling the effluent liquid of the macroporous adsorption resin column upper column obtained in the step (3) to pass through a cation exchange resin column-anion exchange resin column connected in series, and collecting the effluent liquid of the cation exchange resin column-anion exchange resin column upper column; concentrating the effluent liquid on the cation exchange resin column and the anion exchange resin column under reduced pressure to obtain a decolorized concentrated mulberry juice product;
(7) separation of total amino acids: eluting the cation exchange resin column after the column is loaded in the step (6) by using dilute ammonia water, and collecting eluent; and (4) concentrating the eluent under reduced pressure, and drying by microwave to obtain a total amino acid product.
Further, in the step (1), the temperature of the cold water is 0-15 ℃; the anthocyanin protective agent is hydrosulfite, and the concentration of the anthocyanin protective agent in cold water is 0.05-0.5%.
Further, the bisulfite is sodium bisulfite, potassium bisulfite, calcium bisulfite, or ammonium bisulfite.
The purpose of using the anthocyanin protective agent is to prevent the anthocyanin from being oxidized and degraded in the processes of extraction, centrifugation and column loading. If the concentration of the protective agent is too low (the dosage is too small), the purpose of preventing the anthocyanin from being oxidized and degraded cannot be achieved; if the concentration of the protective agent is too high (too much amount), the material is wasted, and the burden of the subsequent desalting step is increased.
Further, in the step (1), stirring and leaching are carried out for 2 times, the amount of cold water used for the first time is 8-10 times of the weight of the mulberry raw material, the amount of cold water used for the second time is 5-8 times of the weight of the mulberry raw material, and the stirring and extracting time is 2-4 hours for the first time and 1-3 hours for the second time; the filtrates obtained by 2 times of leaching and filtration are combined.
The extraction with cold water under stirring is aimed at preventing the degradation of various active ingredients due to the over-high extraction temperature. The purpose of leaching twice is to ensure that various water-soluble active ingredients in the mulberry are thoroughly leached.
Further, in the step (2), the centrifugation is sedimentation type centrifugation, and the separation factor is 2000-5000.
The purpose of centrifugation is to remove water insoluble substances such as fine raw material particles, silt, plant fibers and the like in the cold water leaching liquor, so that the feed liquid is clarified. If the separation factor of the centrifuge is too small, the solid-liquid separation is insufficient, so that the raw material liquid on the macroporous resin column is turbid, and the adsorption and desorption are not facilitated; if the separation factor of the centrifugal machine is too large, the parameter requirement of the equipment is improved, and the input cost of the equipment is increased.
Further, in the step (3), the model of the macroporous adsorption resin is DM21, DM21D, DM28, LK2MG, DM-8 or AB-8; the height-diameter ratio of the macroporous adsorption resin column is 1-5: 1; the dosage of the resin is 0.5-3.0 times (L/kg) of the weight of the mulberry raw material; the flow rate of the upper column is 0.5-2.0 BV/h.
The macroporous adsorption resin column is used for adsorbing and enriching mulberry anthocyanin and mulberry polyphenol in the centrifugate on the macroporous adsorption resin. If the using amount of the macroporous adsorption resin is too small, the flow rate of the macroporous adsorption resin on the column is too high or the height-diameter ratio is too small, the mulberry anthocyanin and the mulberry polyphenol cannot be fully adsorbed; if the dosage of the macroporous absorption resin is too much, the flow rate of the macroporous absorption resin on the column is too slow or the height-diameter ratio is too large, the production period is prolonged and the production cost is increased.
Further, in the step (3), the amount of the pure water is 3-4 BV, and the flow rate of the washing is 1-2 BV/h.
The purpose of the water washing is to remove impurities such as salts and sugars which cannot be adsorbed in the resin column.
Further, in the step (4), the volume concentration of the low-alcohol ethanol is 30-40%; the dosage of the low alcohol is 2-3 BV; the flow rate of low-alcohol elution is 1-2 BV/h.
The purpose of low-alcohol elution is to elute the mulberry anthocyanidin adsorbed on the macroporous adsorption resin. If the volume concentration of the low-alcohol ethanol is too low, the dosage is too small or the elution flow rate is too high, the anthocyanin cannot be completely eluted, and the yield of the anthocyanin is low; if the volume concentration of the low-alcohol ethanol is too high, the dosage is too high or the elution flow rate is too low, part of the mulberry polyphenol can be eluted, so that the purity (content) of the anthocyanin product is low, and the yield of the mulberry polyphenol is low.
Further, in the step (5), the volume concentration of the high-ethanol is 55-70%, the using amount of the high-ethanol is 2-3 BV, and the flow rate of the high-ethanol elution is 1-2 BV/h.
The purpose of the high ethanol elution is to elute the mulberry polyphenol adsorbed on the macroporous adsorbent resin. If the volume concentration of the high-alcohol is too low, the dosage is too small or the elution flow rate is too high, the polyphenol cannot be completely eluted, and the yield of the polyphenol is low; if the volume concentration of the high-alcohol is too high, the dosage is too high or the elution flow rate is too low, the energy and the materials are wasted.
Further, in the step (4), the step (5) and the step (7), the temperature of the reduced pressure concentration is 55-60 ℃, the vacuum degree is-0.08-0.09 MPa, and the concentration is carried out until the solid content is 15-25%; the temperature of the microwave drying is 50-60 ℃, the vacuum degree is-0.08-0.09 MPa, and the microwave frequency is 2450-2550 MHz.
Further, in the step (6), the cation exchange resin is a strongly acidic styrene-based cation exchange resin, and the type of the cation exchange resin is 001 × 7, 001 × 8, 001 × 12, or 001 × 16.
Further, in the step (6), the height-diameter ratio of the cation exchange resin column is 3-6: 1, and the flow rate of the material passing through the cation exchange resin column is 1-2 BV/h; the resin dosage of the cation exchange resin is 0.1-0.5 time (L/kg) of the weight of the mulberry raw material.
The purpose of using the cation exchange resin column is to desalt and adsorb amino acids in the column effluent on the macroporous adsorbent resin column. If the amount of the cation exchange resin used is too small, the aspect ratio of the cation exchange resin column is too small, or the flow rate of the material passing through the cation exchange resin column is too high, the above-mentioned object cannot be sufficiently achieved. If the dosage of the cation exchange resin is too much, the height-diameter ratio of the cation exchange resin column is too large or the flow rate of the material passing through the cation exchange resin column is too slow, the waste of energy or material is caused.
Further, in the step (6), the anion exchange resin is a macroporous strongly basic anion exchange resin; the cation exchange resin is preferably of the type D941, D945, D285 or 330.
Further, in the step (6), the height-diameter ratio of the anion exchange resin column is 3-6: 1; the flow rate of the materials passing through the anion exchange resin column is 1-2 BV/h; the resin dosage of the anion exchange resin is 0.1-0.5 time (L/kg) of the weight of the mulberry raw material.
The purpose of using the anion exchange resin column is to decolor and remove impurities so as to improve the purity of the decolored concentrated juice of the mulberry. If the amount of the anion exchange resin used is too small, the aspect ratio of the anion exchange resin column is too small, or the flow rate of the material passing through the anion exchange resin column is too high, the above-mentioned objects cannot be sufficiently achieved. If the dosage of the anion exchange resin is too much, the height-diameter ratio of the anion exchange resin column is too large or the flow rate of the material passing through the anion exchange resin column is too slow, the waste of energy or material is caused.
Further, in the step (6), the temperature of the reduced pressure concentration is 60-70 ℃, the vacuum degree is-0.08 to-0.09 MPa, and the concentration is carried out until the sugar degree is 55-65 Brix; the concentration of the dilute ammonia water is 0.5-1.0 mol/L, the using amount of the dilute ammonia water is 3-5 BV, and the eluting flow rate of the dilute ammonia water is 1-2 BV/h.
The purpose of elution with dilute ammonia water is to elute the mulberry amino acid adsorbed on the cation exchange resin. If the concentration of the dilute ammonia water is too low, the dosage is too small or the elution flow rate is too high, the amino acid cannot be completely eluted, so that the yield of the amino acid is low; if the concentration of the dilute ammonia water is too high, the dosage is too high or the elution flow rate is too low, the waste of energy and materials is caused.
In the present invention, 1BV =1 column volume.
The principle of the method of the invention is as follows: the low-temperature cold water extraction containing the anthocyanin protective agent can fully leach water-soluble ingredients in the mulberry raw material and ensure that the extracted natural active ingredients have stable properties and are not oxidized and degraded. The mulberry anthocyanin and the mulberry polyphenol in the water-soluble components are adsorbed in the macroporous adsorption resin through selective enrichment of the macroporous adsorption resin, and then the mulberry anthocyanin and the mulberry polyphenol are sequentially eluted from the macroporous adsorption resin column in a gradient elution mode according to different polarities of the mulberry anthocyanin and the mulberry polyphenol, so that the separation of the mulberry anthocyanin and the mulberry polyphenol is realized. Other water-soluble components including amino acids, polysaccharides, sucrose, fructose, glucose, vitamins, inorganic salts, etc. are not adsorbed by the macroporous adsorbent resin and exist in the effluent of the column on the macroporous adsorbent resin column. Desalting and decoloring the column effluent on the macroporous adsorption resin column by using a cation-anion exchange resin column to obtain an important byproduct, namely mulberry decolored concentrated juice. The amino acid is enriched by cation exchange resin, and is eluted by ammonia water, concentrated and dried to obtain the mulberry amino acid product.
Compared with the prior art, the invention has the following beneficial effects:
(1) the anthocyanin content of the mulberry anthocyanin product obtained by the invention is 65.49%, and the yield is 95.27%; the polyphenol content of the mulberry polyphenol product reaches 85.72 percent, and the yield reaches 93.48 percent; the amino acid content of the mulberry amino acid product reaches up to 71.43 percent, and the yield reaches 91.39 percent.
(2) The method can simultaneously extract three natural active ingredients in the mulberry, realizes full and comprehensive utilization of mulberry resources, and has the advantages of simple process, strong operability, low requirement on equipment, low production cost, safety, greenness, environmental protection and suitability for industrial production.
(3) The invention comprehensively treats the effluent liquid on the macroporous adsorption resin column, which is usually used as waste liquid in the actual production, so that the decolorized concentrated juice of mulberry rich in polysaccharide, sucrose, fructose, glucose and vitamins is obtained, the added value of the product is greatly improved, the environmental pollution is reduced, and the resource utilization rate is improved.
Detailed Description
The present invention will be further described with reference to the following examples.
The mulberry raw material used in the embodiment of the invention is purchased from Sichuan, wherein the anthocyanin, the polyphenol and the amino acid are respectively 1.83%, 5.30% and 0.67% in percentage by mass; the macroporous adsorption resin and the ion exchange resin used in the embodiment of the invention are purchased from Aimeikejian (China) biological medicine Co., Ltd; the starting materials or chemicals used in the examples of the present invention are, unless otherwise specified, commercially available in a conventional manner.
In the embodiment of the invention, the content of mulberry anthocyanins (containing cyanidin-3-O-glucoside, cyanidin-3-O-rutinoside, pelargonidin-3-O-glucoside and pelargonidin-3-O-rutinoside) is determined by adopting a High Performance Liquid Chromatography (HPLC) external standard method, the content of mulberry polyphenol is determined by adopting a ferrous tartrate colorimetric method, and the content of mulberry amino acid (total) is determined by adopting a ninhydrin color rendering method.
Example 1
The embodiment comprises the following steps:
(1) crushing raw materials, and leaching in cold water: taking 100kg of dried mulberry raw material, crushing the mulberry raw material by using a crusher until the particle size is 1-2 mm, adding 1000L of cold water (containing sodium bisulfite with the mass concentration of 0.3%) with the temperature of 8 ℃, stirring and leaching for 4 hours, carrying out coarse filtration, and collecting filter residues and filtrate; stirring and leaching the filter residue with 600L of the same cold water for 2 hours again, coarsely filtering, and collecting the filtrate; then combining the two filtrates to obtain a cold water leaching liquor;
(2) centrifuging: centrifuging the cold water leaching liquor obtained in the step (1) by using a sedimentation type centrifuge with a separation factor of 3200, and collecting a centrifugate;
(3) adsorption by macroporous adsorption resin: enabling the centrifugate obtained in the step (2) to pass through a macroporous adsorption resin column (the model of the macroporous adsorption resin is DM21, the height-diameter ratio of the macroporous adsorption resin column is 4:1, the using amount of the macroporous adsorption resin is 150L, and the flow rate of the macroporous adsorption resin column is 1.5 BV/h), and collecting the effluent liquid of the macroporous adsorption resin column on the column for standby; after the column loading, washing the macroporous adsorption resin column to be slightly acidic by using 3BV of pure water at the flow rate of 1.5 BV/h;
(4) and (3) separating anthocyanin: eluting the macroporous adsorption resin column which is washed to be slightly acidic in the step (3) by using low-alcohol with the volume concentration of 32% and the flow rate of elution being 2BV/h, concentrating the low-alcohol eluent under reduced pressure under the conditions that the temperature is 60 ℃ and the vacuum degree is-0.08 MPa until the solid content is 20%, and then carrying out microwave drying on the concentrated solution under the conditions that the temperature is 60 ℃, the vacuum degree is-0.08 MPa and the microwave frequency is 2450MHz to obtain 2.70kg of mulberry anthocyanin product;
(5) and (3) separation of polyphenol: eluting the macroporous adsorption resin column eluted in the step (4) by using high ethanol with the volume concentration of 70% and the flow rate of elution being 1BV/h at 2.5 BV, concentrating the high ethanol eluent under reduced pressure under the conditions that the temperature is 60 ℃ and the vacuum degree is-0.08 MPa until the solid content is 22%, and then carrying out microwave drying on the concentrated solution under the conditions that the temperature is 60 ℃, the vacuum degree is-0.08 MPa and the microwave frequency is 2450MHz to obtain 5.73kg of mulberry polyphenol products;
(6) desalting and decoloring: enabling the effluent liquid of the macroporous adsorption resin column in the step (3) to pass through a cation-anion exchange resin column (the type of the cation exchange resin is 001 multiplied by 16, the using amount of the cation exchange resin is 20L, the height-diameter ratio of the cation exchange resin column is 4:1, the flow rate of the material passing through the cation exchange resin column is 1BV/h, the type of the anion exchange resin is D941, the using amount of the anion exchange resin is 20L, the height-diameter ratio of the anion exchange resin column is 4:1, the flow rate of the material passing through the anion exchange resin column is 1 BV/h), collecting the effluent liquid of the cation-anion exchange resin column, and concentrating under reduced pressure at the temperature of 70 ℃ and the vacuum degree of-0.08 MPa until the sugar degree is 65Brix to obtain 30.77kg of the decolorized concentrated mulberry juice product;
(7) separation of total amino acids: eluting the cation exchange resin column eluted in the step (6) with dilute ammonia water of 4BV and 0.7mol/L concentration at the eluting flow rate of 1.5BV/h, concentrating the dilute ammonia water eluent under reduced pressure, and drying by microwave to obtain 0.85kg of mulberry total amino acid product.
The content of anthocyanin in the mulberry anthocyanin product obtained in the embodiment is 64.57% and the yield of mulberry anthocyanin is 95.27% as determined by a High Performance Liquid Chromatography (HPLC) external standard method; according to the determination of a ferrous tartrate colorimetric method, the polyphenol content of the mulberry polyphenol product obtained in the embodiment is 82.27%, and the yield of the mulberry polyphenol is 88.94%; the amino acid content of the mulberry amino acid product obtained in the example is 71.43% and the yield of total amino acids of the mulberry is 90.62% as determined by a ninhydrin color development method.
Example 2
The embodiment comprises the following steps:
(1) crushing raw materials, and leaching in cold water: taking 100kg of dried mulberry raw material, crushing the mulberry raw material by using a crusher until the particle size is 1-2 mm, adding 800L of cold water (containing potassium bisulfite and the concentration of 0.1%) with the temperature of 5 ℃, stirring and leaching for 3.5 hours, carrying out coarse filtration, and collecting filter residues and filtrate; stirring and leaching the filter residue with 700L of the same cold water for 3 hours again, coarsely filtering, and collecting the filtrate; then combining the two filtrates to obtain a cold water leaching liquor;
(2) centrifuging: centrifuging the cold water leaching liquor obtained in the step (1) by using a decanter centrifuge with the separation factor of 4000, and collecting a centrifugate;
(3) adsorption by macroporous adsorption resin: enabling the centrifugate obtained in the step (2) to pass through a macroporous adsorption resin column (the model of the macroporous adsorption resin is DM21D, the height-diameter ratio of the macroporous adsorption resin column is 3.5:1, the using amount of the macroporous adsorption resin is 200L, and the flow rate of the macroporous adsorption resin column is 2.0 BV/h), and collecting the effluent liquid of the macroporous adsorption resin column; after the column loading, washing the macroporous absorption resin column to be slightly acidic by using 3.5 BV of pure water at the flow rate of 1.5 BV/h;
(4) and (3) separating anthocyanin: eluting the macroporous adsorption resin column which is washed to be slightly acidic in the step (3) by using low-alcohol with the volume concentration of 35% and the flow rate of elution being 1.5BV/h, concentrating the low-alcohol eluent under reduced pressure under the conditions that the temperature is 56 ℃ and the vacuum degree is-0.09 MPa until the solid content is 18%, and then carrying out microwave drying on the concentrated solution under the conditions that the temperature is 56 ℃, the vacuum degree is-0.09 MPa and the microwave frequency is 2450MHz to obtain 2.69kg of mulberry anthocyanin products;
(5) and (3) separation of polyphenol: eluting the macroporous adsorption resin column eluted in the step (4) by using high ethanol with the volume concentration of 65% and the flow rate of elution being 1.5BV/h at 3BV, concentrating the high ethanol eluent under reduced pressure under the conditions that the temperature is 58 ℃ and the vacuum degree is-0.09 MPa until the solid content is 20%, and then performing microwave drying on the concentrated solution under the conditions that the temperature is 58 ℃, the vacuum degree is-0.09 MPa and the microwave frequency is 2450MHz to obtain 5.78kg of mulberry polyphenol product;
(6) desalting and decoloring: enabling the effluent liquid of the macroporous adsorption resin column in the step (3) to pass through a cation-anion exchange resin column (the type of the cation exchange resin is 001 multiplied by 12, the using amount of the cation exchange resin is 30L, the height-diameter ratio of the cation exchange resin column is 5:1, the flow rate of the material passing through the cation exchange resin column is 1.5BV/h, the type of the anion exchange resin is D945, the using amount of the anion exchange resin is 30L, the height-diameter ratio of the anion exchange resin column is 5:1, the flow rate of the material passing through the anion exchange resin column is 1.5 BV/h), collecting the effluent liquid of the cation-anion exchange resin column, and concentrating under reduced pressure under the conditions that the temperature is 68 ℃ and the vacuum degree is-0.08 MPa until the sugar degree is 60 Brix to obtain 32.67kg of the concentrated decolorized mulberry juice;
(7) separation of total amino acids: eluting the cation exchange resin column eluted in the step (6) with dilute ammonia water of 5BV and 0.6mol/L concentration at the elution flow rate of 2BV/h, concentrating the dilute ammonia water eluent under reduced pressure, and drying by microwave to obtain 0.88kg of mulberry total amino acid product.
The content of the anthocyanin in the mulberry anthocyanin product obtained in the embodiment is 63.19% and the yield of the mulberry anthocyanin is 92.89% as determined by a High Performance Liquid Chromatography (HPLC) external standard method; according to the determination of a ferrous tartrate colorimetric method, the polyphenol content of the mulberry polyphenol product obtained in the embodiment is 85.72%, and the yield of the mulberry polyphenol is 93.48%; the amino acid content of the mulberry amino acid product obtained in the example is 69.58% and the yield of total amino acids of mulberry is 91.39% as determined by a ninhydrin color development method.
Example 3
The embodiment comprises the following steps:
(1) crushing raw materials, and leaching in cold water: taking 100kg of dried mulberry raw material, crushing the mulberry raw material by using a crusher until the particle size is 1-2 mm, adding 900L of cold water (containing calcium hydrogen sulfite and the concentration of 0.05%) with the temperature of 10 ℃, stirring and leaching for 3 hours, carrying out coarse filtration, and collecting filter residues and filtrate; stirring and leaching the filter residue with 800L of the same cold water for 2.5 hours again, coarsely filtering, and collecting the filtrate; then combining the two filtrates to obtain a cold water leaching liquor;
(2) centrifuging: centrifuging the cold water leaching liquor obtained in the step (1) by using a sedimentation type centrifuge with a separation factor of 3500, and collecting a centrifugate;
(3) adsorption by macroporous adsorption resin: enabling the centrifugate obtained in the step (2) to pass through a macroporous adsorption resin column (the model of the macroporous adsorption resin is LK2MG, the height-diameter ratio of the macroporous adsorption resin column is 5:1, the using amount of the macroporous adsorption resin is 180L, and the flow rate of the macroporous adsorption resin column is 1.0 BV/h), and collecting the effluent liquid of the macroporous adsorption resin column; after the column loading is finished, washing the macroporous adsorption resin column to be slightly acidic by using 4BV of pure water at the flow rate of 2 BV/h;
(4) and (3) separating anthocyanin: eluting the macroporous adsorption resin column which is washed to be slightly acidic in the step (3) by using low-alcohol with the volume concentration of 30% and the flow rate of elution being 1BV/h, concentrating the low-alcohol eluent under reduced pressure under the conditions of the temperature of 58 ℃ and the vacuum degree of minus 0.08MPa until the content of solid matters is 23%, and then carrying out microwave drying on the concentrated solution under the conditions of the temperature of 58 ℃, the vacuum degree of minus 0.08MPa and the microwave frequency of 2450MHz to obtain 2.63kg of the mulberry anthocyanin product;
(5) and (3) separation of polyphenol: eluting the macroporous adsorption resin column eluted in the step (4) by using high ethanol with the volume concentration of 60% and the flow rate of elution being 1.5BV/h and with the volume concentration of 3BV, concentrating the high ethanol eluent under the conditions of the temperature of 60 ℃ and the vacuum degree of minus 0.08MPa until the solid content is 18%, and then carrying out microwave drying on the concentrated solution under the conditions of the temperature of 60 ℃, the vacuum degree of minus 0.08MPa and the microwave frequency of 2450MHz to obtain 5.46kg of mulberry polyphenol product;
(6) desalting and decoloring: enabling the effluent liquid of the macroporous adsorption resin column in the step (3) to pass through a cation-anion exchange resin column (the type of cation exchange resin is 001 multiplied by 7, the dosage of the cation exchange resin is 25L, the height-diameter ratio of the cation exchange resin column is 6:1, the flow rate of the material passing through the cation exchange resin column is 2BV/h, the type of anion exchange resin is D285, the dosage of the anion exchange resin is 25L, the height-diameter ratio of the anion exchange resin column is 6:1, the flow rate of the material passing through the anion exchange resin column is 2 BV/h), collecting the effluent liquid of the cation-anion exchange resin column, and concentrating under the conditions that the temperature is 65 ℃ and the vacuum degree is-0.09 MPa until the sugar degree is 63 Brix to obtain 31.43kg of the mulberry decolorized concentrated juice product;
(7) separation of total amino acids: eluting the cation exchange resin column eluted in the step (6) with dilute ammonia water of 4.5BV and 0.9mol/L concentration at the elution flow rate of 1BV/h, concentrating the dilute ammonia water eluent under reduced pressure, and performing microwave drying to obtain 0.89kg of mulberry total amino acid product.
The content of the anthocyanin in the mulberry anthocyanin product obtained in the embodiment is 65.49% and the yield of the mulberry anthocyanin is 94.12% as determined by a High Performance Liquid Chromatography (HPLC) external standard method; according to the determination of a ferrous tartrate colorimetric method, the polyphenol content of the mulberry polyphenol product obtained in the embodiment is 83.50%, and the yield of the mulberry polyphenol is 86.02%; the amino acid content of the mulberry amino acid product obtained in the example is 68.74% and the yield of total amino acids of mulberry is 91.31% as determined by a ninhydrin color development method.
Comparative example 1
Comparative example 1 is compared with example 1 except that sodium bisulfite was not added to the cold water used in step (1), and other raw materials and extraction conditions were the same as in example 1.
The content of anthocyanin in the obtained mulberry anthocyanin product is 59.31 percent and the yield of the mulberry anthocyanin is 85.76 percent, which are determined by a High Performance Liquid Chromatography (HPLC) external standard method; according to the determination of a ferrous tartrate colorimetric method, the polyphenol content of the mulberry polyphenol product obtained in the embodiment is 81.37%, and the yield of the mulberry polyphenol is 87.56%; the amino acid content of the mulberry amino acid product obtained in the example is 69.83% and the yield of total mulberry amino acids is 89.74% as determined by a ninhydrin color development method.
Comparative example 2
Comparative example 2 is different from example 1 only in that the concentration of sodium bisulfite in cold water used in step (1) is 0.02%, and other raw materials and extraction conditions are the same as those of example 1.
The anthocyanin content of the obtained mulberry anthocyanin product is 60.18% and the yield of the mulberry anthocyanin is 86.82% as determined by a High Performance Liquid Chromatography (HPLC) external standard method; according to the determination of a ferrous tartrate colorimetric method, the polyphenol content of the mulberry polyphenol product obtained in the embodiment is 84.37%, and the yield of the mulberry polyphenol is 91.65%; the amino acid content of the mulberry amino acid product obtained in the example is 68.68% and the yield of total mulberry amino acids is 90.52% as determined by a ninhydrin color development method.
The above embodiments are specific illustrations of some possible embodiments of the invention, and these embodiments are not intended to limit the scope of the invention, and all equivalent implementations or modifications that do not depart from the scope of the invention are intended to be included within the scope of the claims of the present application.
Claims (10)
1. The method for continuously extracting and separating various natural active ingredients from the mulberries is characterized by comprising the following steps:
(1) crushing raw materials, and leaching in cold water: crushing a mulberry raw material by using a crusher, adding cold water containing an anthocyanin protective agent, stirring, leaching, filtering, and collecting filtrate to obtain cold water leaching liquor;
(2) centrifuging: centrifuging the cold water leaching liquor obtained in the step (1), and collecting a centrifugate;
(3) adsorption by macroporous adsorption resin: passing the centrifugate obtained in the step (2) through a macroporous adsorption resin column, and collecting effluent liquid on the column on the macroporous adsorption resin column for later use; after the column is loaded, washing the macroporous adsorption resin column to be slightly acidic by using pure water;
(4) and (3) separating anthocyanin: eluting the macroporous adsorption resin column which is washed to be slightly acidic in the step (3) by using low-alcohol to obtain low-alcohol eluent; concentrating the low-alcohol eluent under reduced pressure, and performing microwave drying to obtain an anthocyanin product;
(5) and (3) separation of polyphenol: eluting the macroporous adsorption resin column in the step (4) by using high ethanol to obtain high ethanol eluent; concentrating the high-alcohol eluent under reduced pressure, and performing microwave drying to obtain polyphenol products;
(6) desalting and decoloring: enabling the effluent liquid of the macroporous adsorption resin column upper column obtained in the step (3) to pass through a cation exchange resin column-anion exchange resin column connected in series, and collecting the effluent liquid of the cation exchange resin column-anion exchange resin column upper column; concentrating the effluent liquid on the cation exchange resin column and the anion exchange resin column under reduced pressure to obtain a decolorized concentrated mulberry juice product;
(7) separation of total amino acids: eluting the cation exchange resin column after the column is loaded in the step (6) by using dilute ammonia water, and collecting eluent; and (4) concentrating the eluent under reduced pressure, and drying by microwave to obtain a total amino acid product.
2. The method for continuously extracting and separating natural active ingredients from mulberry as claimed in claim 1, wherein in the step (1), the temperature of the cold water is 0-15 ℃; the anthocyanin protective agent is bisulfite, and the concentration of the protective agent in cold water is 0.05-0.5%; the bisulfite is preferably sodium bisulfite, potassium bisulfite, calcium bisulfite, or ammonium bisulfite.
3. The method for continuously extracting and separating multiple natural active ingredients from mulberry according to claim 1 or 2, wherein in the step (1), the stirring extraction is carried out for 2 times, the amount of cold water used for the first time is 8-10 times of the weight of the mulberry raw material, and the amount of cold water used for the second time is 5-8 times of the weight of the mulberry raw material; stirring and extracting for 2-4 hours for the first time and 1-3 hours for the second time; merging the filtrates obtained by leaching and filtering for 2 times; in the step (2), the centrifugation is sedimentation type centrifugation, and the separation factor is 2000-5000.
4. The method for continuously extracting and separating multiple natural active ingredients from the mulberry according to any one of claims 1 to 3, wherein in the step (3), the type of the macroporous adsorption resin is DM21, DM21D, DM28, LK2MG, DM-8 or AB-8, the height-diameter ratio of a macroporous adsorption resin column is 1-5: 1, the amount of the resin is 0.5-3.0 times (L/kg) of the weight of the mulberry raw material, and the flow rate of the resin on the column is 0.5-2.0 BV/h; the amount of the pure water is 3-4 BV, and the flow rate of the washing is 1-2 BV/h.
5. The method for continuously extracting and separating multiple natural active ingredients from mulberry according to any one of claims 1 to 4, wherein in the step (4), the volume concentration of the low-alcohol-content ethanol is 30-40%, the dosage of the low-alcohol-content ethanol is 2-3 BV, and the flow rate of elution of the low-alcohol-content ethanol is 1-2 BV/h.
6. The method for continuously extracting and separating multiple natural active ingredients from mulberry according to any one of claims 1 to 5, wherein in the step (5), the volume concentration of the high-grade ethanol is 55-70%, the using amount of the high-grade ethanol is 2-3 BV, and the flow rate of the high-grade ethanol elution is 1-2 BV/h.
7. The method for continuously extracting and separating multiple natural active ingredients from mulberry according to any one of claims 1 to 6, wherein in the step (4), the step (5) and the step (7), the temperature of the reduced pressure concentration is 55-60 ℃, the vacuum degree is-0.08-0.09 MPa, and the concentration is carried out until the solid content is 15-25%; the temperature of the microwave drying is 50-60 ℃, the vacuum degree is-0.08-0.09 MPa, and the microwave frequency is 2450-2550 MHz.
8. The method for continuously extracting and separating multiple natural active ingredients from mulberry as claimed in any one of claims 1 to 7, wherein in the step (6), the cation exchange resin is a strongly acidic styrene cation exchange resin; the type of the cation exchange resin is preferably 001 × 7, 001 × 8, 001 × 12 or 001 × 16; the height-diameter ratio of the cation exchange resin column is preferably 3-6: 1, and the flow rate of the material passing through the cation exchange resin column is preferably 1-2 BV/h; the dosage of the cation exchange resin is preferably 0.1-0.5 time (L/kg) of the weight of the mulberry raw material.
9. The method for continuously extracting and separating multiple natural active ingredients from mulberry according to any one of claims 1 to 8, wherein in the step (6), the anion exchange resin is a macroporous strong-base anion exchange resin; the cation exchange resin is preferably D941, D945, D285 or 330; the height-diameter ratio of the anion exchange resin column is preferably 3-6: 1; the flow rate of the materials passing through the anion exchange resin column is preferably 1-2 BV/h; the resin dosage of the anion exchange resin is preferably 0.1-0.5 time (L/kg) of the weight of the mulberry raw material.
10. The method for continuously extracting and separating multiple natural active ingredients from mulberry according to any one of claims 1 to 9, wherein in the step (6), the temperature for reduced pressure concentration is 60 to 70 ℃, the vacuum degree is-0.08 to-0.09 MPa, and the concentration is carried out until the sugar degree is 55 to 65 Brix; the concentration of the dilute ammonia water is preferably 0.5-1.0 mol/L, the using amount of the dilute ammonia water is preferably 3-5 BV, and the eluting flow rate of the dilute ammonia water is preferably 1-2 BV/h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110732680.6A CN113397169A (en) | 2021-06-30 | 2021-06-30 | Method for continuously extracting and separating multiple natural active ingredients from mulberries |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110732680.6A CN113397169A (en) | 2021-06-30 | 2021-06-30 | Method for continuously extracting and separating multiple natural active ingredients from mulberries |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113397169A true CN113397169A (en) | 2021-09-17 |
Family
ID=77680341
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110732680.6A Pending CN113397169A (en) | 2021-06-30 | 2021-06-30 | Method for continuously extracting and separating multiple natural active ingredients from mulberries |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113397169A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102018766A (en) * | 2009-09-16 | 2011-04-20 | 博仲盛景医药技术（北京）有限公司 | Plant extractive, extraction method and application thereof as well as composite comprising same |
| CN106832050A (en) * | 2017-02-20 | 2017-06-13 | 湖南华诚生物资源股份有限公司 | The method that pectin is separated from Momordica grosvenori production waste residue |
| CN106954773A (en) * | 2017-03-31 | 2017-07-18 | 中国农业大学 | A kind of processing method of mulberry juice comprehensive utilization |
| CN110105320A (en) * | 2019-05-08 | 2019-08-09 | 湖南华诚生物资源股份有限公司 | From salvia chinensis potato simultaneously separating starch, anthocyanidin and total polyphenols method |
| CN110240584A (en) * | 2019-05-29 | 2019-09-17 | 湖南华诚生物资源股份有限公司 | The method for separating procyanidine, anthocyanidin and ferulic acid simultaneously from purple rice rice bran |
| CN110981921A (en) * | 2019-12-26 | 2020-04-10 | 湖南华诚生物资源股份有限公司 | Continuous method for synchronously extracting multiple effective components from figs |
| CN111533723A (en) * | 2020-05-29 | 2020-08-14 | 禹州市合同泰药业有限公司 | Method for extracting anthocyanin from mature fresh fruits of edible fungus vegetables |
-
2021
- 2021-06-30 CN CN202110732680.6A patent/CN113397169A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102018766A (en) * | 2009-09-16 | 2011-04-20 | 博仲盛景医药技术（北京）有限公司 | Plant extractive, extraction method and application thereof as well as composite comprising same |
| CN106832050A (en) * | 2017-02-20 | 2017-06-13 | 湖南华诚生物资源股份有限公司 | The method that pectin is separated from Momordica grosvenori production waste residue |
| CN106954773A (en) * | 2017-03-31 | 2017-07-18 | 中国农业大学 | A kind of processing method of mulberry juice comprehensive utilization |
| CN110105320A (en) * | 2019-05-08 | 2019-08-09 | 湖南华诚生物资源股份有限公司 | From salvia chinensis potato simultaneously separating starch, anthocyanidin and total polyphenols method |
| CN110240584A (en) * | 2019-05-29 | 2019-09-17 | 湖南华诚生物资源股份有限公司 | The method for separating procyanidine, anthocyanidin and ferulic acid simultaneously from purple rice rice bran |
| CN110981921A (en) * | 2019-12-26 | 2020-04-10 | 湖南华诚生物资源股份有限公司 | Continuous method for synchronously extracting multiple effective components from figs |
| CN111533723A (en) * | 2020-05-29 | 2020-08-14 | 禹州市合同泰药业有限公司 | Method for extracting anthocyanin from mature fresh fruits of edible fungus vegetables |
Non-Patent Citations (3)
| Title |
|---|
| 万正中: "果桑优质高产栽培技术", 《广东蚕业》 * |
| 李俊芳 等: "不同果桑品种成熟桑椹的游离氨基酸主成分分析和综合评价", 《食品科学》 * |
| 李柏榆: "超声辅助提取桑葚多酚及抗氧化活性分析", 《云南民族大学学报: 自然科学版》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105949163B (en) | The method for extraction and purification of anthocyanidin in a kind of Black Box Tracing pomace | |
| CN101912480B (en) | Method for preparing procyanidin extract of lycium ruthenicum murr | |
| CN102732050A (en) | Method for preparing gardenia pigments from Gardenia jasminoides Ellis | |
| CN110746515B (en) | Lycium barbarum polysaccharide, lycium barbarum red element and lycium barbarum polypeptide prepared by synchronous separation and preparation method thereof | |
| CN108186456B (en) | Preparation method of phyllanthus emblica extract for removing freckles and whitening skin | |
| CN111333600A (en) | Method for extracting vitamin C from kiwi fruits | |
| CN103238892A (en) | Production method of smallanthus sonchifolius normal juice and normal juice powder | |
| CN111588043B (en) | Preparation method of dietary fiber based on Siraitia grosvenorii waste | |
| CN110981921B (en) | Continuous method for synchronously extracting multiple effective components from figs | |
| CN107114643A (en) | Jujube health inspissated juice and preparation method thereof | |
| US10968470B2 (en) | Method for preparing rubusoside | |
| CN103880806A (en) | Method for extracting anthocyanin from blueberry | |
| CN106046848A (en) | Method for extracting and purifying anthocyanin from mulberry pomace | |
| JP6944069B2 (en) | How to extract lycopene and citrulline from watermelon at the same time | |
| CN101480216A (en) | Method for extracting composite aminoacid from water melon or black seed melon | |
| CN110777173B (en) | Method for preparing momordica grosvenori amino acid by using momordica grosvenori centrifugal waste residues | |
| CN116332822A (en) | Method for preparing low-chroma 5-hydroxytryptophan from garna seeds | |
| CN112314945A (en) | Method for preparing high-activity cranberry extract by sectional extraction method | |
| CN110669035A (en) | Method for preparing anthocyanin from indigo fruit | |
| CN110679934A (en) | Lutein-containing enzyme capable of clearing liver and improving eyesight and preparation method thereof | |
| CN110938054A (en) | Method for preparing indigo fruit anthocyanin from indigo fruit | |
| CN113397169A (en) | Method for continuously extracting and separating multiple natural active ingredients from mulberries | |
| CN106177555B (en) | A method of extracting sugarcane polyphenol from sugarcane dross | |
| CN112707881B (en) | Preparation method of blueberry anthocyanin | |
| CN112043733B (en) | Production method of water-soluble ginkgo leaf extract |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210917 |
|
| RJ01 | Rejection of invention patent application after publication |