CN109678981A - A kind of preparation method of safflower polysaccharide, product and application - Google Patents
A kind of preparation method of safflower polysaccharide, product and application Download PDFInfo
- Publication number
- CN109678981A CN109678981A CN201811547397.0A CN201811547397A CN109678981A CN 109678981 A CN109678981 A CN 109678981A CN 201811547397 A CN201811547397 A CN 201811547397A CN 109678981 A CN109678981 A CN 109678981A
- Authority
- CN
- China
- Prior art keywords
- safflower
- safflower polysaccharide
- preparation
- polysaccharide
- sephadex
- Prior art date
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- Granted
Links
- 235000003255 Carthamus tinctorius Nutrition 0.000 title claims abstract description 102
- 244000020518 Carthamus tinctorius Species 0.000 title claims abstract description 102
- 150000004676 glycans Chemical class 0.000 title claims abstract description 93
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 93
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 93
- 238000002360 preparation method Methods 0.000 title claims description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000011347 resin Substances 0.000 claims abstract description 28
- 229920005989 resin Polymers 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000000047 product Substances 0.000 claims abstract description 19
- 229920005654 Sephadex Polymers 0.000 claims abstract description 18
- 239000012507 Sephadex™ Substances 0.000 claims abstract description 18
- 239000003814 drug Substances 0.000 claims abstract description 10
- 238000010257 thawing Methods 0.000 claims abstract description 10
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 claims abstract description 9
- 229940079593 drug Drugs 0.000 claims abstract description 9
- 238000001556 precipitation Methods 0.000 claims abstract description 9
- 230000002596 correlated effect Effects 0.000 claims abstract description 8
- 201000010099 disease Diseases 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 239000012141 concentrate Substances 0.000 claims abstract description 5
- 238000005119 centrifugation Methods 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 23
- 238000001179 sorption measurement Methods 0.000 claims description 10
- 239000002250 absorbent Substances 0.000 claims description 9
- 230000002745 absorbent Effects 0.000 claims description 9
- 239000003480 eluent Substances 0.000 claims description 9
- 238000000605 extraction Methods 0.000 claims description 7
- 239000012528 membrane Substances 0.000 claims description 7
- 239000000284 extract Substances 0.000 claims description 5
- 230000036541 health Effects 0.000 claims description 5
- XELZGAJCZANUQH-UHFFFAOYSA-N methyl 1-acetylthieno[3,2-c]pyrazole-5-carboxylate Chemical compound CC(=O)N1N=CC2=C1C=C(C(=O)OC)S2 XELZGAJCZANUQH-UHFFFAOYSA-N 0.000 claims description 5
- 238000001471 micro-filtration Methods 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 239000011343 solid material Substances 0.000 claims description 4
- 239000003937 drug carrier Substances 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 3
- 239000012264 purified product Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 2
- 229930003935 flavonoid Natural products 0.000 claims description 2
- 150000002215 flavonoids Chemical class 0.000 claims description 2
- 235000017173 flavonoids Nutrition 0.000 claims description 2
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 20
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 229930003944 flavone Natural products 0.000 abstract description 4
- 235000011949 flavones Nutrition 0.000 abstract description 4
- 238000005259 measurement Methods 0.000 abstract description 4
- 238000004062 sedimentation Methods 0.000 abstract description 4
- 238000002798 spectrophotometry method Methods 0.000 abstract description 4
- 206010028980 Neoplasm Diseases 0.000 abstract description 3
- 201000011510 cancer Diseases 0.000 abstract description 3
- 239000002955 immunomodulating agent Substances 0.000 abstract description 3
- 230000002584 immunomodulator Effects 0.000 abstract description 3
- 229940121354 immunomodulator Drugs 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- DYQVDISPPLTLLR-HJQYTNQXSA-N Carthamin Natural products CC[C@H]1O[C@H]([C@H](O)[C@@H](O)[C@@H]1O)[C@]2(O)C(=C(C=C/3C(=O)C(=C(O)[C@](O)([C@@H]4O[C@H](CO)[C@@H](O)[C@H](O)[C@H]4O)C3=O)C(=O)C=Cc5ccc(O)cc5)C(=O)C(=C2O)C(=O)C=Cc6ccc(O)cc6)O DYQVDISPPLTLLR-HJQYTNQXSA-N 0.000 abstract description 2
- WLYGSPLCNKYESI-RSUQVHIMSA-N Carthamin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1[C@@]1(O)C(O)=C(C(=O)\C=C\C=2C=CC(O)=CC=2)C(=O)C(\C=C\2C([C@](O)([C@H]3[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O3)O)C(O)=C(C(=O)\C=C\C=3C=CC(O)=CC=3)C/2=O)=O)=C1O WLYGSPLCNKYESI-RSUQVHIMSA-N 0.000 abstract description 2
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 abstract description 2
- 235000009508 confectionery Nutrition 0.000 abstract description 2
- 150000002212 flavone derivatives Chemical class 0.000 abstract description 2
- 235000013402 health food Nutrition 0.000 abstract description 2
- 230000036039 immunity Effects 0.000 abstract description 2
- 239000000843 powder Substances 0.000 abstract description 2
- 239000001117 sulphuric acid Substances 0.000 abstract description 2
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002244 precipitate Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 16
- 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 15
- 235000019441 ethanol Nutrition 0.000 description 15
- 239000008103 glucose Substances 0.000 description 13
- -1 alkaloid compound Chemical class 0.000 description 11
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 description 9
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- SHZGCJCMOBCMKK-UHFFFAOYSA-N D-mannomethylose Natural products CC1OC(O)C(O)C(O)C1O SHZGCJCMOBCMKK-UHFFFAOYSA-N 0.000 description 6
- 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
- PNNNRSAQSRJVSB-UHFFFAOYSA-N L-rhamnose Natural products CC(O)C(O)C(O)C(O)C=O PNNNRSAQSRJVSB-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 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 6
- 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 6
- 210000004027 cell Anatomy 0.000 description 6
- 239000012153 distilled water Substances 0.000 description 6
- 229960004756 ethanol Drugs 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 5
- 238000000746 purification Methods 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 150000002772 monosaccharides Chemical class 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 229910021642 ultra pure water Inorganic materials 0.000 description 4
- 239000012498 ultrapure water Substances 0.000 description 4
- 238000009777 vacuum freeze-drying Methods 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- SHZGCJCMOBCMKK-JFNONXLTSA-N L-rhamnopyranose Chemical compound C[C@@H]1OC(O)[C@H](O)[C@H](O)[C@H]1O SHZGCJCMOBCMKK-JFNONXLTSA-N 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 235000013824 polyphenols Nutrition 0.000 description 3
- OIGNJSKKLXVSLS-VWUMJDOOSA-N prednisolone Chemical compound O=C1C=C[C@]2(C)[C@H]3[C@@H](O)C[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 OIGNJSKKLXVSLS-VWUMJDOOSA-N 0.000 description 3
- 229960005205 prednisolone Drugs 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 206010070834 Sensitisation Diseases 0.000 description 2
- 210000001744 T-lymphocyte Anatomy 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- WFDIJRYMOXRFFG-UHFFFAOYSA-N acetic acid anhydride Natural products CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000001476 alcoholic effect Effects 0.000 description 2
- 239000012491 analyte Substances 0.000 description 2
- 210000003719 b-lymphocyte Anatomy 0.000 description 2
- 238000010828 elution Methods 0.000 description 2
- 150000002213 flavones Chemical class 0.000 description 2
- 230000001900 immune effect Effects 0.000 description 2
- 230000001506 immunosuppresive effect Effects 0.000 description 2
- 230000001939 inductive effect Effects 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 230000000144 pharmacologic effect Effects 0.000 description 2
- 150000008442 polyphenolic compounds Chemical class 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000013558 reference substance Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 230000008313 sensitization Effects 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 1
- 241000208838 Asteraceae Species 0.000 description 1
- 241001061264 Astragalus Species 0.000 description 1
- 206010006187 Breast cancer Diseases 0.000 description 1
- 208000026310 Breast neoplasm Diseases 0.000 description 1
- 102000004127 Cytokines Human genes 0.000 description 1
- 108090000695 Cytokines Proteins 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- 229920001503 Glucan Polymers 0.000 description 1
- 102000014150 Interferons Human genes 0.000 description 1
- 108010050904 Interferons Proteins 0.000 description 1
- 206010058467 Lung neoplasm malignant Diseases 0.000 description 1
- 241001494479 Pecora Species 0.000 description 1
- 206010039491 Sarcoma Diseases 0.000 description 1
- 208000005718 Stomach Neoplasms Diseases 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 230000021736 acetylation Effects 0.000 description 1
- 238000006640 acetylation reaction Methods 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 description 1
- GZCGUPFRVQAUEE-KVTDHHQDSA-N aldehydo-D-mannose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)C=O GZCGUPFRVQAUEE-KVTDHHQDSA-N 0.000 description 1
- PYMYPHUHKUWMLA-VPENINKCSA-N aldehydo-D-xylose Chemical compound OC[C@@H](O)[C@H](O)[C@@H](O)C=O PYMYPHUHKUWMLA-VPENINKCSA-N 0.000 description 1
- PNNNRSAQSRJVSB-BXKVDMCESA-N aldehydo-L-rhamnose Chemical compound C[C@H](O)[C@H](O)[C@@H](O)[C@@H](O)C=O PNNNRSAQSRJVSB-BXKVDMCESA-N 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 150000004056 anthraquinones Chemical class 0.000 description 1
- 230000001093 anti-cancer Effects 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
- 238000003556 assay Methods 0.000 description 1
- 235000006533 astragalus Nutrition 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 201000008275 breast carcinoma Diseases 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000000875 corresponding effect Effects 0.000 description 1
- 125000004093 cyano group Chemical group *C#N 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000003292 diminished effect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000002124 endocrine Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 235000013355 food flavoring agent Nutrition 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 206010017758 gastric cancer Diseases 0.000 description 1
- 238000005227 gel permeation chromatography Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 230000036737 immune function Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229940079322 interferon Drugs 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 201000007270 liver cancer Diseases 0.000 description 1
- 208000014018 liver neoplasm Diseases 0.000 description 1
- 201000005296 lung carcinoma Diseases 0.000 description 1
- 210000004698 lymphocyte Anatomy 0.000 description 1
- 230000004089 microcirculation Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- OQUKIQWCVTZJAF-UHFFFAOYSA-N phenol;sulfuric acid Chemical compound OS(O)(=O)=O.OC1=CC=CC=C1 OQUKIQWCVTZJAF-UHFFFAOYSA-N 0.000 description 1
- 230000001766 physiological effect Effects 0.000 description 1
- 239000000419 plant extract Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000001542 size-exclusion chromatography Methods 0.000 description 1
- 210000004988 splenocyte Anatomy 0.000 description 1
- 201000011549 stomach cancer Diseases 0.000 description 1
- 150000005846 sugar alcohols Chemical class 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 210000004233 talus Anatomy 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
-
- 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
- A23L33/125—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives containing carbohydrate syrups; containing sugars; containing sugar alcohols; containing starch hydrolysates
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/70—Carbohydrates; Sugars; Derivatives thereof
- A61K31/715—Polysaccharides, i.e. having more than five saccharide radicals attached to each other by glycosidic linkages; Derivatives thereof, e.g. ethers, esters
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P35/00—Antineoplastic agents
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P37/00—Drugs for immunological or allergic disorders
- A61P37/02—Immunomodulators
-
- 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
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Medicinal Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Veterinary Medicine (AREA)
- Animal Behavior & Ethology (AREA)
- Pharmacology & Pharmacy (AREA)
- Public Health (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- General Chemical & Material Sciences (AREA)
- Immunology (AREA)
- Polymers & Plastics (AREA)
- Nutrition Science (AREA)
- Materials Engineering (AREA)
- Biochemistry (AREA)
- Sustainable Development (AREA)
- Food Science & Technology (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Mycology (AREA)
- Epidemiology (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a kind of methods for preparing safflower polysaccharide, product and application thereof, method is the following steps are included: safflower is extracted through hot water, low temperature sedimentation, filtering, polar macroporous resin removes general flavone and carthamin, and Thick many candies concentrate low temperature alcohol precipitation precipitates the freeze thawing that is dissolved in water, centrifugation, high-content safflower polysaccharide is obtained through sephadex purifies and separates again, is finally freeze-dried to obtain white powder.It is 85.0%~99.8% with ultraviolet spectrophotometry (phend-sulphuric acid) measurement polyoses content.Present invention process is simple, easily operated, is suitble to industrialized production, gained safflower polysaccharide content is high, it can be developed into drug and health food, immune correlated disease treatment be used for as immunomodulator, also can be used for improving sub-health population and receive the immunity of chemicotherapy cancer patient.
Description
Technical field
The invention belongs to technical field of natural product extraction more particularly to a kind of method for preparing safflower polysaccharide, product and
The purposes of the safflower polysaccharide.
Background technique
Safflower is the dry tubular flower of compositae plant safflower, and property is pungent, warm, has activating microcirculation and removing stasis medicinal, and inducing meastruation to relieve menalgia effect is faced
Bed is very widely used.Safflower complex chemical composition mainly contains carthamin yellow, safflower polysaccharide, flavones, organic acid, safflower
Haematochrome, polyphenol, amino acid etc.." new safflower 7 " is the medicinal white safflower of few thorn of industrial crops institute, Xinjiang academy of agricultural sciences breeding
New varieties, the kind safflower polysaccharide and general flavone content are the several times of common safflower or more.The study found that safflower polysaccharide has
The pharmacological actions such as anti-oxidant, immunological regulation, anticancer, to mouse sarcoma S180cell, mouse LA795 lung carcinoma cell, human liver cancer
SMMC-7721 cell, human breast carcinoma MC-7 cell, Human gastric cancer SGC-7901 cells have good inhibiting effect [new referring to horse
Rich " Chongqing Medical " the 3rd phase " safflower polysaccharide extraction process and suppression cancer Advance on Pharmacological Activities " of volume 43 in 2014].
Currently, the method for extracting safflower polysaccharide mostly uses greatly water extraction and alcohol precipitation method to obtain Thick many candies, then removed using Sevage method
Albumen, hydrogen peroxide decoloration, acetone and ether the serial of methods such as repeatedly wash, dry and being purified, and obtain safflower polysaccharide.It should
Purification process there are complex process, organic reagent type consume more it is big and mostly inflammable and explosive substances, high production cost, can not be suitble to
The shortcoming such as industrialized production, obtained safflower polysaccharide are multicomponent mixture, and color is in yellowish-brown, and content is lower, organic solvent
Residual is high.Therefore, the drug or health care product that there is no the fine work safflower polysaccharide based on high-content to prepare at present.
Summary of the invention
To overcome problem above, the present invention provides a kind of method (or extracting method) for preparing safflower polysaccharide, this method
Advantages of simple, environmentally protective, operation is continuous high-efficient, and production cost is low, and obtained product composition is uniform, and content is high, and raw material
It is resourceful, it is suitable for industrialized production.
The present invention also provides a kind of products of safflower polysaccharide prepared by the above method, and the product composition is uniform,
Content is high, no solvent residue.
The present invention additionally provides simultaneously a kind of to be controlled by what above-mentioned safflower polysaccharide product was prepared for immune correlated disease
The drug and health care product for the treatment of.
A kind of preparation method of safflower polysaccharide, includes the following steps:
(1) safflower is placed in extractant, soak extraction obtains extracting solution；
(2) obtained extracting solution is removed flavonoids impurity and decolourized, collection penetrates by macroporous resin adsorption
Liquid；
(3) liquid concentration will be penetrated, alcohol is added into concentrate, stands alcohol precipitation, separation of solid and liquid obtains solid material；
(4) it is dissolved in water into obtained solid material, low temperature carries out lower freeze thawing centrifugation；
(5) control centrifugate concentration is isolated and purified within the scope of 200mg/mL~600mg/mL with sephadex,
Obtain safflower polysaccharide purified product.
In the preferred embodiment of preparation method of the invention, in step (1), the extractant is water, further excellent
It is selected as ultrapure water, 0~50% methanol-water (i.e. wherein the concentration of volume percent of methanol is 0~50%), 0~50% ethanol water.
Extracting temperature is controlled at 60 DEG C~100 DEG C, is extracted 2~3 times, 0.5~12 hour every time, amount of water was the 10~30 of crude drug weight
Times；After the completion of extraction, combined extract, in 2 DEG C~15 DEG C sedimentations, 4~24 hours removing insoluble impurities, then through liquid cross-flow
Membrane microfiltration system refined filtration, obtains final extracting solution.
In the preferred embodiment of preparation method of the invention, the macroreticular resin non-polar absorbent macroreticular resin (ratio
Such as X-5 non-polar absorbent macroreticular resin, H103 non-polar absorbent macroreticular resin, HPD100 non-polar absorbent macroreticular resin), in
Isopolarity macroporous absorbent resin (such as HPD400 macroporous absorbent resin, ADS-8 macroporous absorbent resin, ADS-17 macroporous absorption tree
Rouge etc.), polar macroporous adsorption resin.More preferably polar macroporous adsorption resin, the polar macroporous adsorption resin, which refers to, to be contained
Amide groups, cyano, phenolic hydroxyl group etc. be nitrogenous, the absorption resin of oxygen, sulphur polar functionalities base, and including but not limited to NKA-2 is polar macroporous
Adsorb one of resin, NKA-9 polar resin, S-8 polar macroporous adsorption resin, HPD600 polar macroporous adsorption resin etc. or
It is a variety of.Or other are suitable for isolated resin (such as the Shanghai Xun Erization of flavones, Polyphenols, Anthraquinones, alkaloid compound
The plant extract of model XR981, H01S, H06S, XR920D of the sale of work Science and Technology Ltd. are resin dedicated)
In the preferred embodiment of preparation method of the invention, in step (3), will penetrate that liquid is concentrated into original volume 1/
4~1/40；The mass percent concentration that concentrate adds alcohol to system alcohol is 75%~95%, latter 2 DEG C~8 DEG C standing alcohol precipitations 1~
18 hours.The separation of solid and liquid can filter, filter, be filtered under diminished pressure etc. modes using room temperature.In the step, it is separated by solid-liquid separation
The liquids recovery arrived alcoholic solvent therein, or can also be recycled directly as alcoholic solvent.
In the preferred embodiment of preparation method of the invention, it is to receive that liquid method for concentration is penetrated described in step (3)
Filter membrane concentration, scraper plate concentration, the concentration of mechanical steam recompression technology (MVR) low temperature, more preferably MVR low temperature are concentrated.It is dense
Alcohol added by contracting liquid is high concentration methanol, ethyl alcohol and other alcohol, more preferably 95% ethyl alcohol or dehydrated alcohol.
In the preferred embodiment of preparation method of the invention, in step (4), freeze thawing temperature is -30 DEG C~0 DEG C, more
Preferably -20 DEG C, the freeze thawing time is 2~48 hours, more preferably 12~24 hours.Centrifugal condition is preferred are as follows: revolving speed is high
In 4000r/pm, time 25min or more.
In the preferred embodiment of preparation method of the invention, centrifugate concentration described in step 5) is 200mg/mL
~600mg/mL, more preferably 300mg/mL~400mg/mL.Preferably, when being isolated and purified with sephadex, on
Sample volume accounts for the 2%~30% of gel column volume, more preferably 10%~20%, and eluent is water.
In the preferred embodiment of preparation method of the invention, sephadex be preferably Sephadex LH-20,
Sephadex G25,Sephadex G50,Sephadex G75.More preferably Sephadex LH-20, Sephadex G50,
Gel column ratio of height to diameter is 2:1~6:1.Eluent is preferably ultrapure water.
After purification by sephadex, eluent is collected, concentrated, vacuum freeze drying obtains purification safflower polysaccharide,
For white powder.It is 85.0%~99.8% with ultraviolet spectrophotometry (phend-sulphuric acid) measurement polyoses content.
In the present invention, the safflower is composite family safflower or new varieties white safflower, more preferably white safflower.Using
It when white safflower is raw material, is monitored by electric conductivity detector and UV detector, can collect 2 fraction eluents, concentrated,
Vacuum freeze drying, the safflower polysaccharide purified product of available two kinds of one-components: safflower polysaccharide A and safflower polysaccharide B, safflower
The content of polysaccharide is 90% or more.
The preparation method of a kind of safflower polysaccharide, the safflower polysaccharide as described in any of the above-described technical solution is prepared.
Preferably, including safflower polysaccharide A and safflower polysaccharide B in the safflower polysaccharide, two mass ratioes are 1:1~2；
Further preferably 1:1.4~1.6.
Preferably, the relative molecular mass of safflower polysaccharide A is 8000~10000, the relative molecular mass of safflower polysaccharide B
It is 4000~6000.Further preferably the relative molecular mass of safflower polysaccharide A is 9400 or so, opposite point of safflower polysaccharide B
Protonatomic mass is 5900 or so.
Preferably, safflower polysaccharide A is by 6 kinds of rhamnose, arabinose, glucose, galactolipin, xylose, mannose monosaccharide
One of or a variety of compositions；As further preferred, the safflower polysaccharide A is by rhamnose, arabinose, glucose, gala
6 kinds of sugar, xylose, mannose monosaccharide are formed with beta chain connection；Preferably, safflower polysaccharide B is by arabinose, glucose, gala
One of 4 kinds of sugar, rhamnose monosaccharide or a variety of compositions；As further preferred, the safflower polysaccharide B is by arabinose, Portugal
4 kinds of grape sugar, galactolipin, rhamnose monosaccharide are formed with beta chain connection.
A kind of drug and health care product for immune correlated disease treatment, containing treating or preventing, immune correlated disease is effective
Safflower polysaccharide described in claims 1 of amount and combinations thereof and pharmaceutical carrier.The pharmaceutical carrier include but
It is not limited to auxiliary agent, adjuvant, moulding agent, flavoring agent etc..
Drug and health care product for immune correlated disease treatment of the invention can be made into oral preparation, ejection preparation.
Safflower polysaccharide prepared by the present invention has following function:
Turn experiment from external leaching and show that safflower polysaccharide and T cell mitogenesis original ConA have synergistic effect, to B cell
Mitogenesis original has no significant effect.But internal PFC test, safflower polysaccharide act on the astragalus polyose of B cell with being generally acknowledged that
Effect trend is consistent.Different to the time of mouse injection safflower polysaccharide, the variation of mouse PFC value is also different: administration group after sensitization
PFC be promoted, and the PFC of administration group is counter before sensitization is suppressed.Show that safflower polysaccharide also shows that the two-way of immune drug
Property.Safflower polysaccharide can obviously fight the immunosuppressive action of prednisolone, it inhibits the Immune-enhancing effect of mouse to make prednisolone
With relatively being become apparent to the effect of normal mouse.Therefore, safflower polysaccharide can promote lymphocyte transformation, and it is red to sheep to increase splenocyte
The cell number of cell plaque test fights the immunosuppressive action etc. of prednisolone.Safflower polysaccharide constituents can pass through " lFN-
LL-NKC " network, inductive formation interferon, by adjusting cytokine network, T cell network, organism endocrine immunological network,
To enhance the immune function of body.Therefore, safflower polysaccharide can be used as immunomodulator and be used for immune correlated disease treatment.
The invention has the following advantages:
Present invention process is simple, easily operated, is suitble to industrialized production, and gained safflower polysaccharide content is high, can be developed into medicine
Product and health food are used for immune correlated disease treatment as immunomodulator, also can be used for improving sub-health population and connect
By the immunity of chemicotherapy cancer patient.
The present invention can use medicinal white safflower new varieties " new safflower 7 " for raw material, and the variety source is abundant, and red
Flower polyoses content is the several times of common safflower or more, ensure that the purity and entirety yield of final products from source.
Preparation method provided by the invention use extensive membrane microfiltration, the absorption of macroreticular resin specificity and directional separation,
The efficient isolation and purification methods such as sephadex purification, products obtained therefrom safflower polysaccharide content are 85.0%~99.8%, are ensured
The disadvantages of curative effect of product, reproducibility is good, overcomes low prior art safflower polysaccharide recovery rate, poor reproducibility, it is important
It is easy to carry and use, and activity is better than safflower decocting liquid.
Present invention employs the preparation processes such as the concentration of low energy consumption MVR low temperature, alcohol precipitation freeze thawing, freeze-drying, avoid existing
Effective component structure change caused by technology high temperature condition, loss and the reduction of physiological activity, products obtained therefrom quality are stablized,
It is easy to be mass produced.
Specific embodiment
In order to keep objects and advantages of the present invention more explicit, the present invention is carried out with reference to embodiments further
It illustrates.It should be understood that the specific embodiments described herein are merely illustrative of the present invention, the protection being not intended to restrict the invention
Range.
Safflower polysaccharide assay uses Phenol sulfuric acid procedure, is first hydrolyzed into monosaccharide under the action of sulfuric acid using polysaccharide, and
Rapid dehydration generates alditol derivative, then generates orange-yellow compound with phenol.
A) preparation of glucose standards solution:
The preparation of glucose standards solution: precision weighs 105 DEG C of dryings to the DEXTROSE ANHYDROUS 10.71mg of constant weight, is placed in
In 100mL measuring bottle, scale is settled to distilled water, is configured to the stock solution of 107.1 μ g/mL.It is accurate from stock solution to draw
0.1,0.2,0.4,0.6,0.8,1.0mL glucose solution is added on respectively in the tool plug test tube of 20mL, and adds distilled water to mend respectively
To 2.0mL, it is configured to Glucose standards serial solution.2.0mL distilled water is taken to return to zero as blank.
B) drafting of standard curve
5% phenol solution 1.0mL is added into Glucose standards serial solution and distilled water, mixes, then rapidly along pipe
The 5.0mL concentrated sulfuric acid is added in wall, shakes up, and seals, and boiling water bath heats 15min, room temperature is rapidly cooled in ice-water bath, in absorption maximum
Absorbance is measured at wavelength 490nm, with absorbance (A) for ordinate, is with glucose standards solution mass concentration (C, μ g/mL)
Abscissa draws standard curve, and obtaining regression equation is y=0.0134x-0.0113, R2=0.9992.
C) measurement of the polysaccharide content in sample
Precision weighs refined polysaccharide 10mg, and constant volume shakes up to obtain sample liquid in 10mL measuring bottle.Above-mentioned solution is drawn again
2.0mL is settled to 20mL.Analyte sample fluid 1.0mL is drawn, distilled water is mended to 2mL, surveys its suction by method prepared by standard curve
Shading value substitutes into regression equation, obtains glucose mass concentration (μ g/mL).The mass fraction of polysaccharide is calculated as follows:
Glucose mass concentration × extension rate ÷ sample quality in mass fraction of polysaccharide %=polysaccharide
Embodiment 1:
The water of 10 times of weight is added in extracting waste safflower 500g, and 60 DEG C of stirrings are lower to impregnate 2h, filtration, the dregs of a decoction 8 times of weight of addition
Water, 60 DEG C of stirrings are lower to impregnate 1h, filters out the dregs of a decoction, combined extract about 8.1L.5 DEG C of sedimentation 6h of extracting solution, take supernatant through liquid
The filtering of body cross-flow membrane microfiltration systems.Filtrate flows through polar macroporous adsorption resin (column volume the 1200mL) (Shanghai XR920D Xun Erization
Work Science and Technology Ltd.), it collects safflower polysaccharide and penetrates liquid about 8.6L (eluant, eluent is water).It is concentrated (using MVR low temperature to penetrate liquid
Concentration) to about 300mL, 95% ethyl alcohol 3000mL, 4 DEG C of sealing and standing 12h are added with stirring, suction filtration obtains safflower polysaccharide precipitating
88.2g filtrate recycling ethanol.Polysaccharide precipitation add 220mL water dissolve, -20 DEG C freeze thawing 12 hours, be centrifuged off albumen (revolving speed
4500r/pm, time 30min).It is pure to cross Sephadex LH-20 sephadex in 400mg/mL or so for the control of centrifugate concentration
To change (loading volume account for gel column volume 10%), gel column ratio of height to diameter is 4:1, elution safflower polysaccharide component is taken water as a solvent,
2 different fractions eluents are collected (to detect by electric conductivity detector and UV detector, collect the red of two different components respectively
Flower polysaccharide), concentrated, vacuum freeze drying must refine safflower polysaccharide A12.1g and safflower polysaccharide B 18.0g, total recovery respectively
It is 6.02%.It is measured with spectrophotometry, content is respectively 93.60% and 92.75%.
Embodiment 2:
The water of 12 times of weight is added in extracting waste safflower 500g, and 100 DEG C of stirrings are lower to impregnate 2h, filtration, the dregs of a decoction 10 times of weights of addition
The water of amount, 100 DEG C of stirrings are lower to impregnate 1h, filters out the dregs of a decoction, combined extract about 10.5L.5 DEG C of sedimentation 6h of extracting solution, take supernatant
It is filtered through liquid cross-flow membrane microfiltration systems.Filtrate flows through polar macroporous adsorption resin (column volume 1200mL), and (Shanghai XR920D is inferior
That Chemical Industry Science Co., Ltd) (eluant, eluent is water), it collects safflower polysaccharide and penetrates liquid about 11L.It is concentrated (using MVR to penetrate liquid
Low temperature concentration) to about 400mL, 95% ethyl alcohol 4000mL, 4 DEG C of sealing and standing 16h are added with stirring, it is heavy that suction filtration obtains safflower polysaccharide
Shallow lake 96.5g, filtrate recycling ethanol.Polysaccharide precipitation add 300mL water dissolve, -10 DEG C freeze thawing 24 hours, be centrifuged off albumen (revolving speed
5000r/pm, time 30min).It is pure to cross Sephadex LH-20 sephadex in 300mg/mL or so for the control of centrifugate concentration
To change (loading volume account for gel column volume 20%), gel column ratio of height to diameter is 5:1, elution safflower polysaccharide component is taken water as a solvent,
2 different fractions eluents are collected (to detect by electric conductivity detector and UV detector, collect the red of two different components respectively
Flower polysaccharide), concentrated, vacuum freeze drying must refine safflower polysaccharide A13.5g and safflower polysaccharide B 20.3g, total recovery respectively
It is 6.76%.It is measured with spectrophotometry, content is respectively 91.92% and 91.39%.
Safflower polysaccharide A and the detection of safflower polysaccharide B structure:
Gel permeation chromatography (size exclusion chromatography) method measures its relative molecular mass:
1, chromatographic condition chromatographic column: TSK-GELG4000PWXLColumn (300mm × 7.8mm, 10 μm)；Mobile phase: ultrapure water；
Column temperature: 30 DEG C；Detector: differential refraction detector (RID), 30 DEG C of detector temperature；Flow velocity: 0.5mLmin-1；Sample introduction body
Product: 10 μ L.
2, the production of standard curve takes the glucan pair of known relative molecular mass (relative molecular weight is 2000~50000)
According to product, respectively plus ultrapure water is made solution of every 1mL containing 1mg, cross 0.45 μm of miillpore filter to get.With reference substance molecular weight
(MW) standard curve is made in the retention time (tR) of logarithm corresponding thereto.
3, safflower polysaccharide is made into 1mgmL with distilled water by the measurement of molecular weight analyte respectively-1Solution, cross 0.45 μm it is micro-
Hole filter membrane, sample introduction is analyzed under chromatographic condition, records retention time, substitutes into the relative molecular mass that regression equation seeks each component.
As a result the relative molecular mass of safflower polysaccharide A is 9400 or so, and the relative molecular mass of safflower polysaccharide B is 5900 or so.
Derivative GC method is formed to its monosaccharide and structure parses:
1, chromatographic condition chromatographic column: HP-5 (30m × 0.32mm)；Temperature programming:
100℃(5℃·min-1)→190℃(4℃·min-1)→240℃(5min)；Carrier gas: high pure nitrogen；Sample injector
Temperature: 260 DEG C；Input mode: it shunts；Detector: FID；Injector temperature: 250 DEG C.
2, the preparation of the sugared nitrile acetic ester derivative of monosaccharide reference substance and Polysaccharides accurately weigh L- rhamnose, L- I
Uncle's sugar, D- xylose, D-MANNOSE, D-Glucose, 6 kinds of standard monosaccharide of D- galactolipin and 2 kinds of polysaccharide sample 10mg hydrolyzed, respectively
It is put into tool plug test tube, hydroxylamine hydrochloride 10mg and internal standard 7mg is added, anhydrous pyridine lmL is added, is put into 90 DEG C of water-baths and heats
30min simultaneously vibrates, and room temperature is cooled to after taking-up, and acetic anhydride acid anhydride lmL is added, and the reaction was continued at 90 DEG C, and 30min carries out acetylation,
Sample introduction after chloroform extraction.
As the result is shown safflower polysaccharide A by 6 kinds of rhamnose, arabinose, glucose, galactolipin, xylose, mannose monosaccharide with
Beta chain connection composition；Safflower polysaccharide B is made of 4 kinds of arabinose, glucose, galactolipin, rhamnose monosaccharide with beta chain connection.
Claims (10)
1. a kind of preparation method of safflower polysaccharide, which comprises the steps of:
(1) safflower is placed in extractant, soak extraction obtains extracting solution；
(2) obtained extracting solution is removed flavonoids impurity and decolourized, collection penetrates liquid by macroporous resin adsorption；
(3) liquid concentration will be penetrated, alcohol is added into concentrate, stands alcohol precipitation, separation of solid and liquid obtains solid material；
(4) it is dissolved in water into obtained solid material, low temperature carries out lower freeze thawing centrifugation；
(5) control centrifugate concentration is isolated and purified with sephadex, is obtained within the scope of 200mg/mL~600mg/mL
Safflower polysaccharide purified product.
2. the preparation method of safflower polysaccharide according to claim 1, which is characterized in that in step (1), the extractant is
Water, 0~50% methanol-water, 0~50% ethanol water, Extracting temperature are controlled at 60 DEG C~100 DEG C, extract 2~3 times, every time 0.5~
12 hours, amount of water was 10~30 times of crude drug weight；After the completion of extraction, combined extract settles 4~24 in 2 DEG C~15 DEG C
Hour removes insoluble impurities, then through liquid cross-flow membrane microfiltration systems refined filtration, obtains final extracting solution.
3. the preparation method of safflower polysaccharide according to claim 1, which is characterized in that the macroreticular resin non-polar absorbent
Macroreticular resin, middle polarity macroporous absorbent resin, polar macroporous adsorption resin.
4. the preparation method of safflower polysaccharide according to claim 1, which is characterized in that in step (3), liquid concentration will be penetrated
To the 1/4~1/40 of original volume；Concentrate add alcohol to system alcohol mass percent concentration be 75%~95%, latter 2 DEG C~8 DEG C
Stand alcohol precipitation 1~18 hour.
5. the preparation method of safflower polysaccharide according to claim 1, which is characterized in that in step (4), freeze thawing temperature be-
30 DEG C~0 DEG C, the freeze thawing time is 2~48 hours, centrifugal condition are as follows: revolving speed is higher than 4000r/pm, time 25min or more.
6. the preparation method of safflower polysaccharide according to claim 1, which is characterized in that separate with sephadex pure
When change, loading volume accounts for the 2%~30% of gel column volume, and eluent is water.
7. the preparation method of safflower polysaccharide according to claim 1 or 6, which is characterized in that the sephadex is
One of Sephadex LH-20, Sephadex G25, Sephadex G50, Sephadex G75 or a variety of.
8. the preparation method of safflower polysaccharide according to claim 7, which is characterized in that the gel column ratio of height to diameter is 2:1
~6:1.
9. a kind of safflower polysaccharide, which is characterized in that prepared by the preparation method of any one of claim 1~8 safflower polysaccharide
It obtains.
10. a kind of drug and health care product for immune correlated disease treatment, which is characterized in that phase is immunized containing treating or preventing
Safflower polysaccharide described in a effective amount of claims 1 of related disorders and combinations thereof and pharmaceutical carrier.
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| CN115120529A (en) * | 2022-06-17 | 2022-09-30 | 山东农业大学 | Red sage root and safflower composite polysaccharide and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS53126089A (en) * | 1977-04-11 | 1978-11-02 | Akiyama Jiyouzai Kk | Cyclodextrin clathrate compound including safflower oil |
| CN107189081A (en) * | 2017-06-07 | 2017-09-22 | 兰州理工大学 | A kind of Preparation method and use of multi-functional polysaccharide hydrogel |
-
2018
- 2018-12-18 CN CN201811547397.0A patent/CN109678981B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS53126089A (en) * | 1977-04-11 | 1978-11-02 | Akiyama Jiyouzai Kk | Cyclodextrin clathrate compound including safflower oil |
| CN107189081A (en) * | 2017-06-07 | 2017-09-22 | 兰州理工大学 | A kind of Preparation method and use of multi-functional polysaccharide hydrogel |
Non-Patent Citations (2)
| Title |
|---|
| 任爱农等: "红花多糖的分离纯化及单糖组成分析", 《药物分析杂志》 * |
| 霍贤等: "红花水溶性多糖的分离、纯化及初步研究", 《中国药学杂志》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115120529A (en) * | 2022-06-17 | 2022-09-30 | 山东农业大学 | Red sage root and safflower composite polysaccharide and preparation method and application thereof |
| CN115120529B (en) * | 2022-06-17 | 2023-10-24 | 山东农业大学 | Red sage root and safflower compound polysaccharide, and preparation method and application thereof |
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Denomination of invention: A preparation method, product and application of safflower polysaccharide Effective date of registration: 20210914 Granted publication date: 20210601 Pledgee: Industrial Commercial Bank of China Ltd. Taizhou Huangyan branch Pledgor: ZHEJIANG YONGNING PHARMACEUTICAL Co.,Ltd. Registration number: Y2021330001585 |