CN110279735A - A kind of CAULIS SCHEFFLERAE KWANGSIENSIS active component and preparation method thereof - Google Patents
A kind of CAULIS SCHEFFLERAE KWANGSIENSIS active component and preparation method thereof Download PDFInfo
- Publication number
- CN110279735A CN110279735A CN201910734547.7A CN201910734547A CN110279735A CN 110279735 A CN110279735 A CN 110279735A CN 201910734547 A CN201910734547 A CN 201910734547A CN 110279735 A CN110279735 A CN 110279735A
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- CN
- China
- Prior art keywords
- alcohol
- extract
- water
- elution
- caulis schefflerae
- Prior art date
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- Granted
Links
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 233
- 239000000284 extract Substances 0.000 claims abstract description 124
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 108
- 238000010828 elution Methods 0.000 claims abstract description 73
- 239000000843 powder Substances 0.000 claims abstract description 52
- 239000011347 resin Substances 0.000 claims abstract description 35
- 229920005989 resin Polymers 0.000 claims abstract description 35
- 239000006286 aqueous extract Substances 0.000 claims abstract description 33
- 238000001914 filtration Methods 0.000 claims abstract description 28
- 239000008367 deionised water Substances 0.000 claims abstract description 20
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 18
- 238000001556 precipitation Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 15
- 239000012141 concentrate Substances 0.000 claims abstract description 14
- 150000001875 compounds Chemical class 0.000 claims abstract description 12
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003480 eluent Substances 0.000 claims abstract description 10
- 238000005292 vacuum distillation Methods 0.000 claims abstract description 10
- 235000019441 ethanol Nutrition 0.000 claims description 165
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- 238000012360 testing method Methods 0.000 description 19
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- 229930003944 flavone Natural products 0.000 description 13
- 235000011949 flavones Nutrition 0.000 description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 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 description 12
- 150000002212 flavone derivatives Chemical class 0.000 description 12
- 239000001397 quillaja saponaria molina bark Substances 0.000 description 12
- 229930182490 saponin Natural products 0.000 description 12
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- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 12
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- 208000000114 Pain Threshold Diseases 0.000 description 9
- CGIGDMFJXJATDK-UHFFFAOYSA-N indomethacin Chemical compound CC1=C(CC(O)=O)C2=CC(OC)=CC=C2N1C(=O)C1=CC=C(Cl)C=C1 CGIGDMFJXJATDK-UHFFFAOYSA-N 0.000 description 9
- 239000007788 liquid Substances 0.000 description 8
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- 241000699666 Mus <mouse, genus> Species 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 238000000605 extraction Methods 0.000 description 7
- MIJYXULNPSFWEK-GTOFXWBISA-N 3beta-hydroxyolean-12-en-28-oic acid Chemical compound C1C[C@H](O)C(C)(C)[C@@H]2CC[C@@]3(C)[C@]4(C)CC[C@@]5(C(O)=O)CCC(C)(C)C[C@H]5C4=CC[C@@H]3[C@]21C MIJYXULNPSFWEK-GTOFXWBISA-N 0.000 description 6
- JKLISIRFYWXLQG-UHFFFAOYSA-N Epioleonolsaeure Natural products C1CC(O)C(C)(C)C2CCC3(C)C4(C)CCC5(C(O)=O)CCC(C)(C)CC5C4CCC3C21C JKLISIRFYWXLQG-UHFFFAOYSA-N 0.000 description 6
- YBRJHZPWOMJYKQ-UHFFFAOYSA-N Oleanolic acid Natural products CC1(C)CC2C3=CCC4C5(C)CCC(O)C(C)(C)C5CCC4(C)C3(C)CCC2(C1)C(=O)O YBRJHZPWOMJYKQ-UHFFFAOYSA-N 0.000 description 6
- MIJYXULNPSFWEK-UHFFFAOYSA-N Oleanolinsaeure Natural products C1CC(O)C(C)(C)C2CCC3(C)C4(C)CCC5(C(O)=O)CCC(C)(C)CC5C4=CCC3C21C MIJYXULNPSFWEK-UHFFFAOYSA-N 0.000 description 6
- 229930003935 flavonoid Natural products 0.000 description 6
- 150000002215 flavonoids Chemical class 0.000 description 6
- 235000017173 flavonoids Nutrition 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 229940100243 oleanolic acid Drugs 0.000 description 6
- HZLWUYJLOIAQFC-UHFFFAOYSA-N prosapogenin PS-A Natural products C12CC(C)(C)CCC2(C(O)=O)CCC(C2(CCC3C4(C)C)C)(C)C1=CCC2C3(C)CCC4OC1OCC(O)C(O)C1O HZLWUYJLOIAQFC-UHFFFAOYSA-N 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 5
- 229960000905 indomethacin Drugs 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 4
- JMGZEFIQIZZSBH-UHFFFAOYSA-N Bioquercetin Natural products CC1OC(OCC(O)C2OC(OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5)C(O)C2O)C(O)C(O)C1O JMGZEFIQIZZSBH-UHFFFAOYSA-N 0.000 description 4
- 240000002381 Prunus davidiana Species 0.000 description 4
- 235000015533 Prunus davidiana Nutrition 0.000 description 4
- 238000002835 absorbance Methods 0.000 description 4
- 230000036592 analgesia Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- IVTMALDHFAHOGL-UHFFFAOYSA-N eriodictyol 7-O-rutinoside Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C=C3C(C(C(O)=C(O3)C=3C=C(O)C(O)=CC=3)=O)=C(O)C=2)O1 IVTMALDHFAHOGL-UHFFFAOYSA-N 0.000 description 4
- FDRQPMVGJOQVTL-UHFFFAOYSA-N quercetin rutinoside Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 FDRQPMVGJOQVTL-UHFFFAOYSA-N 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- IKGXIBQEEMLURG-BKUODXTLSA-N rutin 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(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-BKUODXTLSA-N 0.000 description 4
- ALABRVAAKCSLSC-UHFFFAOYSA-N rutin Natural products CC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5 ALABRVAAKCSLSC-UHFFFAOYSA-N 0.000 description 4
- 235000005493 rutin Nutrition 0.000 description 4
- 229960004555 rutoside Drugs 0.000 description 4
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 208000008765 Sciatica Diseases 0.000 description 3
- 229960000583 acetic acid Drugs 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 201000010099 disease Diseases 0.000 description 3
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 3
- 230000000857 drug effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000012362 glacial acetic acid Substances 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002504 physiological saline solution Substances 0.000 description 3
- 239000013558 reference substance Substances 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- 239000002893 slag Substances 0.000 description 3
- 239000012086 standard solution Substances 0.000 description 3
- 206010044652 trigeminal neuralgia Diseases 0.000 description 3
- 206010067484 Adverse reaction Diseases 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 206010061218 Inflammation Diseases 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 230000006838 adverse reaction Effects 0.000 description 2
- 125000003158 alcohol group Chemical group 0.000 description 2
- 239000003957 anion exchange resin Substances 0.000 description 2
- 239000000730 antalgic agent Substances 0.000 description 2
- 230000000146 antalgic effect Effects 0.000 description 2
- 210000003445 biliary tract Anatomy 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000007667 floating Methods 0.000 description 2
- 230000002496 gastric effect Effects 0.000 description 2
- 229940093915 gynecological organic acid Drugs 0.000 description 2
- 230000004054 inflammatory process Effects 0.000 description 2
- 238000001802 infusion Methods 0.000 description 2
- 210000003734 kidney Anatomy 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000013642 negative control Substances 0.000 description 2
- 235000005985 organic acids Nutrition 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 230000000144 pharmacologic effect Effects 0.000 description 2
- 239000013641 positive control Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 201000003068 rheumatic fever Diseases 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 235000010288 sodium nitrite Nutrition 0.000 description 2
- -1 somedon Chemical compound 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- 239000012085 test solution Substances 0.000 description 2
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 2
- MWOOGOJBHIARFG-UHFFFAOYSA-N vanillin Chemical compound COC1=CC(C=O)=CC=C1O MWOOGOJBHIARFG-UHFFFAOYSA-N 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- 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 description 1
- 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
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- 241000143437 Aciculosporium take Species 0.000 description 1
- 244000144730 Amygdalus persica Species 0.000 description 1
- 206010002091 Anaesthesia Diseases 0.000 description 1
- 241000208340 Araliaceae Species 0.000 description 1
- BSYNRYMUTXBXSQ-UHFFFAOYSA-N Aspirin Chemical compound CC(=O)OC1=CC=CC=C1C(O)=O BSYNRYMUTXBXSQ-UHFFFAOYSA-N 0.000 description 1
- 208000008035 Back Pain Diseases 0.000 description 1
- 241000218176 Corydalis Species 0.000 description 1
- 206010052804 Drug tolerance Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 208000008930 Low Back Pain Diseases 0.000 description 1
- 241000699670 Mus sp. Species 0.000 description 1
- 241000180649 Panax notoginseng Species 0.000 description 1
- 235000003143 Panax notoginseng Nutrition 0.000 description 1
- 235000006040 Prunus persica var persica Nutrition 0.000 description 1
- 208000004078 Snake Bites Diseases 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 210000001015 abdomen Anatomy 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229960001138 acetylsalicylic acid Drugs 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 230000037005 anaesthesia Effects 0.000 description 1
- 238000010171 animal model Methods 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 239000003729 cation exchange resin Substances 0.000 description 1
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- 239000000470 constituent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 239000002024 ethyl acetate extract Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 150000002213 flavones Chemical class 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 230000026781 habituation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 241000411851 herbal medicine Species 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 210000000936 intestine Anatomy 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000004255 ion exchange chromatography Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 208000030208 low-grade fever Diseases 0.000 description 1
- 231100000417 nephrotoxicity Toxicity 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229940021182 non-steroidal anti-inflammatory drug Drugs 0.000 description 1
- 239000002674 ointment Substances 0.000 description 1
- 230000001151 other effect Effects 0.000 description 1
- 229960005489 paracetamol Drugs 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000003285 pharmacodynamic effect Effects 0.000 description 1
- 229960002895 phenylbutazone Drugs 0.000 description 1
- VYMDGNCVAMGZFE-UHFFFAOYSA-N phenylbutazonum Chemical compound O=C1C(CCCC)C(=O)N(C=2C=CC=CC=2)N1C1=CC=CC=C1 VYMDGNCVAMGZFE-UHFFFAOYSA-N 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000002040 relaxant effect Effects 0.000 description 1
- 208000004124 rheumatic heart disease Diseases 0.000 description 1
- RZJQGNCSTQAWON-UHFFFAOYSA-N rofecoxib Chemical compound C1=CC(S(=O)(=O)C)=CC=C1C1=C(C=2C=CC=CC=2)C(=O)OC1 RZJQGNCSTQAWON-UHFFFAOYSA-N 0.000 description 1
- 229960000371 rofecoxib Drugs 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 210000002435 tendon Anatomy 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 150000008130 triterpenoid saponins Chemical class 0.000 description 1
- 231100000611 venom Toxicity 0.000 description 1
- 230000001755 vocal effect Effects 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/25—Araliaceae (Ginseng family), e.g. ivy, aralia, schefflera or tetrapanax
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P29/00—Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
Landscapes
- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- Medicinal Chemistry (AREA)
- Animal Behavior & Ethology (AREA)
- Chemical & Material Sciences (AREA)
- Pharmacology & Pharmacy (AREA)
- Engineering & Computer Science (AREA)
- Biotechnology (AREA)
- Rheumatology (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Pain & Pain Management (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Alternative & Traditional Medicine (AREA)
- Organic Chemistry (AREA)
- Botany (AREA)
- Medical Informatics (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Epidemiology (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The present invention relates to a kind of CAULIS SCHEFFLERAE KWANGSIENSIS active components and preparation method thereof.The CAULIS SCHEFFLERAE KWANGSIENSIS active component is prepared with the following method: 1) CAULIS SCHEFFLERAE KWANGSIENSIS medicinal material being carried out alcohol extracting, filtering obtains alcohol extract and residue；2) residue is subjected to water extract-alcohol precipitation, obtains Aqueous extracts；3) alcohol extract and Aqueous extracts are merged, concentrate drying obtains medicinal extract powder；4) medicinal extract powder is dissolved in the water, upper resin column, after successively carry out gradient elution with the ethanol water of deionized water, 10%, 20%, 30%, 50%, 75%, collect the eluent of each gradient, vacuum distillation to equivalent extract state；Equivalent extract residual moisture is removed afterwards, finally obtain the freeze-dried powder at each position, according to containing compound similarity degree, elution position is merged into water, three positions of 10%+20%+30% alcohol elution and 50%+75% alcohol elution, as CAULIS SCHEFFLERAE KWANGSIENSIS active component.
Description
Technical field
Extraction separation and applied technical field the present invention relates to plant active component, specifically, being related to a kind of Chinese peach
Leaf effective-part and preparation method thereof.
Background technique
Pain is clinical common sympton, and the complication of many diseases all with pain, is brought great pain to patients.Mesh
Preceding clinically common anodyne refer to can partially or completely medicine for relieving pain, have non-steroidal anti-inflammatory drugs and central analgesic
Two class of medicine.Common anodyne has aspirin, somedon, paracetamol, phenylbutazone, rofecoxib etc..But it is used for a long time, stomach and intestine
Road reaction and renal toxicity increase, erious adverse reaction, are unfavorable for the treatment and recovery of patient disease, and some anesthesia classes have habituation
Property, therefore it is unable to prolonged application.And Chinese Traditional Medicine significantly improves clinical symptoms and sign treating pain or have when complication,
Such as rhizoma corydalis, Radix Notoginseng, with adverse reaction is few and the advantages such as light.CAULIS SCHEFFLERAE KWANGSIENSIS is in treatment sciatica, trigeminal neuralgia etc.
The special efficacy of stubborn and stupid pain causes people and more and more pays close attention to.
CAULIS SCHEFFLERAE KWANGSIENSIS is Chinese medicine simply with Guangxi national characters, records in " Guangxi Chinese herbal medicine ", is Araliaceae
The drying stem and branch with leaf or stem branch of Radix Schfflerae kwangisensis Schefllera kwangsiensis Merr.ex Li.Its nature and flavor slight bitter,
It is puckery, warm, there is wind-expelling pain-stopping, relaxing tendons and activating collaterals and other effects.It is mainly used for treating rheumatic arthritis, sciatica, trigeminal neuralgia
Pain and kidney, biliary tract pains and other diseases.CAULIS SCHEFFLERAE KWANGSIENSIS main product is distributed mainly on the counties such as Wuming, the Fusui in Guangxi in Guangxi." the Guangxi people
Race's medicine short course " in CAULIS SCHEFFLERAE KWANGSIENSIS the effect of and common method be described: root, stem are decocted in water for oral dose, treating rheumatic heart disease, premenstrual abdomen
Bitterly, it catches a cold；Wine clothes are rushed in decocting, control lumbago due to wind-wetness evil；Be decocted in water for oral dose simultaneous ablution, harnesses the river swollen；Deposited affected part is mashed, fracture is controlled；Mash deposited wound
Around mouthful, venomous snake bite is controlled.The research to CAULIS SCHEFFLERAE KWANGSIENSIS domestic at present is reported few, and Liu Xian etc. publishes thesis " the anti-inflammatory town of CAULIS SCHEFFLERAE KWANGSIENSIS
Pain acts on the screening of active component " in, preliminary screening is carried out to the petroleum ether, ethyl acetate, n-butanol portion of CAULIS SCHEFFLERAE KWANGSIENSIS, as a result
Show that ethyl acetate extract has more significant antalgic and inflammation relieving effect, but there are no further mentioning suitable for large-scale production
Take the report of purification process and application.Hu book equality develops CAULIS SCHEFFLERAE KWANGSIENSIS organic acid composition Study and ointment, using ion
Exchange chromatography and modern separation technology determine the optimum extraction process of total organic acids, and carry out pharmacological research, but extracting method
Complicated, high production cost, is not suitable for industrialized production.
CN109010396A discloses CAULIS SCHEFFLERAE KWANGSIENSIS active component and preparation method thereof, which is CAULIS SCHEFFLERAE KWANGSIENSIS medicinal material warp
After crushing, is infiltrated, then use 30-40% ethyl alcohol heating and refluxing extraction, filtered, filtrate is cold at 0-4 DEG C with 5% sodium bicarbonate solution
24-48 hours are stood in library, is filtered, medicinal extract is obtained after decompression filtrate recycling ethanol, adds water, is mixed, being adjusted with acid solution ph is
N-butanol is recovered under reduced pressure in 3-4, then the butanol solution extraction being saturated with water, extract liquor, and obtained extract is that CAULIS SCHEFFLERAE KWANGSIENSIS has
Imitate position.Application of the CAULIS SCHEFFLERAE KWANGSIENSIS active component in terms of the health care product or drug of preparation prevention or treatment pain symptom, it is special
It is not the pain such as rheumatic arthritis, sciatica, trigeminal neuralgia and kidney, biliary tract.The effective portion of CAULIS SCHEFFLERAE KWANGSIENSIS provided by the invention
The preparation method of position, operation is simple, and the active component high income of extraction, strong operability, production cost is low, is suitble to industry
Scale mass production.
However, the content of general flavone and total saposins is relatively low in the CAULIS SCHEFFLERAE KWANGSIENSIS extract that the method for the prior art obtains, how
Improve the content of the general flavone and total saposins difficulty that this field faces always in CAULIS SCHEFFLERAE KWANGSIENSIS extract.
In view of this present invention is specifically proposed.
Summary of the invention
The purpose of the present invention is to provide a kind of CAULIS SCHEFFLERAE KWANGSIENSIS active components and preparation method thereof, and this method substantially increases the Chinese
The content of general flavone and total saposins in peach leaf extract.
In order to solve the above technical problems, the present invention adopts the following technical scheme:
A kind of CAULIS SCHEFFLERAE KWANGSIENSIS active component, wherein the CAULIS SCHEFFLERAE KWANGSIENSIS active component is prepared with the following method:
1) CAULIS SCHEFFLERAE KWANGSIENSIS medicinal material is subjected to alcohol extracting, filtering obtains alcohol extract and residue；
2) the resulting residue of step 1) is subjected to water extract-alcohol precipitation, obtains Aqueous extracts；
3) the resulting alcohol extract of step 1) and the resulting Aqueous extracts of step 2) are merged, concentrate drying obtains medicinal extract powder；
4) the resulting medicinal extract powder of step 3) is dissolved in the water, upper resin column, after successively with deionized water, 10%,
20%, 30%, 50%, 75% ethanol water carries out gradient elution, collects the eluent of each gradient, is evaporated under reduced pressure to dense
Medicinal extract state；Equivalent extract residual moisture is removed afterwards, the freeze-dried powder at each position is finally obtained, according to containing compound similar
Elution position is merged into water, 10%+20%+30% alcohol elution and 50%+75% alcohol elution three by degree
Position, as CAULIS SCHEFFLERAE KWANGSIENSIS active component.
The method that the prior art uses water extract-alcohol precipitation as the extraction of CAULIS SCHEFFLERAE KWANGSIENSIS in pharmacopeia, and water extract-alcohol precipitation is difficult big
Part flavonoids and saponin(e substance extract.How preferably flavonoids most of in CAULIS SCHEFFLERAE KWANGSIENSIS and saponin(e substance to be mentioned
Take out the problem of always this field.The present inventor analyzes from structure, Flavonoid substances be it is fat-soluble, be insoluble in water, easily
It is dissolved in ethyl alcohol.Further surprisingly find that first carrying out alcohol extracting to CAULIS SCHEFFLERAE KWANGSIENSIS medicinal material obtains alcohol extract and residual by largely testing
Then slag carries out water extract-alcohol precipitation to the residue after alcohol extracting, obtains Aqueous extracts；Alcohol extract and Aqueous extracts are merged again, are concentrated and dried
Obtain medicinal extract powder.General flavone content and total saponin content are significantly improved in the medicinal extract powder obtained in this way.And into
One step proves that flavonoids and saponin(e substance have positive effect to analgesia, and the method for the prior art only uses water by pharmacodynamic test
Most of flavonoids and saponin(e substance can be lost by mentioning alcohol precipitation, certainly will reduce analgesic effect；The method of the present invention significantly improves leaching
The content of general flavone and total saposins in cream powder, to improve analgesic effect.
Furthermore, it was found that by resin column gradient elution obtains on the medicinal extract powder obtained only with water extract-alcohol precipitation water,
10%, the amount of the powder at 20%, 30%, 50%, 75% each position is fewer, and the water extracting alcohol again of first alcohol precipitation through the invention
The powder of resin column gradient elution obtains on heavy obtained medicinal extract powder water, 10%, 20%, 30%, 50%, 75% each position
The amount at end greatly improves.
Meanwhile the present invention through analgesia effect experiments have shown that, water, 10%+20%+30% alcohol elution, 50%+75%
Alcohol elution shows analgesic activities, and wherein the analgesic activities at water elution position are more stable compared with other two groups, and
50%+75% alcohol elution activity is better than 10%+20%+30% alcohol elution.Therefore, water, 10%+20%+
Three positions of 30% alcohol elution and 50%+75% alcohol elution, are CAULIS SCHEFFLERAE KWANGSIENSIS active component.
The present invention also provides the preparation methods of the CAULIS SCHEFFLERAE KWANGSIENSIS active component, wherein the preparation method includes such as
Lower step:
1) CAULIS SCHEFFLERAE KWANGSIENSIS medicinal material is subjected to alcohol extracting, filtering obtains alcohol extract and residue；
2) water extract-alcohol precipitation is carried out after the resulting residue of step 1) being volatilized residual alcoholic solvent, obtains Aqueous extracts；
3) the resulting alcohol extract of step 1) and the resulting Aqueous extracts of step 2) are merged, concentrate drying obtains medicinal extract powder；
4) the resulting medicinal extract powder of step 3) is dissolved in the water, upper resin column, after successively with deionized water, 10%,
20%, 30%, 50%, 75% ethanol water carries out gradient elution, collects the eluent of each gradient, is evaporated under reduced pressure to dense
Medicinal extract state；Equivalent extract residual moisture is removed afterwards, the freeze-dried powder at each position is finally obtained, according to containing compound similar
Elution position is merged into water, 10%+20%+30% alcohol elution and 50%+75% alcohol elution three by degree
Position, as CAULIS SCHEFFLERAE KWANGSIENSIS active component.
Further, in step 1), the alcohol extracting is to be extracted twice with 70% ethyl alcohol.
Further, in step 4), 4 times of column volumes of each gradient elution.
Further, in step 4), the resin column is HP20 macroporous resin column.
Further, in step 4), before upper HP20 macroporous resin column, first HP20 macroporous resin column is located as follows
Reason:
HP20 macroreticular resin 1L is taken, is first used alcohol solution dipping 24 hours, will be drifted along and suspended matter washes away, fill column afterwards, is used
Ethyl alcohol continues to rinse 3 volumes, washes away residual impurity in resin.
In the present invention, related mass percent is percent by volume.
In the present invention, the water extract-alcohol precipitation in step 2) is carried out according to the method for water extract-alcohol precipitation in pharmacopeia, and the specific method is as follows:
By the resulting residue of step 1) volatilize residual alcoholic solvent after add water to cook it is secondary, 1.5 hours every time, filter, merge
Filtrate is concentrated into the clear cream that relative density is about 1.2 (50 DEG C), adds ethyl alcohol to alcohol content up to 60%, stands, second is recycled in filtration
Alcohol, gained filtrate are Aqueous extracts.
Water extract-alcohol precipitation described in step 2) of the present invention can also carry out by the following method: the resulting residue of step 1) is waved
Add the water of 6-20 times of weight to decoct after dry residual alcoholic solvent secondary, decocts 2 hours for the first time, second is 1 hour pan-fried, collecting decoction,
Filtering, filtrate are concentrated into the clear cream of relative density 1.0-1.3 (60 DEG C), add ethyl alcohol to alcohol content up to 60%, stand, filter, return
Ethyl alcohol is received, gained filtrate is Aqueous extracts.
The present invention furthermore provides the CAULIS SCHEFFLERAE KWANGSIENSIS active component in preparation prevention and/or the guarantor for the treatment of pain symptom
Application in terms of strong product or drug.
After adopting the above technical scheme, compared with the prior art, the invention has the following beneficial effects:
1, the present invention is by first obtaining alcohol extract and residue to the progress alcohol extracting of CAULIS SCHEFFLERAE KWANGSIENSIS medicinal material, then to the residue after alcohol extracting into
Row water extract-alcohol precipitation, obtains Aqueous extracts；Alcohol extract and Aqueous extracts are merged, concentrate drying obtains medicinal extract powder；It will be on medicinal extract powder
Resin column is eluted with water, ethanol solution, screens, obtained with the effective portion of the significant CAULIS SCHEFFLERAE KWANGSIENSIS of analgesic activity in conjunction with pharmacological evaluation
Position；Show to all have significant analgesic activity through hot plate test；
2, the CAULIS SCHEFFLERAE KWANGSIENSIS active component provided by the invention with analgesic activity can be prepared into drug or health care product, can be convenient
Patient clinical uses.Simultaneously CAULIS SCHEFFLERAE KWANGSIENSIS active component provided by the invention preparation method, operation is simple, extraction it is effective
Position high income, strong operability, production cost is low, is suitble to industrial scale mass production.
A specific embodiment of the invention is described in further detail with reference to the accompanying drawing.
Detailed description of the invention
Fig. 1 is CAULIS SCHEFFLERAE KWANGSIENSIS total extract hot plate test drug effect figure, and wherein Indometacin is positive drug group, and HTY is CAULIS SCHEFFLERAE KWANGSIENSIS
Group, Vehicle are blank control group；
Fig. 2 is CAULIS SCHEFFLERAE KWANGSIENSIS different parts hot plate test drug effect figure, and wherein Indometacin is positive drug group, HTY
(organic acid) is organic acid position group, and HTY (water) is water elution position group, and HTY (30%alcohol) is 10%+
20%+30% alcohol elution group, HTY (50%alcohol) are 50%+75% alcohol elution group, and Vehicle is sky
White control group.
It should be noted that these attached drawings and verbal description are not intended to the design model limiting the invention in any way
It encloses, but illustrates idea of the invention by referring to specific embodiments for those skilled in the art.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, the technical solution in embodiment is clearly and completely described, the following examples are intended to illustrate the invention, but
It is not intended to limit the scope of the invention.
Embodiment 1
1) take CAULIS SCHEFFLERAE KWANGSIENSIS medicinal material 15kg, extracted twice with 70% ethyl alcohol first, each 120kg, filtering, obtain alcohol extract and
Residue；
2) the resulting residue of step 1) is volatilized into residual ethanol solvent, adds 6 times of amount water to decoct secondary, 1.5 hours every time, filter
It crosses, merging filtrate, is concentrated into the clear cream that relative density is about 1.2 (50 DEG C), add ethyl alcohol to alcohol content up to 60%, stand, filtration,
Ethyl alcohol is recycled, gained filtrate is Aqueous extracts；
3) the resulting alcohol extract of step 1) is merged with the resulting Aqueous extracts of step 2), concentrate drying obtains medicinal extract powder
1.23kg；
4) HP20 macroreticular resin 1L is taken, first uses alcohol solution dipping 24 hours, floating dust and suspended matter is washed away, fill column afterwards,
Continued to rinse 3 volumes with ethyl alcohol, washes away residual impurity in resin.It is rinsed with deionized water until efflux does not have alcohol taste.It takes
CAULIS SCHEFFLERAE KWANGSIENSIS medicinal extract powder 65g, is dissolved completely in the deionized water of 300ml, loading, after successively use deionized water, 10%,
20%, 30%, 50%, 75% ethanol water carries out gradient elution, and 4 times of column volumes of each gradient elution are collected each afterwards
The eluent of gradient, vacuum distillation to equivalent extract state.Equivalent extract is placed on freeze drier afterwards, removes residual moisture, most
Obtain the freeze-dried powder at each position: water (20.8g, 32%) eventually, 10% (3.2g, 4.9%), 20% (5.5g, 8.4%),
30% (4.2g, 6.4%), 50% (10.3g, 15.8%), 75% (2.3g, 3.5%).According to containing compound similar journey
Elution position is merged into three water, 10%+20%+30% alcohol elution and 50%+75% alcohol elution portions by degree
Position, as CAULIS SCHEFFLERAE KWANGSIENSIS active component.
Embodiment 2
1) take CAULIS SCHEFFLERAE KWANGSIENSIS medicinal material 15kg, extracted twice with 70% ethyl alcohol first, each 120kg, filtering, obtain alcohol extract and
Residue；
2) the resulting residue of step 1) is volatilized into residual ethanol solvent, adds 10 times of amount water to decoct secondary, 1.5 hours every time,
Filtration, merging filtrate are concentrated into the clear cream that relative density is about 1.2 (50 DEG C), add ethyl alcohol to alcohol content up to 60%, stand, filter
It crosses, recycles ethyl alcohol, gained filtrate is Aqueous extracts；
3) the resulting alcohol extract of step 1) is merged with the resulting Aqueous extracts of step 2), concentrate drying obtains medicinal extract powder
1.22kg；
4) HP20 macroreticular resin 1L is taken, is first used alcohol solution dipping 24 hours, will be drifted along and suspended matter washes away, fill column afterwards,
Continued to rinse 3 volumes with ethyl alcohol, wash away residual impurity in resin, rinsed with deionized water until efflux does not have alcohol taste.It will
The resulting medicinal extract powder 65g of step 3) is dissolved in 300ml water, upper resin column, after successively with deionized water, 10%, 20%,
30%, 50%, 75% ethanol water carries out gradient elution, and 4 times of column volumes of each gradient elution collect washing for each gradient
De- liquid, vacuum distillation to equivalent extract state；Equivalent extract residual moisture is removed afterwards, finally obtains the freeze-dried powder at each position, root
According to containing compound similarity degree, elution position is merged into water, 10%+20%+30% alcohol elution and 50%+
75% position of alcohol elution three, as CAULIS SCHEFFLERAE KWANGSIENSIS active component.
Embodiment 3
1) take CAULIS SCHEFFLERAE KWANGSIENSIS medicinal material 15kg, extracted twice with 70% ethyl alcohol first, each 120kg, filtering, obtain alcohol extract and
Residue；
2) the resulting residue of step 1) is volatilized into residual ethanol solvent, adds 14 times of amount water to decoct secondary, 1.5 hours every time,
Filtration, merging filtrate are concentrated into the clear cream that relative density is about 1.2 (50 DEG C), add ethyl alcohol to alcohol content up to 60%, stand, filter
It crosses, recycles ethyl alcohol, gained filtrate is Aqueous extracts；
3) the resulting alcohol extract of step 1) is merged with the resulting Aqueous extracts of step 2), concentrate drying obtains medicinal extract powder
1.23kg；
4) the resulting medicinal extract powder 65g of step 3) is dissolved in 300ml water, upper HP20 macroporous resin column, after successively use
Deionized water, 10%, 20%, 30%, 50%, 75% ethanol water carry out gradient elution, 4 times of cylinders of each gradient elution
Product collects the eluent of each gradient, vacuum distillation to equivalent extract state；Equivalent extract residual moisture is removed afterwards, is finally obtained each
Elution position is merged into water, 10%+20%+30% second according to containing compound similarity degree by the freeze-dried powder at a position
Alcohol elutes three positions in position and 50%+75% alcohol elution, as CAULIS SCHEFFLERAE KWANGSIENSIS active component.
Embodiment 4
1) CAULIS SCHEFFLERAE KWANGSIENSIS medicinal material 15kg is taken, is extracted twice with 70% ethyl alcohol, each 120kg, filtering obtains alcohol extract and residual
Slag；
2) add the water of 16 times of weight to decoct 2 times after the resulting residue of step 1) being volatilized residual alcoholic solvent, it is small to decoct 2 for the first time
When, second is 1 hour pan-fried, collecting decoction, filtering, and filtrate is concentrated into the clear cream that relative density is about 1.3 (60 DEG C), adds ethyl alcohol extremely
Alcohol content is stood up to 60%, and ethyl alcohol is recycled in filtration, and gained filtrate is Aqueous extracts；
3) the resulting alcohol extract of step 1) and the resulting Aqueous extracts of step 2) are merged, concentrate drying obtains medicinal extract powder；
4) HP20 macroreticular resin 1L is taken, is first used alcohol solution dipping 24 hours, will be drifted along and suspended matter washes away, fill column afterwards,
Continued to rinse 3 volumes with ethyl alcohol, wash away residual impurity in resin, rinsed with deionized water until efflux does not have alcohol taste.It will
The resulting medicinal extract powder 65g of step 3) is dissolved in 300ml water, upper resin column, after successively with deionized water, 10%, 20%,
30%, 50%, 75% ethanol water carries out gradient elution, and 4 times of column volumes of each gradient elution collect washing for each gradient
De- liquid, vacuum distillation to equivalent extract state；Equivalent extract residual moisture is removed afterwards, finally obtains the freeze-dried powder at each position, root
According to containing compound similarity degree, elution position is merged into water, 10%+20%+30% alcohol elution and 50%+
75% position of alcohol elution three, as CAULIS SCHEFFLERAE KWANGSIENSIS active component.
Embodiment 5
1) CAULIS SCHEFFLERAE KWANGSIENSIS medicinal material 15kg is taken, is extracted twice with 70% ethyl alcohol, each 120kg, filtering obtains alcohol extract and residual
Slag；
2) add the water of 20 times of weight to decoct 2 times after the resulting residue of step 1) being volatilized residual alcoholic solvent, it is small to decoct 2 for the first time
When, second is 1 hour pan-fried, collecting decoction, filtering, and filtrate is concentrated into the clear cream that relative density is about 1.0 (60 DEG C), adds ethyl alcohol extremely
Alcohol content is stood up to 60%, and ethyl alcohol is recycled in filtration, and gained filtrate is Aqueous extracts；
3) the resulting alcohol extract of step 1) and the resulting Aqueous extracts of step 2) are merged, concentrate drying obtains medicinal extract powder；
4) the resulting medicinal extract powder 65g of step 3) is dissolved in 300ml water, upper HP20 macroporous resin column, after successively use
Deionized water, 10%, 20%, 30%, 50%, 75% ethanol water carry out gradient elution, 4 times of cylinders of each gradient elution
Product collects the eluent of each gradient, vacuum distillation to equivalent extract state；Equivalent extract residual moisture is removed afterwards, is finally obtained each
Elution position is merged into water, 10%+20%+30% second according to containing compound similarity degree by the freeze-dried powder at a position
Alcohol elutes three positions in position and 50%+75% alcohol elution, as CAULIS SCHEFFLERAE KWANGSIENSIS active component.
The preparation of comparative example 1, CAULIS SCHEFFLERAE KWANGSIENSIS total extract
1) take CAULIS SCHEFFLERAE KWANGSIENSIS medicinal material 15kg, extracted twice with 70% ethyl alcohol first, each 120kg, filtering, obtain alcohol extract and
Residue；
2) the resulting residue of step 1) is volatilized into residual ethanol solvent, add water to cook it is secondary, 1.5 hours every time, filter, close
And filtrate, it is concentrated into the clear cream that relative density is about 1.2 (50 DEG C), adds ethyl alcohol to alcohol content up to 60%, stands, filter, recycling
Ethyl alcohol, gained filtrate are Aqueous extracts；
3) the resulting alcohol extract of step 1) is merged with the resulting Aqueous extracts of step 2), concentrate drying obtains medicinal extract powder
1.23kg, as CAULIS SCHEFFLERAE KWANGSIENSIS total extract.
The preparation of comparative example 2, CAULIS SCHEFFLERAE KWANGSIENSIS organic acid position
1) take CAULIS SCHEFFLERAE KWANGSIENSIS medicinal material 15kg, extracted twice with 70% ethyl alcohol first, each 120kg, filtering, obtain alcohol extract and
Residue；
2) the resulting residue of step 1) is volatilized into residual ethanol solvent, add water to cook it is secondary, 1.5 hours every time, filter, close
And filtrate, it is concentrated into the clear cream that relative density is about 1.2 (50 DEG C), adds ethyl alcohol to alcohol content up to 60%, stands, filter, recycling
Ethyl alcohol, gained filtrate are Aqueous extracts；
3) the resulting alcohol extract of step 1) is merged with the resulting Aqueous extracts of step 2), concentrate drying obtains medicinal extract powder
1.23kg；
4) 201*7 anion exchange resin 800ml is taken, first washes away suspended matter with deionized water immersion, afterwards with 70-80 DEG C
Water impregnates 4 hours, is swollen to resin.By the resin being swollen in the chromatographic column of 1.5L, the 5% of 1.5L is successively used
The 5%HCl solution of the 5%HCl solution of NaOH, 1.5L, the 5%NaOH of 2L, 2L activates resin.Finally be rinsed with water to
It is neutral.
5) CAULIS SCHEFFLERAE KWANGSIENSIS extract powder 35g is taken to be dissolved in 200ml deionized water, after be splined on anion exchange resin
On, it is first rinsed with the deionized water of 4 times of column volumes, is rinsed afterwards with the 1%HCl of 4 times of column volumes, collects the elution of 1%HCl
Liquid, then vacuum distillation concentration, obtains initial organic acid enrichment positions medicinal extract liquid.
6) 001*7 cation exchange resin 800ml is taken, is swollen, activated.The organic acid medicinal extract liquid that will be enriched to
100ml loading is eluted with 4 times of column volume deionized waters, is recycled eluent, is concentrated under reduced pressure into equivalent extract, is placed on freeze-drying
Machine gets on moisture removal, obtains organic acid powder 7.2g (20%).
Comparative example 3, the active component obtained only with water extract-alcohol precipitation
1) CAULIS SCHEFFLERAE KWANGSIENSIS medicinal material 15kg is taken, adds water to cook secondary, 1.5 hours every time, filtration, merging filtrate was concentrated into opposite
Density is about the clear cream of 1.2 (50 DEG C), adds ethyl alcohol to alcohol content up to 60%, stands, ethyl alcohol is recycled in filtration, and filtrate is condensed into thick
Paste is dried to dry extract, obtains medicinal extract powder 0.85kg.
2) HP20 macroreticular resin 1L is taken, first uses alcohol solution dipping 24 hours, floating dust and suspended matter is washed away, fill column afterwards,
Continued to rinse 3 volumes with ethyl alcohol, washes away residual impurity in resin.It is rinsed with deionized water until efflux does not have alcohol taste.It takes
CAULIS SCHEFFLERAE KWANGSIENSIS medicinal extract powder 65g, is dissolved completely in the deionized water of 300ml, loading, after successively use deionized water, 10%,
20%, 30%, 50%, 75% ethanol water carries out gradient elution, and 4 times of column volumes of each gradient elution are collected each afterwards
The eluent of gradient, vacuum distillation to equivalent extract state.Equivalent extract is placed on freeze drier afterwards, removes residual moisture, most
Obtain the freeze-dried powder at each position: water (16.2g, 25.9%) eventually, 10% (2.2g, 3.4%), 20% (3.5g, 5.4%),
30% (2.2g, 3.4%), 50% (4.5g, 6.9%), 75% (0.5g, 0.8%).According to containing compound similarity degree,
Elution position is merged into three water, 10%+20%+30% alcohol elution and 50%+75% alcohol elution positions,
As CAULIS SCHEFFLERAE KWANGSIENSIS active component.
The general flavone and total saponin content of the total medicinal extract of test example 1, CAULIS SCHEFFLERAE KWANGSIENSIS measure
In 2015 editions pharmacopeia, CAULIS SCHEFFLERAE KWANGSIENSIS piece is that the content of general flavone is surveyed using rutin as reference substance using Ultraviolet Photometric Method
To carry out quality control, therefore general flavone content progress of the measuring method of the general flavone in this experimental applications pharmacopeia to total medicinal extract
Measurement.Know that CAULIS SCHEFFLERAE KWANGSIENSIS contains a large amount of triterpenoid saponins by existing document report.Have been reported that such components have
The drug effect of preferable antalgic and inflammation relieving, therefore the present invention is using oleanolic acid as reference substance surveys containing for total saposins constituents in each position
Amount.
1) preparation of the total medicinal extract of CAULIS SCHEFFLERAE KWANGSIENSIS
1.1 total medicinal extract(alcohol extracting+water mentions)Preparation
A. take CAULIS SCHEFFLERAE KWANGSIENSIS medicinal material 15kg, extracted twice with 70% ethyl alcohol first, each 120kg, filtering, obtain alcohol extract and
Residue；
B. the resulting residue of step a) is volatilized into residual ethanol solvent, add water to cook it is secondary, 1.5 hours every time, filter, close
And filtrate, it is concentrated into the clear cream that relative density is about 1.2 (50 DEG C), adds ethyl alcohol to alcohol content up to 60%, stands, filter, recycling
Ethyl alcohol, gained filtrate are Aqueous extracts；
C. the resulting alcohol extract of step a) is merged with the resulting Aqueous extracts of step b), concentrate drying is always soaked
Cream(alcohol extracting+water mentions)。
1.2 total medicinal extract(water mentions)Preparation
CAULIS SCHEFFLERAE KWANGSIENSIS medicinal material 15kg is taken, adds water to cook secondary, 1.5 hours every time, filtration, merging filtrate was concentrated into relatively close
Degree is about the clear cream of 1.2 (50 DEG C), adds ethyl alcohol to alcohol content up to 60%, stands, ethyl alcohol is recycled in filtration, and filtrate is condensed into thick paste
Shape is dried to dry extract, as total medicinal extract(water mentions)。
2) determination of total flavonoids
Anhydrous control substance of Rutin 10.1mg is taken, it is accurately weighed, it is placed in 10mL measuring bottle, adds 60% ethyl alcohol 5mL, low-grade fever makes molten
Solution, lets cool, is diluted to scale with 60% ethyl alcohol, shakes up.Precision measures 1mL, sets in 5mL measuring bottle, adds water to scale, shake up, i.e.,
It obtains (containing about anhydrous rutin 0.2mg in every 1mL).
The preparation of standard curve: precision measures reference substance solution 0.4mL, 0.8mL, 1.2mL, 1.6mL, 2.0mL, 2.4mL,
It is set in 10mL measuring bottle respectively, adds water to 2.4mL, add 5% sodium nitrite solution 0.4mL, mixed, placed 6min, add 10% nitric acid
Aluminum solutions 0.4mL is mixed, and places 6min, and adding sodium hydroxide test solution 4mL is added water to scale, shaken up, and 15min is placed, with phase
The reagent answered makees blank, according to UV-VIS spectrophotometry (general rule 0401), measures absorbance, at 500nm wavelength with extinction
Degree is ordinate, and concentration is abscissa, draws standard curve.
Sample measurement: taking each sample about 0.16g, accurately weighed, sets in 20mL measuring bottle, adds 60% ethyl alcohol 15mL, 80 DEG C add
Heat 30 minutes, and constantly shake, it lets cool, adds 60% ethyl alcohol to scale, shake up, filter.Precision draws each subsequent filtrate 1.0ml, point
It does not set in 10mL measuring bottle, adds water to 2.4mL, add 5% sodium nitrite solution 0.4mL, mix, place 6min, add 10% aluminum nitrate
Solution 0.4mL is mixed, and places 6min, and adding sodium hydroxide test solution 4mL is added water to scale, shaken up, and 15min is placed, with corresponding
Reagent makees blank, and according to UV-VIS spectrophotometry (general rule 0401), absorbance, another accurate absorption are measured at 500nm wavelength
Subsequent filtrate 1.0mL, is diluted with water to 10mL, shakes up, and makees blank, measures absorbance in accordance with the law, test sample is read from standard curve
In anhydrous rutin amount, calculate to get.It the results are shown in Table 1.
The total medicinal extract general flavone content of table 1, CAULIS SCHEFFLERAE KWANGSIENSIS
Establishing standard curve by ultraviolet spectrophotometry is y=12.766x+0.0071.
As shown in Table 3, general flavone content is 4.48% in total medicinal extract powder that alcohol extracting+water mentions, total medicinal extract powder that water mentions
Middle general flavone content is 3.68%, and total medicinal extract powder flavones content that only water mentions as the result is shown mentions low than alcohol extracting+water.
3) total saponin content measures
The configuration of oleanolic acid standard solution: it accurately weighs oleanolic acid standard items 1mg and is placed in 5ml volumetric flask, use first
Alcohol constant volume obtains the oleanolic acid standard solution stock solution of 0.2mg/ml.
The preparation of oleanolic acid standard curve: it weighs 25mg vanillic aldehyde and is mixed with 5ml glacial acetic acid solution, it is molten to obtain vanillic aldehyde
Liquid.Oleanolic acid standard solution stock solution 0,40,80,120,160,200ul is taken to be placed in 10ml centrifuge tube respectively, at 40 DEG C
Under be dried with nitrogen.Then 50ul vanillic aldehyde-glacial acetic acid solution and 200ul perchloric acid solution is added, obtained 250ul solution is existed
5min is cooled down after 70 DEG C of water-bath 15min again.The glacial acetic acid of 650ul is added after cooling, after obtained 900ul solution is mixed
10min is stood, 2.7ml is diluted to, then measures A with ultraviolet specrophotometer540nm, using absorbance as ordinate, concentration is cross
Coordinate draws standard curve.
The measurement of sample: sample is respectively weighed to 10mg and is dissolved in the methanol of 5ml, 5ml sample liquid is obtained.By above-mentioned neat pier
Tartaric acid standard curve preparation flow, is measured sample liquid, and obtained numerical value is substituted into equation of linear regression, calculates sample
Middle total saponin content.It the results are shown in Table 2.
The total medicinal extract total saponin content of table 2, CAULIS SCHEFFLERAE KWANGSIENSIS
Establishing standard curve by ultraviolet spectrophotometry is y=35.569x+0.0478.
As shown in Table 2, total saponin content is 16.51% in total medicinal extract powder that alcohol extracting+water mentions, total medicinal extract powder that water mentions
Middle total saponin content is 8.77%, and total medicinal extract powder total saponin content that only water mentions as the result is shown mentions low than alcohol extracting+water.
Test example 2, hot plate test
1) test medicine
CAULIS SCHEFFLERAE KWANGSIENSIS total extract and different enrichment positions.
The test dose of total extract is 5g/kg/d, and administration solution concentration is total for the CAULIS SCHEFFLERAE KWANGSIENSIS that can be dissolved in physiological saline
The maximum value of extract, dosage are equivalent to 18 times of adult taking dose.
In second of different enrichment positions activity experiment, the dosage at four positions is 1.8 times of the reality in total extract
It tests on the basis of dosage (9g/kg/d), is obtained by weight of the percentage composition that this position accounts for total extract carries out.This conversion
Mode is while investigation different parts respective drug activity, it is contemplated that the quality in total extract of different compounds accounts for
Than being more in line with medication actual conditions.Final several regional administration amounts are respectively that 2.8g/kg/d (water elution position) (is implemented
It is prepared by example 1), 1.8g/kg/d (10%+20%+30% alcohol elution) (preparation of embodiment 1), 1.7g/kg/d (50%+
75% alcohol elution) (preparation of embodiment 1), 2.8g/kg/d (organic acid position) (preparation of comparative example 2).
2) experimental animal
SPF grades of KM kind mouse, 18-22g, female (hot plate) are provided by Shenyang Pharmaceutical University's experimental animal center, purchased from north
Capital Fukang biotech inc, quality certification number: laboratory keeps on file
3) medicine and reagent
4) test apparatus
5) test method
Female mice is put into hot plate induced pain instrument, by the control of hot plate induced pain instrument temperature in (55 ± 0.5) DEG C, until occurring
Pain threshold of the time (s) as the mouse for licking metapedes, gives it up less than 5s or greater than 30s or leaper.The qualified female of screening
Its normal pain threshold is surveyed in mouse, repetition, pain threshold before taking the average value of the two subnormal threshold of pains to be administered as the mouse.Random grouping,
Every group 12.
Dosage regimen (first time): negative control group, physiological saline；Positive controls, Indomethacin, 20mg/kg/d；The Chinese
Peach leaf extract high dose group, 5g/kg/d.Every group, daily according to mouse weight with dosage 0.1mL/10g gastric infusion 1 time, connects
Continuous 7d.
Dosage regimen (for the second time): negative control group, physiological saline；Positive controls, Indomethacin, 20mg/kg/d；The Chinese
Peach leaf organic acids extract, CAULIS SCHEFFLERAE KWANGSIENSIS water extract, CAULIS SCHEFFLERAE KWANGSIENSIS 10%+20%+30% alcohol elution, CAULIS SCHEFFLERAE KWANGSIENSIS 50%+
75% alcohol elution, every group daily according to mouse weight with dosage 0.1mL/10g gastric infusion 1 time, continuous 7d.
Measure the pain threshold of the 30th, 60,90,120min after mouse is administered.If the threshold of pain is more than 60s, recorded by 60s, and
Calculate threshold of pain increase rate.Pain threshold × 100 before threshold of pain increase rate (%)=(pain threshold before pain threshold-administration after administration)/administration.
6) test result
Test result is shown in Table 3 and table 4:
Table 3, CAULIS SCHEFFLERAE KWANGSIENSIS total extract hot plate test record sheet
Table 4, CAULIS SCHEFFLERAE KWANGSIENSIS different parts hot plate test record sheet
7) conclusion and discussion
(1) CAULIS SCHEFFLERAE KWANGSIENSIS total extract is in hot-plate analgesia test, four time points 30min, 60min, 90min, 120min with
It is compared before administration, shows analgesic activities, it is respectively 30%, 81%, 80%, 50% (table 3, figure that pain threshold, which improves percentage,
1), it is weaker than positive drug Indomethacin group.
(2) in the hot-plate analgesia test of four extractive parts, CAULIS SCHEFFLERAE KWANGSIENSIS (organic acid) does not show analgesic activities,
Excess-three group has analgesic activities.Wherein, CAULIS SCHEFFLERAE KWANGSIENSIS (10%+20%+30% alcohol elution) only shows town in 90min
Pain activity, it is 77.84% that percentage is improved in the threshold of pain；CAULIS SCHEFFLERAE KWANGSIENSIS (50%+75% alcohol elution) analgesic activities are better than Chinese peach
Leaf (10%+20%+30% alcohol elution) shows analgesic activities in 90min and 120min, and percentage is improved in the threshold of pain
For 116.23% and 84.93%, and it is better than the positive drug group Indomethacin 90min (88.27%) and 120min at the time point
(58.93%).CAULIS SCHEFFLERAE KWANGSIENSIS (water elution position) group is in four time points 30min, 60min, 90min, 120min and phase before administration
Than showing analgesic activities, it is respectively 32.95%, 46.82%, 47.98%, 60.12% that pain threshold, which improves percentage, is resisted
Scorching analgesic activities are weaker than positive drug group, but are better than CAULIS SCHEFFLERAE KWANGSIENSIS (50%+75% ethanol elution portion at 30min and 60min time point
Position) group.
The above is only presently preferred embodiments of the present invention, is not intended to limit the present invention in any form, though
So the present invention has been disclosed as a preferred embodiment, and however, it is not intended to limit the invention, any to be familiar with technology people of the invention
Member without departing from the scope of the present invention, when the technology contents using above-mentioned prompt make it is a little variation or be modified to
The equivalent embodiment of equivalent variations, but anything that does not depart from the technical scheme of the invention content, it is right according to the technical essence of the invention
Any simple modification, equivalent change and modification made by above embodiments, in the range of still falling within the present invention program.
Claims (8)
1. a kind of CAULIS SCHEFFLERAE KWANGSIENSIS active component, which is characterized in that the CAULIS SCHEFFLERAE KWANGSIENSIS active component is to be prepared into the following method
It arrives:
1) CAULIS SCHEFFLERAE KWANGSIENSIS medicinal material is subjected to alcohol extracting, filtering obtains alcohol extract and residue；
2) the resulting residue of step 1) is subjected to water extract-alcohol precipitation, obtains Aqueous extracts；
3) the resulting alcohol extract of step 1) and the resulting Aqueous extracts of step 2) are merged, concentrate drying obtains medicinal extract powder；
4) the resulting medicinal extract powder of step 3) is dissolved in the water, upper resin column, after successively with deionized water, 10%, 20%,
30%, 50%, 75% ethanol water carries out gradient elution, collects the eluent of each gradient, vacuum distillation to equivalent extract
State；Equivalent extract residual moisture is removed afterwards, the freeze-dried powder at each position is finally obtained, according to containing compound similar journey
Elution position is merged into three water, 10%+20%+30% alcohol elution and 50%+75% alcohol elution portions by degree
Position, as CAULIS SCHEFFLERAE KWANGSIENSIS active component.
2. a kind of preparation method of CAULIS SCHEFFLERAE KWANGSIENSIS active component described in claim 1, which is characterized in that the preparation method packet
Include following steps:
1) CAULIS SCHEFFLERAE KWANGSIENSIS medicinal material is subjected to alcohol extracting, filtering obtains alcohol extract and residue；
2) water extract-alcohol precipitation is carried out after the resulting residue of step 1) being volatilized residual alcoholic solvent, obtains Aqueous extracts；
3) the resulting alcohol extract of step 1) and the resulting Aqueous extracts of step 2) are merged, concentrate drying obtains medicinal extract powder；
4) the resulting medicinal extract powder of step 3) is dissolved in the water, upper resin column, after successively with deionized water, 10%, 20%,
30%, 50%, 75% ethanol water carries out gradient elution, collects the eluent of each gradient, vacuum distillation to equivalent extract
State；Equivalent extract residual moisture is removed afterwards, the freeze-dried powder at each position is finally obtained, according to containing compound similar journey
Elution position is merged into three water, 10%+20%+30% alcohol elution and 50%+75% alcohol elution portions by degree
Position, as CAULIS SCHEFFLERAE KWANGSIENSIS active component.
3. preparation method according to claim 2, which is characterized in that in step 1), the alcohol extracting is with 70% ethyl alcohol
It extracts twice.
4. preparation method according to claim 2 or 3, which is characterized in that in step 4), 4 times of cylinders of each gradient elution
Product.
5. according to preparation method described in claim 2-4 any one, which is characterized in that in step 4), the resin column
For HP20 macroporous resin column.
6. preparation method according to claim 5, which is characterized in that in step 4), before upper HP20 macroporous resin column, first
HP20 macroporous resin column is handled as follows:
HP20 macroreticular resin 1L is taken, is first used alcohol solution dipping 24 hours, will be drifted along and suspended matter washes away, fill column afterwards, use ethyl alcohol
Continue to rinse 3 volumes, washes away residual impurity in resin.
7. according to preparation method described in claim 2-6 any one, which is characterized in that water extract-alcohol precipitation described in step 2)
Are as follows: by the resulting residue of step 1) volatilize residual alcoholic solvent after add water to cook it is secondary, 1.5 hours every time, filtration, merging filtrate,
It is concentrated into the clear cream that relative density is 1.2 at 50 DEG C, adds ethyl alcohol to alcohol content up to 60%, stands, ethyl alcohol, gained are recycled in filtration
Filtrate is Aqueous extracts.
8. a kind of CAULIS SCHEFFLERAE KWANGSIENSIS active component described in claim 1 preparation prevention and/or treatment pain symptom health care product or
Application in terms of drug.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1454631A (en) * | 2003-01-24 | 2003-11-12 | 贵州三力制药有限责任公司 | Schefflera (Hantaoye) soft capsule and preparing method thereof |
| CN102836190A (en) * | 2012-09-25 | 2012-12-26 | 广西金海堂药业有限责任公司 | Preparation method and quality control method for schefflera kwangsiensis general flavone extract |
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2019
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1454631A (en) * | 2003-01-24 | 2003-11-12 | 贵州三力制药有限责任公司 | Schefflera (Hantaoye) soft capsule and preparing method thereof |
| CN102836190A (en) * | 2012-09-25 | 2012-12-26 | 广西金海堂药业有限责任公司 | Preparation method and quality control method for schefflera kwangsiensis general flavone extract |
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| 黄婧等: "汉桃叶总黄酮的提取及其镇痛抗炎活性研究", 《中国药业》 * |
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