CN109157524B - Preparation method of Wulingshen polysaccharide dropping pill - Google Patents
Preparation method of Wulingshen polysaccharide dropping pill Download PDFInfo
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- CN109157524B CN109157524B CN201811179540.5A CN201811179540A CN109157524B CN 109157524 B CN109157524 B CN 109157524B CN 201811179540 A CN201811179540 A CN 201811179540A CN 109157524 B CN109157524 B CN 109157524B
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- polysaccharide
- wulingshen
- dropping
- pill
- polyethylene glycol
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- 150000004676 glycans Chemical class 0.000 title claims abstract description 98
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 98
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 98
- 239000006187 pill Substances 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229940057838 polyethylene glycol 4000 Drugs 0.000 claims abstract description 15
- 229940093429 polyethylene glycol 6000 Drugs 0.000 claims abstract description 15
- 238000000502 dialysis Methods 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- 108010059892 Cellulase Proteins 0.000 claims abstract description 9
- 229940106157 cellulase Drugs 0.000 claims abstract description 9
- 238000001556 precipitation Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000002390 rotary evaporation Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 45
- 239000011159 matrix material Substances 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 17
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 16
- 239000012153 distilled water Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000002244 precipitate Substances 0.000 claims description 14
- 239000000725 suspension Substances 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 13
- 239000000110 cooling liquid Substances 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- 241000208340 Araliaceae Species 0.000 claims description 9
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 claims description 9
- 235000003140 Panax quinquefolius Nutrition 0.000 claims description 9
- 235000008434 ginseng Nutrition 0.000 claims description 9
- 238000004090 dissolution Methods 0.000 claims description 8
- 239000003208 petroleum Substances 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 238000000643 oven drying Methods 0.000 claims description 7
- 238000010298 pulverizing process Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 239000006228 supernatant Substances 0.000 claims description 7
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 7
- 229940057995 liquid paraffin Drugs 0.000 claims description 4
- 241000146029 Lindera aggregata Species 0.000 claims description 3
- 239000010495 camellia oil Substances 0.000 claims description 3
- AMTWCFIAVKBGOD-UHFFFAOYSA-N dioxosilane;methoxy-dimethyl-trimethylsilyloxysilane Chemical compound O=[Si]=O.CO[Si](C)(C)O[Si](C)(C)C AMTWCFIAVKBGOD-UHFFFAOYSA-N 0.000 claims description 3
- 239000010499 rapseed oil Substances 0.000 claims description 3
- 229940083037 simethicone Drugs 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 2
- 239000009137 wuling Substances 0.000 claims 2
- 230000000694 effects Effects 0.000 abstract description 10
- 230000000857 drug effect Effects 0.000 abstract description 5
- 239000001913 cellulose Substances 0.000 abstract description 3
- 229920002678 cellulose Polymers 0.000 abstract description 3
- 238000000605 extraction Methods 0.000 abstract description 3
- 230000036039 immunity Effects 0.000 abstract description 3
- 238000002844 melting Methods 0.000 abstract description 3
- 230000008018 melting Effects 0.000 abstract description 3
- 239000000758 substrate Substances 0.000 abstract description 3
- 238000001816 cooling Methods 0.000 abstract description 2
- 239000003814 drug Substances 0.000 abstract description 2
- 238000005238 degreasing Methods 0.000 abstract 1
- 238000009740 moulding (composite fabrication) Methods 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 241001558929 Sclerotium <basidiomycota> Species 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- NYHBQMYGNKIUIF-UUOKFMHZSA-N Guanosine Chemical compound C1=NC=2C(=O)NC(N)=NC=2N1[C@@H]1O[C@H](CO)[C@@H](O)[C@H]1O NYHBQMYGNKIUIF-UUOKFMHZSA-N 0.000 description 2
- 241000699666 Mus <mouse, genus> Species 0.000 description 2
- 241000699670 Mus sp. Species 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- DRTQHJPVMGBUCF-XVFCMESISA-N Uridine Chemical compound O[C@@H]1[C@H](O)[C@@H](CO)O[C@H]1N1C(=O)NC(=O)C=C1 DRTQHJPVMGBUCF-XVFCMESISA-N 0.000 description 2
- OIRDTQYFTABQOQ-KQYNXXCUSA-N adenosine Chemical compound C1=NC=2C(N)=NC=NC=2N1[C@@H]1O[C@H](CO)[C@@H](O)[C@H]1O OIRDTQYFTABQOQ-KQYNXXCUSA-N 0.000 description 2
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- BTCSSZJGUNDROE-UHFFFAOYSA-N gamma-aminobutyric acid Chemical compound NCCCC(O)=O BTCSSZJGUNDROE-UHFFFAOYSA-N 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 150000002632 lipids Chemical class 0.000 description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 230000000242 pagocytic effect Effects 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 210000000952 spleen Anatomy 0.000 description 2
- 210000001541 thymus gland Anatomy 0.000 description 2
- OGNSCSPNOLGXSM-UHFFFAOYSA-N (+/-)-DABA Natural products NCCC(N)C(O)=O OGNSCSPNOLGXSM-UHFFFAOYSA-N 0.000 description 1
- OILXMJHPFNGGTO-UHFFFAOYSA-N (22E)-(24xi)-24-methylcholesta-5,22-dien-3beta-ol Natural products C1C=C2CC(O)CCC2(C)C2C1C1CCC(C(C)C=CC(C)C(C)C)C1(C)CC2 OILXMJHPFNGGTO-UHFFFAOYSA-N 0.000 description 1
- RQOCXCFLRBRBCS-UHFFFAOYSA-N (22E)-cholesta-5,7,22-trien-3beta-ol Natural products C1C(O)CCC2(C)C(CCC3(C(C(C)C=CCC(C)C)CCC33)C)C3=CC=C21 RQOCXCFLRBRBCS-UHFFFAOYSA-N 0.000 description 1
- OQMZNAMGEHIHNN-UHFFFAOYSA-N 7-Dehydrostigmasterol Natural products C1C(O)CCC2(C)C(CCC3(C(C(C)C=CC(CC)C(C)C)CCC33)C)C3=CC=C21 OQMZNAMGEHIHNN-UHFFFAOYSA-N 0.000 description 1
- 229930024421 Adenine Natural products 0.000 description 1
- GFFGJBXGBJISGV-UHFFFAOYSA-N Adenine Chemical compound NC1=NC=NC2=C1N=CN2 GFFGJBXGBJISGV-UHFFFAOYSA-N 0.000 description 1
- 239000002126 C01EB10 - Adenosine Substances 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 241000222680 Collybia Species 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- MIKUYHXYGGJMLM-GIMIYPNGSA-N Crotonoside Natural products C1=NC2=C(N)NC(=O)N=C2N1[C@H]1O[C@@H](CO)[C@H](O)[C@@H]1O MIKUYHXYGGJMLM-GIMIYPNGSA-N 0.000 description 1
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 description 1
- NYHBQMYGNKIUIF-UHFFFAOYSA-N D-guanosine Natural products C1=2NC(N)=NC(=O)C=2N=CN1C1OC(CO)C(O)C1O NYHBQMYGNKIUIF-UHFFFAOYSA-N 0.000 description 1
- DNVPQKQSNYMLRS-NXVQYWJNSA-N Ergosterol Natural products CC(C)[C@@H](C)C=C[C@H](C)[C@H]1CC[C@H]2C3=CC=C4C[C@@H](O)CC[C@]4(C)[C@@H]3CC[C@]12C DNVPQKQSNYMLRS-NXVQYWJNSA-N 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 description 1
- CKLJMWTZIZZHCS-REOHCLBHSA-N L-aspartic acid Chemical compound OC(=O)[C@@H](N)CC(O)=O CKLJMWTZIZZHCS-REOHCLBHSA-N 0.000 description 1
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 description 1
- KDXKERNSBIXSRK-YFKPBYRVSA-N L-lysine Chemical compound NCCCC[C@H](N)C(O)=O KDXKERNSBIXSRK-YFKPBYRVSA-N 0.000 description 1
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 description 1
- 239000004472 Lysine Substances 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229930195725 Mannitol Natural products 0.000 description 1
- 241000866536 Odontotermes formosanus Species 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 241000576755 Sclerotia Species 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229960000643 adenine Drugs 0.000 description 1
- 229960005305 adenosine Drugs 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 235000001014 amino acid Nutrition 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 235000003704 aspartic acid Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229940076810 beta sitosterol Drugs 0.000 description 1
- DRTQHJPVMGBUCF-PSQAKQOGSA-N beta-L-uridine Natural products O[C@H]1[C@@H](O)[C@H](CO)O[C@@H]1N1C(=O)NC(=O)C=C1 DRTQHJPVMGBUCF-PSQAKQOGSA-N 0.000 description 1
- LGJMUZUPVCAVPU-UHFFFAOYSA-N beta-Sitostanol Natural products C1CC2CC(O)CCC2(C)C2C1C1CCC(C(C)CCC(CC)C(C)C)C1(C)CC2 LGJMUZUPVCAVPU-UHFFFAOYSA-N 0.000 description 1
- OQFSQFPPLPISGP-UHFFFAOYSA-N beta-carboxyaspartic acid Natural products OC(=O)C(N)C(C(O)=O)C(O)=O OQFSQFPPLPISGP-UHFFFAOYSA-N 0.000 description 1
- NJKOMDUNNDKEAI-UHFFFAOYSA-N beta-sitosterol Natural products CCC(CCC(C)C1CCC2(C)C3CC=C4CC(O)CCC4C3CCC12C)C(C)C NJKOMDUNNDKEAI-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 210000000748 cardiovascular system Anatomy 0.000 description 1
- 235000012000 cholesterol Nutrition 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- DNVPQKQSNYMLRS-SOWFXMKYSA-N ergosterol Chemical compound C1[C@@H](O)CC[C@]2(C)[C@H](CC[C@]3([C@H]([C@H](C)/C=C/[C@@H](C)C(C)C)CC[C@H]33)C)C3=CC=C21 DNVPQKQSNYMLRS-SOWFXMKYSA-N 0.000 description 1
- 239000003797 essential amino acid Substances 0.000 description 1
- 235000020776 essential amino acid Nutrition 0.000 description 1
- 229960003692 gamma aminobutyric acid Drugs 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 235000013922 glutamic acid Nutrition 0.000 description 1
- 239000004220 glutamic acid Substances 0.000 description 1
- 229940029575 guanosine Drugs 0.000 description 1
- 235000013402 health food Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 210000002540 macrophage Anatomy 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000000594 mannitol Substances 0.000 description 1
- 235000010355 mannitol Nutrition 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007721 medicinal effect Effects 0.000 description 1
- 210000000653 nervous system Anatomy 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 229930182490 saponin Natural products 0.000 description 1
- 150000007949 saponins Chemical class 0.000 description 1
- 235000017709 saponins Nutrition 0.000 description 1
- KZJWDPNRJALLNS-VJSFXXLFSA-N sitosterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CC[C@@H](CC)C(C)C)[C@@]1(C)CC2 KZJWDPNRJALLNS-VJSFXXLFSA-N 0.000 description 1
- 229950005143 sitosterol Drugs 0.000 description 1
- 239000007962 solid dispersion Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- DRTQHJPVMGBUCF-UHFFFAOYSA-N uracil arabinoside Natural products OC1C(O)C(CO)OC1N1C(=O)NC(=O)C=C1 DRTQHJPVMGBUCF-UHFFFAOYSA-N 0.000 description 1
- 229940045145 uridine Drugs 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- 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
- 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
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/20—Pills, tablets, discs, rods
- A61K9/2004—Excipients; Inactive ingredients
- A61K9/2022—Organic macromolecular compounds
- A61K9/2031—Organic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polyethylene glycol, polyethylene oxide, poloxamers
-
- 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
- A61P37/04—Immunostimulants
-
- 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
- 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
-
- 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
- A61K36/06—Fungi, e.g. yeasts
- A61K36/062—Ascomycota
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Medicinal Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Animal Behavior & Ethology (AREA)
- Molecular Biology (AREA)
- Veterinary Medicine (AREA)
- Immunology (AREA)
- Pharmacology & Pharmacy (AREA)
- Engineering & Computer Science (AREA)
- Polymers & Plastics (AREA)
- Epidemiology (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Biochemistry (AREA)
- Sustainable Development (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Materials Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Mycology (AREA)
- Nutrition Science (AREA)
- Food Science & Technology (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention relates to the technical field of health products, solves the problem of drug effect reduction of a dripping pill caused by poor heat resistance of polysaccharide, and discloses a preparation method of a wulingshen polysaccharide dripping pill. The preparation method of the Wulingshen polysaccharide dropping pill comprises the steps of firstly crushing Wulingshen, then degreasing and drying, adding cellulase, carrying out enzymolysis to remove cellulose, then carrying out heating extraction to obtain Wulingshen polysaccharide, carrying out rotary evaporation concentration, alcohol precipitation, dialysis and drying to obtain Wulingshen polysaccharide, finally mixing and melting dropping pill substrate polyethylene glycol 4000 and polyethylene glycol 6000, adding the mixed and melted liquid into a liquid storage chamber of a dropping pill machine, injecting Wulingshen polysaccharide ethanol water solution into a dropping tube of the dropping pill machine in the dropping process, and carrying out cooling forming, separation, washing and drying to obtain the Wulingshen polysaccharide dropping pill. The Wulingshen polysaccharide dropping pill can play a stronger role of medicine and has better effect of improving the immunity of human bodies.
Description
Technical Field
The invention relates to the technical field of health products, in particular to a preparation method of a Wulingshen polysaccharide dropping pill.
Background
Wulingshen is one of the medicinal materials. The mycelium is white and has a diameter of 8-14 μm, and is woven into a net shape and densely distributed in the waste odontotermes formosanus fungus garden. When mature, part of the hyphae aggregate to form sclerotia. The sclerotium is spherical, oval or ovoid, so it is called egg of Collybia albuminosa. The outer surface is brown or black, the diameter is 1.5-8cm, a round pit is arranged at the joint of the sclerotium and the hyphae, and the sclerotium gradually separates from the hyphae after growing to form a navel shape. Contains polysaccharide, protein, and trace elements such as iron, manganese, and tin. Contains 19 amino acids (9 essential amino acids) such as adenosine, adenine, uridine, guanosine, sugar, mannitol, ergosterol, cholesterol, beta-sitosterol, aspartic acid, glutamic acid, gamma-aminobutyric acid, lysine and the like, and also contains a plurality of components such as iron, zinc, manganese, copper, phosphorus, magnesium, calcium, germanium, vitamins (B1, B2, B6, E, A, D2, K1) and the like, wherein the wulingshen polysaccharide has the effects of enhancing immunity and resisting oxidation. Chinese patent publication No. CN105395496 discloses a ginseng drop pill and a preparation method thereof, wherein the ginseng drop pill is a drop pill preparation prepared from ginseng total saponins, ginseng polysaccharide and polyethylene glycol, and is prepared by adopting the solid dispersion technical principle of the modern pharmaceutical technology, and the ginseng drop pill has the characteristics of high uniformity, high dissolution rate, high bioavailability and the like, and mainly has antitumor activity, nervous system activity, cardiovascular system activity and the like. The preparation process of the dripping pill adopts boiling water extraction and the ginseng polysaccharide and the dripping pill substrate are melted and mixed at the temperature of 80-100 ℃, and because the thermal stability of the polysaccharide is poor, the bioactivity of the polysaccharide is damaged and changed when the polysaccharide is in the temperature range for a long time, thereby reducing the drug effect of the polysaccharide dripping pill.
Disclosure of Invention
The invention aims to overcome the problem that the drug effect of a dripping pill is reduced due to poor heat resistance of polysaccharides in the prior art, and provides a preparation method of the wulingshen polysaccharide.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a Wulingshen polysaccharide dropping pill comprises the following steps:
1) pulverizing radix Linderae, adding into Soxhlet extractor, defatting with petroleum ether for 10-15 hr, and oven drying to obtain dried radix Linderae powder;
2) adding radix Linderae powder into distilled water to form suspension, heating to 48-52 deg.C, adding cellulase 0.5-1.5 wt% of the suspension, performing enzymolysis for 3-5 hr, and heating for 8-12 hr;
3) centrifuging at 7000-8500r/min for 10-20min, filtering, collecting supernatant, and concentrating by rotary evaporation to obtain concentrated solution;
4) adding absolute ethanol into the concentrated solution for alcohol precipitation, standing for 8-12h, separating precipitate, adding the precipitate into distilled water according to the mass ratio of 1:30-50 for dissolution, performing centrifugal dialysis for 65-75h, and performing vacuum freeze drying on the dialyzed substance to obtain the polysaccharide of the lindera aggregata;
5) mixing the dripping pill matrix polyethylene glycol 4000 and polyethylene glycol 6000, heating to melt at 92-94 deg.C to obtain a mixed solution, and maintaining the temperature for use;
6) adding the wulingshen polysaccharide into an ethanol water solution, stirring and dissolving to obtain the wulingshen polysaccharide ethanol water solution for later use; adding the mixed solution into a liquid storage chamber of a pill dropping machine, injecting an ethanol water solution of the polysaccharide of the radix Linderae from a dropper of the pill dropping machine during the dropping process, dropping into the cooling liquid at a speed of 25-30 drops per minute for forming, separating, washing and drying to obtain the final product.
The invention firstly uses petroleum ether to remove lipid substances, and then adds cellulase to carry out enzymolysis to remove cellulose, thereby avoiding the reduction of the content and purity of the effective component of the polysaccharide of the black ginseng in the dripping pill preparation caused by the lipid substances, the cellulose and other impurity substances, and improving the drug effect; enzymolysis at 48-52 deg.C during enzymolysis process, which will not cause decomposition of radix Linderae polysaccharide and avoid activity reduction of radix Linderae polysaccharide; in addition, in the process of mixing the wulingshen polysaccharide with the dropping pill matrix polyethylene glycol 4000 and polyethylene glycol 6000, the method adopted by the prior art is to directly mix the wulingshen polysaccharide with the melted dropping pill matrix polyethylene glycol 4000 and polyethylene glycol 6000, and then add the mixture into a liquid storage chamber of a dropping pill machine to keep the temperature for a dropping procedure, because the melting temperature of the polyethylene glycol 4000 and the polyethylene glycol 6000 is higher than 80 ℃, the activity of the wulingshen polysaccharide is greatly reduced due to the long-time temperature of the wulingshen polysaccharide, so that the medicinal effect of the wulingshen polysaccharide is greatly reduced, the invention solves the problem, firstly heats the dropping pill matrix polyethylene glycol 4000 and the polyethylene glycol 6000 to a melting state, then sends the dropping pill matrix polyethylene glycol 4000 and the polyethylene glycol 6000 into the liquid storage chamber of the dropping pill machine, adds the wulingshen polysaccharide into the dropping pill matrix in the dropping procedure, immediately drops the dropping pill matrix polyethylene glycol, the influence of short-time high temperature on the molecular structure of the wulingshen polysaccharide is small, so that the higher activity of the wulingshen polysaccharide is kept, and the drug effect of the dripping pill is greatly improved compared with the prior art. In the research process, the invention finds that the high activity of the wulingshen polysaccharide can be maintained by mixing the wulingshen polysaccharide with the molten matrix in a short time, but the problem of uneven mixing can be caused by the short time contact of the wulingshen polysaccharide and the molten matrix.
Preferably, the mass ratio of the wulingshen powder to the distilled water in the step 2) is 1: 15-25.
Preferably, the heating and extracting temperature in the step 2) is 55-58 ℃.
The invention controls the extraction temperature of the wulingshen polysaccharide to be 55-58 ℃, and the stability of the wulingshen polysaccharide can not be influenced at the temperature, in addition, the invention adopts the method of crushing wulingshen into powder and extracting wulingshen polysaccharide at low temperature for a long time, thereby fully extracting the wulingshen polysaccharide in wulingshen as far as possible and improving the utilization rate of raw materials.
Preferably, the volume of the absolute ethyl alcohol in the step 4) is 4 to 6 times of the volume of the concentrated solution.
Preferably, the mass ratio of the polyethylene glycol 4000 to the polyethylene glycol 6000 in the step 5) is 1: 0.5-0.8.
Preferably, the mass fraction of the ethanol water solution in the step 6) is 65-70%.
The inventor researches and discovers that the mass fraction of the ethanol water solution is controlled to be 65-70%, so that the lindera aggregata polysaccharide can be uniformly mixed with the dripping pill substrate in the shortest time.
Preferably, the concentration of the polysaccharide of the radix linderae in the dropper in the step 6) is controlled to be 25-30 wt%.
Preferably, the cooling liquid in the step 6) is at least one of simethicone, liquid paraffin, rape oil and tea oil.
Therefore, the invention has the following beneficial effects:
1) the invention carries out enzymolysis and extraction on the wulingshen under the condition of low temperature, thereby avoiding the activity reduction caused by the decomposition of wulingshen polysaccharide under the condition of high temperature; 2) the Wulingshen polysaccharide is added into the matrix of the dripping pill in the dropping process, and because the Wulingshen polysaccharide is immediately dropped into the cooling liquid for cooling after being contacted and mixed with the molten matrix for a short time, the influence of the short-time high temperature on the molecular structure of the Wulingshen polysaccharide is small, thereby keeping the higher activity of the Wulingshen polysaccharide.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
In the present invention, unless otherwise specified, all the raw materials and equipment used are commercially available or commonly used in the art, and the methods in the examples are conventional in the art unless otherwise specified.
Example 1
The preparation method of the Wulingshen polysaccharide dropping pill comprises the following steps:
1) pulverizing radix Linderae, adding into Soxhlet extractor, defatting with petroleum ether for 13 hr, and oven drying to obtain dried radix Linderae powder;
2) adding the Wulingshen powder into distilled water according to the mass ratio of 1:20 to form a suspension, heating to 50 ℃, adding cellulase accounting for 1% of the mass of the suspension, performing enzymolysis for 4 hours, and heating and extracting at 56 ℃ for 10 hours;
3) centrifuging at 8000r/min for 15min, filtering, collecting supernatant, and rotary evaporating for concentration to obtain concentrated solution; 4) adding absolute ethyl alcohol with the volume 5 times of that of the concentrated solution into the concentrated solution for alcohol precipitation, standing for 10h, separating precipitates, adding the precipitates into distilled water according to the mass ratio of 1:40 for dissolution, performing centrifugal dialysis for 70h, and performing vacuum freeze drying on substances obtained by dialysis to obtain the wulingshen polysaccharide;
5) mixing the dripping pill matrix polyethylene glycol 4000 and polyethylene glycol 6000 at a mass ratio of 1:0.6, heating to melt at 93 ℃ to obtain a mixed solution, and keeping the temperature for later use;
6) adding the wulingshen polysaccharide into an ethanol water solution with the mass concentration of 68% according to the mass ratio of 1:8, and stirring for dissolving to obtain the wulingshen polysaccharide ethanol water solution for later use; adding the mixed solution into a liquid storage chamber of a pill dropping machine, injecting an ethanol water solution of the radix Linderae polysaccharide from a dropper of the pill dropping machine in the dropping process, controlling the concentration of the radix Linderae polysaccharide in the dropper to be 27 wt%, dropping the radix Linderae polysaccharide into cooling liquid simethicone at the speed of 28 drops per minute for forming, separating, washing and drying to obtain the product.
Example 2
The preparation method of the Wulingshen polysaccharide dropping pill comprises the following steps:
1) pulverizing radix Linderae, adding into Soxhlet extractor, defatting with petroleum ether for 11 hr, and oven drying to obtain dried radix Linderae powder;
2) adding the Wulingshen powder into distilled water according to the mass ratio of 1:16 to form a suspension, heating to 49 ℃, adding cellulase accounting for 0.8 percent of the mass of the suspension, performing enzymolysis for 3.5 hours, and heating and extracting at 55.5 ℃ for 8.5 hours;
3) centrifuging at 8000r/min for 11min, filtering, collecting supernatant, and rotary evaporating for concentration to obtain concentrated solution;
4) adding absolute ethyl alcohol with the volume 4 times that of the concentrated solution into the concentrated solution for alcohol precipitation, standing for 8h, separating precipitates, adding the precipitates into distilled water according to the mass ratio of 1:35 for dissolution, performing centrifugal dialysis for 66h, and performing vacuum freeze drying on substances obtained by dialysis to obtain the wulingshen polysaccharide;
5) mixing the dripping pill matrix polyethylene glycol 4000 and polyethylene glycol 6000 at a mass ratio of 1:0.6, heating to melt at 92.5 deg.C to obtain a molten mixture, and maintaining the temperature for use;
6) adding the wulingshen polysaccharide into 65% ethanol water solution according to the mass ratio of 1:6, stirring and dissolving to obtain the wulingshen polysaccharide ethanol water solution for later use; adding the mixed solution into a liquid storage chamber of a pill dropping machine, injecting an ethanol water solution of the radix Linderae polysaccharide from a dropper of the pill dropping machine in the dropping process, controlling the concentration of the radix Linderae polysaccharide in the dropper to be 26 wt%, dropping the radix Linderae polysaccharide into liquid paraffin of cooling liquid at the speed of 26 drops per minute for molding, separating, washing and drying to obtain the product.
Example 3
The preparation method of the Wulingshen polysaccharide dropping pill comprises the following steps:
1) pulverizing radix Linderae, adding into Soxhlet extractor, defatting with petroleum ether for 14 hr, and oven drying to obtain dried radix Linderae powder;
2) adding the Wulingshen powder into distilled water according to the mass ratio of 1:23 to form a suspension, heating to 51 ℃, adding cellulase accounting for 1.3 percent of the mass of the suspension, performing enzymolysis for 4.5 hours, and heating and extracting at 57 ℃ for 11 hours;
3) centrifuging at 8000r/min for 18min, filtering, collecting supernatant, and rotary evaporating for concentration to obtain concentrated solution;
4) adding absolute ethyl alcohol with the volume 6 times that of the concentrated solution into the concentrated solution for alcohol precipitation, standing for 11h, separating precipitates, adding the precipitates into distilled water according to the mass ratio of 1:45 for dissolution, performing centrifugal dialysis for 73h, and performing vacuum freeze drying on substances obtained by dialysis to obtain the wulingshen polysaccharide;
5) mixing the dripping pill matrix polyethylene glycol 4000 and polyethylene glycol 6000 at a mass ratio of 1:0.7, heating to melt at 93.5 deg.C to obtain a mixed solution, and maintaining the temperature for use;
6) adding the wulingshen polysaccharide into 70% ethanol water solution according to the mass ratio of 1:9, stirring and dissolving to obtain the wulingshen polysaccharide ethanol water solution for later use; adding the mixed solution into a liquid storage chamber of a pill dropping machine, injecting an ethanol water solution of the radix Linderae polysaccharide from a dropper of the pill dropping machine in the dropping process, controlling the concentration of the radix Linderae polysaccharide in the dropper to be 28 wt%, dropping the radix Linderae polysaccharide into cooling liquid rape oil at the speed of 30 drops per minute for forming, separating, washing and drying to obtain the Chinese medicinal preparation.
Example 4
The preparation method of the Wulingshen polysaccharide dropping pill comprises the following steps:
1) pulverizing radix Linderae, adding into Soxhlet extractor, defatting with petroleum ether for 15 hr, and oven drying to obtain dried radix Linderae powder;
2) adding the Wulingshen powder into distilled water according to the mass ratio of 1:25 to form a suspension, heating to 52 ℃, adding cellulase accounting for 1.5 percent of the mass of the suspension, performing enzymolysis for 5 hours, and heating and extracting at 58 ℃ for 12 hours;
3) centrifuging at 8500r/min for 20min, filtering, collecting supernatant, and concentrating by rotary evaporation to obtain concentrated solution;
4) adding absolute ethyl alcohol with the volume 6 times that of the concentrated solution into the concentrated solution for alcohol precipitation, standing for 12h, separating precipitates, adding the precipitates into distilled water according to the mass ratio of 1:50 for dissolution, performing centrifugal dialysis for 75h, and performing vacuum freeze drying on substances obtained by dialysis to obtain the wulingshen polysaccharide;
5) mixing the dripping pill matrix polyethylene glycol 4000 and polyethylene glycol 6000 at a mass ratio of 1:0.8, heating to melt at 94 ℃ to obtain a mixed solution, and keeping the temperature for later use;
6) adding the wulingshen polysaccharide into 70% ethanol water solution according to the mass ratio of 1:10, stirring and dissolving to obtain the wulingshen polysaccharide ethanol water solution for later use; adding the mixed solution into a liquid storage chamber of a pill dropping machine, injecting an ethanol water solution of the radix Linderae polysaccharide from a dropper of the pill dropping machine in the dropping process, controlling the concentration of the radix Linderae polysaccharide in the dropper to be 30wt%, dropping into cooling liquid tea oil at a speed of 30 drops per minute for forming, separating, washing and drying to obtain the product.
Example 5
The preparation method of the Wulingshen polysaccharide dropping pill comprises the following steps:
1) pulverizing radix Linderae, adding into Soxhlet extractor, defatting with petroleum ether for 10 hr, and oven drying to obtain dried radix Linderae powder;
2) adding the Wulingshen powder into distilled water according to the mass ratio of 1:15 to form a suspension, heating to 48 ℃, adding cellulase accounting for 0.5 percent of the mass of the suspension, performing enzymolysis for 3 hours, and heating and extracting at 55 ℃ for 8 hours;
3) centrifuging at 7000r/min for 10min, filtering, collecting supernatant, and concentrating by rotary evaporation to obtain concentrated solution;
4) adding absolute ethyl alcohol with the volume 4 times that of the concentrated solution into the concentrated solution for alcohol precipitation, standing for 8h, separating precipitates, adding the precipitates into distilled water according to the mass ratio of 1:30 for dissolution, performing centrifugal dialysis for 65h, and performing vacuum freeze drying on substances obtained by dialysis to obtain the wulingshen polysaccharide;
5) mixing the dripping pill matrix polyethylene glycol 4000 and polyethylene glycol 6000 at a mass ratio of 1:0.5, heating to melt at 92 ℃ to obtain a mixed solution, and keeping the temperature for later use;
6) adding the wulingshen polysaccharide into 65% ethanol water solution according to the mass ratio of 1:5, stirring and dissolving to obtain the wulingshen polysaccharide ethanol water solution for later use; adding the mixed solution into a liquid storage chamber of a pill dropping machine, injecting an ethanol water solution of the radix Linderae polysaccharide from a dropper of the pill dropping machine in the dropping process, controlling the concentration of the radix Linderae polysaccharide in the dropper to be 25 wt%, dropping the radix Linderae polysaccharide into liquid paraffin of cooling liquid at the speed of 25 drops per minute for molding, separating, washing and drying to obtain the product.
Comparative example 1
Comparative example 1 is a conventional dripping pill of radix Linderae Glaucae polysaccharide prepared on the market.
Test of
The traditional Chinese medicine composition is prepared by taking a medium-dose dripping pill for a mouse according to a health food functional evaluation program and a detection method, and then detecting the phagocytic function, the spleen index and the thymus index of the macrophage of the mouse, wherein the results are as follows:
the comparison of the examples and the comparative examples can obtain that the phagocytic index, the spleen index and the thymus index of the mice of the pill preparation are obviously higher than those of the common pill preparation purchased in the market after the pill preparation is taken by the mice, and the pill preparation has higher nonspecific immunity function and regulation function to organisms.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (7)
1. A preparation method of a Wulingshen polysaccharide dropping pill is characterized by comprising the following steps:
1) pulverizing radix Linderae, adding into Soxhlet extractor, defatting with petroleum ether for 10-15 hr, and oven drying to obtain dried radix Linderae powder;
2) adding radix Linderae powder into distilled water to form suspension, heating to 48-52 deg.C, adding cellulase 0.5-1.5 wt% of the suspension, performing enzymolysis for 3-5 hr, and heating for 8-12 hr;
3) centrifuging at 7000-8500r/min for 10-20min, filtering, collecting supernatant, and concentrating by rotary evaporation to obtain concentrated solution;
4) adding absolute ethanol into the concentrated solution for alcohol precipitation, standing for 8-12h, separating precipitate, adding the precipitate into distilled water according to the mass ratio of 1:30-50 for dissolution, performing centrifugal dialysis for 65-75h, and performing vacuum freeze drying on the dialyzed substance to obtain the polysaccharide of the lindera aggregata;
5) mixing the dripping pill matrix polyethylene glycol 4000 and polyethylene glycol 6000, heating to melt at 92-94 deg.C to obtain a mixed solution, and maintaining the temperature for use;
6) adding the wulingshen polysaccharide into 65-70% ethanol water solution according to the mass ratio of 1:5-10, stirring and dissolving to obtain the wulingshen polysaccharide ethanol water solution for later use; adding the mixed solution into a liquid storage chamber of a pill dropping machine, injecting an ethanol water solution of the polysaccharide of the radix Linderae from a dropper of the pill dropping machine during the dropping process, dropping into the cooling liquid at a speed of 25-30 drops per minute for forming, separating, washing and drying to obtain the final product.
2. The method for preparing wuling ginseng polysaccharide dripping pills according to claim 1, wherein the mass ratio of wuling ginseng powder to distilled water in step 2) is 1: 15-25.
3. The method for preparing wulingshen polysaccharide dripping pills according to claim 1, wherein the heating and extracting temperature in step 2) is 55-58 ℃.
4. The method for preparing wulingshen polysaccharide dripping pills according to claim 1, wherein the volume of the absolute ethyl alcohol in the step 4) is 4-6 times of the volume of the concentrated solution.
5. The method for preparing wulingshen polysaccharide dripping pills according to claim 1, wherein the mass ratio of polyethylene glycol 4000 to polyethylene glycol 6000 in the step 5) is 1: 0.5-0.8.
6. The method for preparing wulingshen polysaccharide dripping pills according to claim 1, wherein the concentration of wulingshen polysaccharide in the dripping tube in the step 6) is controlled to be 25-30 wt%.
7. The method for preparing wulingshen polysaccharide dripping pills according to claim 1, wherein the cooling liquid in step 6) is at least one of simethicone, liquid paraffin, rape oil and tea oil.
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| 茶叶功效成分研究进展;李娟;《浙江科技学院学报》;20051231;第17卷(第4期);第285-289页，尤其是第287页右栏"茶多糖提取工艺"部分 * |
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