CN110801477A - Preparation method of particles for stopping bleeding and regulating menstruation - Google Patents
Preparation method of particles for stopping bleeding and regulating menstruation Download PDFInfo
- Publication number
- CN110801477A CN110801477A CN201911153686.7A CN201911153686A CN110801477A CN 110801477 A CN110801477 A CN 110801477A CN 201911153686 A CN201911153686 A CN 201911153686A CN 110801477 A CN110801477 A CN 110801477A
- Authority
- CN
- China
- Prior art keywords
- powder
- parts
- extract
- water
- donkey
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000002245 particle Substances 0.000 title claims description 57
- 230000005906 menstruation Effects 0.000 title claims description 28
- 230000000740 bleeding effect Effects 0.000 title claims description 24
- 230000001105 regulatory effect Effects 0.000 title claims description 24
- 239000000843 powder Substances 0.000 claims abstract description 132
- 239000000284 extract Substances 0.000 claims abstract description 104
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 52
- 235000006533 astragalus Nutrition 0.000 claims abstract description 50
- 239000008187 granular material Substances 0.000 claims abstract description 42
- 108010010803 Gelatin Proteins 0.000 claims abstract description 40
- 229920000159 gelatin Polymers 0.000 claims abstract description 40
- 239000008273 gelatin Substances 0.000 claims abstract description 40
- 235000019322 gelatine Nutrition 0.000 claims abstract description 40
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 40
- 240000007126 Citrus medica var. sarcodactylis Species 0.000 claims abstract description 39
- 238000002156 mixing Methods 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 30
- 229920000858 Cyclodextrin Polymers 0.000 claims abstract description 26
- 241001061264 Astragalus Species 0.000 claims abstract description 25
- 239000001116 FEMA 4028 Substances 0.000 claims abstract description 25
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims abstract description 25
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims abstract description 25
- 229960004853 betadex Drugs 0.000 claims abstract description 25
- 210000004233 talus Anatomy 0.000 claims abstract description 25
- 239000000341 volatile oil Substances 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 24
- 230000005484 gravity Effects 0.000 claims abstract description 18
- 238000001291 vacuum drying Methods 0.000 claims abstract description 18
- 241000007126 Codonopsis pilosula Species 0.000 claims abstract description 17
- 244000307697 Agrimonia eupatoria Species 0.000 claims abstract description 16
- 241000123589 Dipsacus Species 0.000 claims abstract description 16
- 241000123069 Ocyurus chrysurus Species 0.000 claims abstract description 16
- 235000006484 Paeonia officinalis Nutrition 0.000 claims abstract description 15
- 235000000125 common agrimony Nutrition 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 230000002439 hemostatic effect Effects 0.000 claims abstract description 4
- 238000003825 pressing Methods 0.000 claims description 29
- 238000007906 compression Methods 0.000 claims description 27
- 230000006835 compression Effects 0.000 claims description 27
- 241000125175 Angelica Species 0.000 claims description 26
- 235000001287 Guettarda speciosa Nutrition 0.000 claims description 26
- 241000045403 Astragalus propinquus Species 0.000 claims description 25
- 238000007873 sieving Methods 0.000 claims description 25
- 238000001035 drying Methods 0.000 claims description 21
- 239000009636 Huang Qi Substances 0.000 claims description 19
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 19
- 229930006000 Sucrose Natural products 0.000 claims description 19
- 239000005720 sucrose Substances 0.000 claims description 18
- 238000007908 dry granulation Methods 0.000 claims description 16
- 150000001875 compounds Chemical class 0.000 claims description 15
- 229920000881 Modified starch Polymers 0.000 claims description 14
- 241001106477 Paeoniaceae Species 0.000 claims description 14
- 238000010298 pulverizing process Methods 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 241000382455 Angelica sinensis Species 0.000 claims description 9
- 238000009835 boiling Methods 0.000 claims description 9
- 239000000110 cooling liquid Substances 0.000 claims description 9
- 238000003809 water extraction Methods 0.000 claims description 9
- 238000000605 extraction Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 6
- VYQNWZOUAUKGHI-UHFFFAOYSA-N monobenzone Chemical compound C1=CC(O)=CC=C1OCC1=CC=CC=C1 VYQNWZOUAUKGHI-UHFFFAOYSA-N 0.000 claims description 5
- 241000756943 Codonopsis Species 0.000 claims description 3
- 241000726221 Gemma Species 0.000 claims description 3
- 235000020985 whole grains Nutrition 0.000 claims description 3
- 238000005538 encapsulation Methods 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 3
- 238000004821 distillation Methods 0.000 abstract description 2
- 241000213006 Angelica dahurica Species 0.000 abstract 6
- 244000170916 Paeonia officinalis Species 0.000 abstract 1
- 238000005469 granulation Methods 0.000 description 18
- 230000003179 granulation Effects 0.000 description 18
- 229960004793 sucrose Drugs 0.000 description 17
- 230000001276 controlling effect Effects 0.000 description 10
- 238000005086 pumping Methods 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 9
- 238000001694 spray drying Methods 0.000 description 8
- 238000005550 wet granulation Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 238000006073 displacement reaction Methods 0.000 description 5
- 230000023597 hemostasis Effects 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- 239000007779 soft material Substances 0.000 description 4
- 238000003892 spreading Methods 0.000 description 4
- 239000000080 wetting agent Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 229940107666 astragalus root Drugs 0.000 description 3
- 230000033228 biological regulation Effects 0.000 description 3
- 239000008280 blood Substances 0.000 description 3
- 210000004369 blood Anatomy 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 235000016993 Agrimonia Nutrition 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000002671 adjuvant Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 108010052008 colla corii asini Proteins 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 239000008213 purified water Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 206010000060 Abdominal distension Diseases 0.000 description 1
- 206010024642 Listless Diseases 0.000 description 1
- 229920000168 Microcrystalline cellulose Polymers 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 210000001015 abdomen Anatomy 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 208000002173 dizziness Diseases 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 208000017971 listlessness Diseases 0.000 description 1
- 230000002175 menstrual effect Effects 0.000 description 1
- 230000003821 menstrual periods Effects 0.000 description 1
- 235000019813 microcrystalline cellulose Nutrition 0.000 description 1
- 239000008108 microcrystalline cellulose Substances 0.000 description 1
- 229940016286 microcrystalline cellulose Drugs 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 238000001256 steam distillation Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 238000009736 wetting Methods 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)
- A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
- A61K36/481—Astragalus (milkvetch)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K35/00—Medicinal preparations containing materials or reaction products thereof with undetermined constitution
- A61K35/12—Materials from mammals; Compositions comprising non-specified tissues or cells; Compositions comprising non-embryonic stem cells; Genetically modified cells
- A61K35/36—Skin; Hair; Nails; Sebaceous glands; Cerumen; Epidermis; Epithelial cells; Keratinocytes; Langerhans cells; Ectodermal cells
-
- 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)
-
- 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)
- A61K36/23—Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
- A61K36/232—Angelica
-
- 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)
- A61K36/34—Campanulaceae (Bellflower family)
- A61K36/344—Codonopsis
-
- 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)
- A61K36/65—Paeoniaceae (Peony family), e.g. Chinese peony
-
- 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)
- A61K36/71—Ranunculaceae (Buttercup family), e.g. larkspur, hepatica, hydrastis, columbine or goldenseal
-
- 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)
- A61K36/73—Rosaceae (Rose family), e.g. strawberry, chokeberry, blackberry, pear or firethorn
-
- 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)
- A61K36/74—Rubiaceae (Madder family)
-
- 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)
- A61K36/75—Rutaceae (Rue family)
- A61K36/752—Citrus, e.g. lime, orange or lemon
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/50—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates
- A61K47/69—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the conjugate being characterised by physical or galenical forms, e.g. emulsion, particle, inclusion complex, stent or kit
- A61K47/6949—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the conjugate being characterised by physical or galenical forms, e.g. emulsion, particle, inclusion complex, stent or kit inclusion complexes, e.g. clathrates, cavitates or fullerenes
- A61K47/6951—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the conjugate being characterised by physical or galenical forms, e.g. emulsion, particle, inclusion complex, stent or kit inclusion complexes, e.g. clathrates, cavitates or fullerenes using cyclodextrin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P15/00—Drugs for genital or sexual disorders; Contraceptives
-
- 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
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
Landscapes
- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Medicinal Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Biotechnology (AREA)
- Medical Informatics (AREA)
- Mycology (AREA)
- Microbiology (AREA)
- Botany (AREA)
- Alternative & Traditional Medicine (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Cell Biology (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Reproductive Health (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Organic Chemistry (AREA)
- Endocrinology (AREA)
- Dermatology (AREA)
- Biomedical Technology (AREA)
- Developmental Biology & Embryology (AREA)
- Immunology (AREA)
- Virology (AREA)
- Zoology (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention relates to a preparation method of a hemostatic and menstruation-regulating granule, which comprises the following steps of preparing materials according to a formula of the hemostatic and menstruation-regulating granule, mixing Chinese angelica and fingered citron, extracting by a distillation method, collecting volatile oil, obtaining mixed extract of the Chinese angelica and the fingered citron and mixed dregs, clathrating the volatile oil by β -cyclodextrin to obtain β -cyclodextrin clathrate, crushing donkey-hide gelatin into donkey-hide gelatin powder, taking half of the Chinese angelica, crushing to respectively obtain superfine powder of the Chinese astragalus and coarse powder of the Chinese astragalus, mixing the coarse powder of the Chinese angelica, the mixed dregs of the Chinese angelica and the fingered citron, codonopsis pilosula, white paeony root, hairyvein agrimony, madder and teasel root, extracting by water, filtering and removing impurities to obtain water, then mixing the water with the mixed extract of the Chinese angelica and the fingered citron, concentrating to obtain extract with a specific gravity of 1.25-1.35, carrying out vacuum drying treatment on the extract, crushing to obtain dry extract powder, mixing the dry extract powder, the donkey-hide gelatin powder, the superfine powder and auxiliary materials.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicine preparations, in particular to a preparation method of a granule for stopping bleeding and regulating menstruation.
Background
The granule for stopping bleeding and regulating menstruation is mainly prepared from nine medicinal materials such as donkey-hide gelatin, Chinese angelica, fingered citron, astragalus, codonopsis pilosula, white paeony root and the like, has the effects of tonifying qi and enriching blood, and stopping bleeding and regulating menstruation, and can be used for treating deficiency of both qi and blood during menstrual period extension caused by ring insertion, symptoms of menstrual blood overdue, pale menstruation, listlessness, dizziness, lower abdomen distention, pale tongue, thin and white fur and thready and weak pulse.
At present, the preparation of the hemostasis and menstruation-regulating granules mainly adopts a wet granulation process and a one-step granulation process. Wherein, in the wet granulation process, the traditional Chinese medicine extract is concentrated into extract with the relative density of about 1.1, then spray drying is carried out to obtain dry extract powder, then donkey-hide gelatin powder, astragalus superfine powder and a proper amount of auxiliary materials are added according to the prescription, the even mixing is carried out, the wetting agent is added for granulation, and the drying and the granule finishing are carried out. In the wet granulation process, on one hand, the yield of dry extract powder is low due to the fact that the wet particles are easy to stick to the wall in the spray drying process of the extract, and on the other hand, the wet particles are easy to stick to form blocks or collide to be loose to form powder due to unstable structure when not being dried, so that the yield of qualified particles is low, and the particle size is not uniform.
And (2) directly performing spray granulation on the extract by a one-step granulation process, taking donkey-hide gelatin medium powder, astragalus superfine powder, sucrose powder and pregelatinized starch as bottom materials, mixing the extract and the pregelatinized starch to be used as a bonding agent, performing spray granulation, setting the air inlet temperature to be 50-80 ℃, finishing granules, adding the volatile oil inclusion compound, and uniformly mixing to obtain the particles for stopping bleeding and regulating menstruation. Although the process omits the step of spray drying of concentrated extract, the formula contains donkey-hide gelatin and cane sugar, so that the material has strong viscosity, the material is easily softened and adhered to the inner wall of equipment when being subjected to spray granulation, the hygroscopicity is strong, the bed is easy to collapse, the operation of the one-step granulation process is difficult, and the prepared particles are loose and small, have strong hygroscopicity and are not favorable for storage.
Therefore, the preparation method of the hemostatic and menstruation-regulating granule needs to be further improved.
Disclosure of Invention
Based on the above, the preparation method of the particles for stopping bleeding and regulating menstruation is provided, and the preparation efficiency and the product percent of pass can be improved.
A preparation method of a granule for stopping bleeding and regulating menstruation comprises the following steps:
taking radix astragali, colla Corii Asini, radix Codonopsis, radix Paeoniae alba, radix Angelicae sinensis, herba et Gemma Agrimoniae, radix Rubiae, fructus Citri Sarcodactylis, radix Dipsaci and adjuvants according to the formula of the granule for stopping bleeding and regulating menstruation;
mixing the angelica and the fingered citron, distilling and extracting, collecting volatile oil, and obtaining mixed water extract of the angelica and the fingered citron and mixed dregs of the angelica and the fingered citron, wherein the volatile oil is included by β -cyclodextrin to obtain β -cyclodextrin inclusion compound;
pulverizing the donkey-hide gelatin into donkey-hide gelatin powder; taking half amount of radix astragali, pulverizing, sieving to obtain radix astragali coarse powder and radix astragali fine powder, and pulverizing the radix astragali fine powder to obtain radix astragali superfine powder;
mixing the astragalus coarse powder, the other half of astragalus, the mixed dregs of angelica and fingered citron, codonopsis pilosula, white paeony root, hairyvein agrimony, madder and teasel root, carrying out water extraction and filtration to obtain a water extract, combining the water extract and the mixed water extract of angelica and fingered citron, and concentrating to obtain an extract with the specific gravity of 1.25-1.35;
carrying out vacuum drying treatment and crushing on the extract to obtain dry extract powder, wherein the water content of the dry extract powder is 3-7 wt%;
uniformly mixing the dry extract powder, the donkey-hide gelatin powder, the astragalus superfine powder and the auxiliary materials, performing dry granulation, and then adding the β -cyclodextrin inclusion compound for total mixing to obtain the particles for stopping bleeding and regulating menstruation;
wherein the dry granulation parameters are as follows: the feeding speed is 65r/min to 75r/min, the pressure of a compression roller is 6MPa to 17.5MPa, the running speed of the compression roller is 8r/min to 20r/min, the liquid inlet temperature of cooling liquid of the compression roller is 6 ℃ to 16.5 ℃, and the whole grain speed is 60r/min to 100 r/min.
According to the method, firstly, distilling angelica and fingered citron to extract volatile oil according to the material characteristics of the particles for stopping bleeding and regulating menstruation, preparing the volatile oil into β -cyclodextrin inclusion compound, improving the utilization rate of the volatile oil, extracting the medicine residues with astragalus, codonopsis pilosula, white paeony root, hairyvein agrimony, madder and teasel root by water, combining the extracted liquid with the water-steaming distillation extract of the angelica and the fingered citron, concentrating the extract to obtain an extract with the specific gravity of 1.25-1.35, and then carrying out dry paste by adopting a vacuum drying process to obtain dry paste powder with high density, compact texture and 3-7 wt% of water content.
In one embodiment, the temperature of the vacuum drying treatment is 60-80 ℃, the vacuum degree is-0.06 MPa-0.08 MPa, and the drying time is 15-20 h.
In one embodiment, the dry extract powder has a particle size of 150 to 250 μm.
In one embodiment, the dry granulation adopts a dry granulator to carry out primary pressing and secondary pressing, the materials with the average particle size of less than 65 meshes and more than 10 meshes are subjected to secondary pressing after the primary pressing, and dry particles with the average particle size of 10 meshes to 65 meshes are obtained after the secondary pressing.
In one embodiment, the pressure of the primarily pressed compression roller is 9MPa to 17MPa, and the liquid inlet temperature of the cooling liquid of the compression roller is 9 ℃ to 15 ℃; the pressure of the re-pressing press roll is 10 MPa-16.5 MPa, and the liquid inlet temperature of the cooling liquid of the press roll is 9-12 ℃.
In one embodiment, the weight of the astragalus membranaceus ultrafine powder is 15% -20% of the total weight of the astragalus membranaceus.
In one embodiment, the inclusion is that the volatile oil is added into a mixture of β -cyclodextrin and water in an amount which is 7-10 times that of the volatile oil, and the mixture is ground for 20-30 minutes.
In one embodiment, the number of times of water extraction after mixing the astragalus coarse powder, the other half of astragalus, the mixed dregs of angelica and fingered citron, codonopsis pilosula, white paeony root, hairyvein agrimony, madder and teasel root is twice, 8-10 times of water is added for boiling extraction for 1-2 hours for the first time, 6-8 times of water is added for boiling extraction for 1-1.5 hours for the second time; and combining the extracting solutions obtained by the two water extractions, and filtering to obtain the water extracting solution.
In one embodiment, the particles for hemostasis and menstruation regulation comprise the following raw materials in parts by weight: 45-50 parts of astragalus membranaceus, 45-50 parts of donkey-hide gelatin, 43-48 parts of codonopsis pilosula, 12-16 parts of white paeony root, 10-15 parts of angelica sinensis, 45-50 parts of hairyvein agrimony, 20-28 parts of madder, 12-16 parts of fingered citron, 12-16 parts of teasel root, 15-20 parts of pregelatinized starch and 25-30 parts of sucrose powder.
In one embodiment, the raw materials comprise, by weight, 48 parts of astragalus membranaceus, 48 parts of donkey-hide gelatin, 45 parts of codonopsis pilosula, 15 parts of radix paeoniae alba, 12 parts of angelica sinensis, 48 parts of hairyvein agrimonia herb and bud, 24 parts of madder, 12 parts of fingered citron, 12 parts of teasel roots, 18 parts of pregelatinized starch and 27 parts of sucrose powder.
Compared with the traditional preparation method, the method disclosed by the invention has the following beneficial effects:
1) the method saves multiple links of soft material preparation, granulation, drying and the like in a wet granulation process, shortens the production period, simplifies the process flow and improves the process controllability.
2) The method adopts dry granulation and can be carried out under the controllable condition at low temperature, and qualified granules can be prepared by controlling the condition parameters of the dry granulation without adding other adhesives and wetting agents except sucrose and pregelatinized starch, so that the method is more energy-saving and environment-friendly.
3) The method reasonably utilizes the characteristic of heat softening of the donkey-hide gelatin, and the donkey-hide gelatin powder and the sucrose powder are heated and softened in extrusion in the dry granulation step, so that the donkey-hide gelatin powder and the sucrose powder can be fully bonded with other materials, the formability of the granules is effectively improved, and no extra dry adhesive such as microcrystalline cellulose is needed to be added.
4) The method aims at the contradiction that the extract has strong hygroscopicity, is difficult to dry at low temperature and the donkey-hide gelatin is easy to soften at high temperature to affect granulation, reasonably utilizes the properties of materials, adopts a vacuum drying method to dry the extract, obtains the dry extract with high density, reduces the hygroscopicity of the crushed dry extract powder, controls the moisture content of the dry extract powder to be 3-7%, meets the moisture requirement of the dry granulated material, can play a role in binding by combining with the heat softening of the donkey-hide gelatin powder, improves the hardness of granules, is convenient for subsequent granule finishing, and has good integrity of the prepared granules.
5) The preparation method of the particles for stopping bleeding and regulating menstruation has the advantages that the product percent of pass can reach more than 90%, the productivity can reach more than 100 Kg/h, and the method can be suitable for industrial mass production.
Detailed Description
In order that the invention may be more fully understood, a more particular description of the invention will now be rendered by reference to specific embodiments thereof that are illustrated in the appended drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The applicant finds in production practice that the difficulty of the bleeding stopping and menstruation regulating granular preparation lies in that the dry extract of the traditional Chinese medicine extract has strong hygroscopicity, the donkey-hide gelatin is easy to soften and bond, and the drying and crushing of the extract, the subsequent granulation and the finished product storage have great influence.
For example, in the traditional wet granulation process, spray drying is adopted to dry the extract to obtain dry extract powder, the particle size is small, the water content is usually 1 wt% -3 wt%, the hygroscopicity is very strong, the amount of a wetting agent is not easy to control when a soft material is prepared, and the distribution of the wetting agent is not uniform, so that the prepared soft material is uneven in dryness and wetness, the particle forming is not good when granulation is performed, the particle size distribution is wide, part of soft materials are difficult to granulate, and the yield is low; in addition, wet granulation needs drying at 60-80 ℃, donkey-hide gelatin is heated and easily softened in the drying process, so that granules are easy to form plates and long in drying time, and the particle density of the dried whole granules is not uniform, thereby affecting the granularity of finished products. In the traditional one-step granulation process, the air inlet temperature of a boiling granulator is high (70-100 ℃), donkey-hide gelatin is easy to soften when heated, the formation of a fluidized bed is not facilitated, extract can be attached to a bottom material after being sprayed, wet granules are easy to aggregate due to strong viscosity of the extract, the drying time is prolonged, and if the continuous spraying granulation time is long, the bed is easy to collapse; if the particles prepared by intermittent spraying have small particle size, low density, more pores and easy moisture absorption, the particles are easy to adhere to the inner wall in equipment, so that the one-step granulation process is difficult to operate, the granulation time is long, the energy consumption is high, the yield is not high, and the finished product has strong moisture absorption and is not favorable for storage.
Aiming at the contradiction problems that the extract has strong hygroscopicity, is difficult to dry at low temperature and the donkey-hide gelatin is easy to soften at high temperature to influence granulation, long-time exploration and a large number of experimental researches are carried out, and according to the material characteristics of the granules for stopping bleeding and regulating menstruation, the dry extract powder with higher density and compact texture is prepared by adopting vacuum drying, the hygroscopicity of the powder can be effectively reduced, the forming of granular preparation is facilitated, and improves the stability of the finished product, solves the problems of fine granularity, loose granules and strong hygroscopicity of the dry paste powder obtained by spray drying, and then, the dry granulation process is selected to prepare the granules, so that the process of drying materials is avoided, the technical problems that the donkey-hide gelatin powder is easy to soften at high temperature, the dry extract powder and the sucrose powder have strong hygroscopicity, the wet granulation is difficult, the one-step granulation is easy to collapse and the like are successfully solved, the production period is shortened, the qualified granules can be quickly prepared, and the product yield is high.
One embodiment of the present invention provides a method for preparing particles for hemostasis and menstruation regulation, comprising the following steps S1-S6.
S1, taking radix astragali, colla Corii Asini, radix Codonopsis, radix Paeoniae alba, radix Angelicae sinensis, herba et Gemma Agrimoniae, radix Rubiae, fructus Citri Sarcodactylis, radix Dipsaci and adjuvants according to the formula of the granule for stopping bleeding and regulating menstruation.
In one embodiment, the particles for stopping bleeding and regulating menstruation comprise the following raw materials in parts by weight: 45-50 parts of astragalus membranaceus, 45-50 parts of donkey-hide gelatin, 43-48 parts of codonopsis pilosula, 12-16 parts of white paeony root, 10-15 parts of angelica sinensis, 45-50 parts of hairyvein agrimony, 20-28 parts of madder, 12-16 parts of fingered citron, 12-16 parts of teasel root, 10-20 parts of pregelatinized starch and 25-30 parts of sucrose powder.
Further, the raw materials of the particles for hemostasis and menstruation regulation comprise, by weight, 48 parts of astragalus mongholicus, 48 parts of donkey-hide gelatin, 45 parts of codonopsis pilosula, 15 parts of white paeony root, 12 parts of Chinese angelica, 48 parts of hairyvein agrimony, 24 parts of madder, 12 parts of fingered citron, 12 parts of teasel root, 18 parts of pregelatinized starch and 27 parts of sucrose powder.
S2, mixing the angelica and the fingered citron, distilling and extracting, collecting volatile oil, obtaining mixed water extract of the angelica and the fingered citron and mixed dregs of the angelica and the fingered citron, and clathrating the volatile oil with β -cyclodextrin to obtain a β -cyclodextrin inclusion compound.
In one embodiment, 5-7 times of water is added into the angelica and the fingered citron, and the mixture is distilled and extracted for 3-5 hours.
In one embodiment, the volatile oil is added into a mixture of β -cyclodextrin and a proper amount of water, wherein the amount of the mixture is 7-10 times that of the cyclodextrin, and the mixture is ground for 20-30 minutes.
In one embodiment, the volatile oil is added to a mixture of 8 times the amount of β -cyclodextrin and an appropriate amount of water and ground for 20 minutes.
Specifically, β -cyclodextrin with the quantity of 8 times of the volatile oil is added with a proper amount of purified water and mixed evenly to be blended into paste, the volatile oil is diluted by 95% ethanol with the quantity of 4 times of the volatile oil, the paste is included for 20 minutes by a colloid mill, the filtering is carried out, and filter residue is dried at 50-60 ℃ to obtain the β -cyclodextrin inclusion compound.
S3, crushing the donkey-hide gelatin into donkey-hide gelatin powder; taking half amount of radix astragali, pulverizing, sieving to obtain radix astragali coarse powder and radix astragali fine powder, and pulverizing the radix astragali fine powder to obtain radix astragali superfine powder.
In one embodiment, the weight of the astragalus membranaceus ultrafine powder is 15% -20% of the total weight of the astragalus membranaceus.
In one embodiment, half of the astragalus membranaceus is taken, dried for 4-5 hours at 70-80 ℃, crushed and sieved by a 100-mesh sieve to obtain coarse astragalus membranaceus powder and fine astragalus membranaceus powder, the fine astragalus membranaceus powder is crushed again to obtain fine astragalus membranaceus powder, 8-10 parts of the fine astragalus membranaceus powder are reserved for later use, and the rest part is subjected to water extraction treatment.
S4, mixing the coarse powder of the astragalus, the other half of the astragalus, the mixed dregs of the angelica and the fingered citron, the codonopsis pilosula, the white paeony root, the hairyvein agrimony, the madder and the teasel root, carrying out water extraction, filtering and impurity removal to obtain a water extract, combining the water extract and the mixed water extract of the angelica and the fingered citron, and concentrating to obtain an extract with the specific gravity of 1.25-1.35.
The specific gravity of the extract is measured at 60 ℃.
In one embodiment, the coarse powder of the astragalus, the fine powder of the rest of the astragalus, the other half of the astragalus, the mixed dregs of the angelica and the fingered citron, the codonopsis pilosula, the white paeony root, the hairyvein agrimony, the madder and the teasel root are extracted twice by water, 8-10 times of water is added for boiling extraction for 1-2 hours for the first time, 6-8 times of water is added for boiling extraction for 1-1.5 hours for the second time; and combining the extracting solutions obtained by the two water extractions, and filtering to obtain the water extracting solution.
S5, carrying out vacuum drying treatment and crushing on the extract obtained in the step S4 to obtain dry extract powder, wherein the water content of the dry extract powder is 3-7 wt%.
In one embodiment, the temperature of the vacuum drying treatment is 60-80 ℃, the vacuum degree is-0.06 MPa-0.08 MPa, and the drying time is 15-20 h.
The applicant searches a large number of vacuum drying parameters of extracts with different specific gravities (relative densities) of 1, finally determines the optimal process parameters, concentrates the extracting solution to the optimal specific gravity of 1.25-1.35 (measured at 60 ℃), then dries for 15-20 h under the conditions that the temperature is 60-80 ℃ and the vacuum degree is-0.06 MPa-0.08 MPa, obtains dry extract with the water content of 3-7 wt%, is easy to crush, has compact texture and large density, obviously reduces the hygroscopicity of the crushed dry extract powder, is beneficial to forming granular preparations, and successfully solves the problems of fine granularity, loose granules and strong hygroscopicity of the dry extract powder obtained by spray drying.
In one embodiment, the particle size of the dry paste powder is 150-250 μm.
S6, mixing the dry extract powder, the donkey-hide gelatin powder, the astragalus superfine powder and the auxiliary materials uniformly, performing dry granulation, and then adding the β -cyclodextrin inclusion compound for total mixing to obtain the particles for stopping bleeding and regulating menstruation.
Wherein the dry granulation parameters are as follows: the feeding speed is 65r/min to 75r/min, the pressure of a compression roller is 6MPa to 17.5MPa, the running speed of the compression roller is 8r/min to 20r/min, the liquid inlet temperature of cooling liquid of the compression roller is 6 ℃ to 16.5 ℃, and the whole grain speed is 60r/min to 100 r/min.
Through a series of trial production and long-time equipment selection and process parameter search, the applicant finally adopts a dry granulation process to granulate, reduces the material heating process, shortens the production period, and successfully solves the technical problems of the product such as the donkey-hide gelatin powder is easy to soften when meeting high temperature, the dry paste powder, the sucrose powder and the like have strong hygroscopicity, the wet granulation is difficult, the one-step granulation collapses, and the like.
In one embodiment, a granulator is used for primary pressing and secondary pressing, the materials with the average particle size of less than 65 meshes and more than 10 meshes are subjected to secondary pressing after the primary pressing is controlled, and dry particles with the average particle size of 10 meshes to 65 meshes are obtained after the secondary pressing is controlled. In one embodiment, the pressure of the primarily pressed compression roller is 9MPa to 17MPa, and the liquid inlet temperature of the cooling liquid of the compression roller is 9 ℃ to 15 ℃; the pressure of the re-pressed press roll is 10MPa to 16.5MPa, and the liquid inlet temperature of the cooling liquid of the press roll is 9 ℃ to 12 ℃.
Specifically, an LG200 type dry granulation machine is selected to perform trial production of the hemostasis and menstruation-regulating granules, and the parameters of the dry granulation are as follows: pressure, feeding speed, compression roller rotating speed, granulating speed, cooling water wetting and pressing times are searched, and finally determined parameters are shown as the following table:
after primary pressing and one-time re-pressing, the yield reaches 91.3 percent, and the temperature of the materials can be controlled below 60 ℃ in the whole pressing process by controlling the temperature of cooling water to be between 6 and 16.5 ℃, so that the influence of high temperature on the quality of finished products is reduced.
In one embodiment, the number of re-pressing times is 2-3. The product yield can be ensured through primary pressing and 2-3 times of secondary pressing.
The following are specific examples
Example 1
1) Preparing materials: 48kg of astragalus membranaceus, 48kg of donkey-hide gelatin, 45kg of codonopsis pilosula, 15kg of white paeony root, 12kg of Chinese angelica, 48kg of hairyvein agrimonia herb and bud, 24kg of madder, 12kg of fingered citron, 12kg of teasel root, 18kg of pre-crosslinked starch and 27kg of sucrose powder.
2) Extracting volatile oil from angelica and fingered citron, namely adding 6 times of water into the angelica and the fingered citron, carrying out steam distillation extraction for 4 hours, collecting the volatile oil, taking the mixed water extract of the angelica and the fingered citron for later use, taking the dregs of the angelica and the fingered citron for later use, taking β -cyclodextrin with 8 times of the volatile oil, adding a proper amount of purified water, uniformly mixing, mixing into paste, diluting the volatile oil with 4 times of 95% ethanol, carrying out inclusion for 20 minutes by using a colloid mill, filtering, and drying at 50-60 ℃ to obtain the β -cyclodextrin inclusion compound.
3) Taking half of the astragalus membranaceus, drying for 4 hours at 70-80 ℃ on a belt dryer, sieving with a 100-mesh sieve by using an automatic control pulverizer set, pulverizing to obtain astragalus membranaceus coarse powder, pulverizing with a micro pulverizer to obtain astragalus membranaceus ultrafine powder, taking 9kg of astragalus membranaceus ultrafine powder to be sterilized, and extracting the rest part of the astragalus membranaceus with water.
4) Mixing the coarse powder of the astragalus root in the step 3) with the rest fine powder of the astragalus root, the other half of the astragalus root, the mixed dregs of the angelica and the fingered citron, the codonopsis pilosula, the white paeony root, the hairyvein agrimony, the madder and the teasel root, extracting the mixture twice, adding 10 times of water for the first time, and boiling and extracting the mixture for 1.5 hours; adding 8 times of water for the second time, boiling and extracting for 1 hour, filtering decoction obtained by the two water extractions to remove impurities to obtain water extract, and combining the water extract with the mixed water extract of the angelica and the fingered citron in the step 2) to obtain extract.
5) Pumping the extractive solution into a concentrator, concentrating to obtain extract with specific gravity of 1.25 (measured at 60 deg.C).
6) And (3) putting the extract into a baking pan for vacuum drying, uniformly spreading, controlling the temperature to be 60-80 ℃, controlling the vacuum degree to be-0.06-0.08 MPa, drying for 20 hours to obtain dry extract, and pulverizing to obtain dry extract powder with the particle size of 150-250 mu m and the water content of 5.8 wt%, wherein about 60kg of the dry extract powder is obtained.
7) Taking the ground dry extract powder, the donkey-hide gelatin powder and the sucrose powder, adding the astragalus superfine powder and the pregelatinized starch, uniformly mixing, pumping to a hopper of an LG200 type dry granulator through a vacuum feeder, and horizontally feeding at a rotating speed of 65 r/min; the pressure is 17MPa, the running speed of the compression roller is 8r/min, and the displacement of the compression roller is 3-4 mm; crushing by a crushing knife, sieving by a 10-mesh sieve, grading, wherein the grading rotating speed is 70r/min, then feeding to a sieving machine, and sieving by a 10-mesh sieve and a 65-mesh sieve to obtain particles with the granularity meeting the specification; and re-pressing the fine powder with the granularity smaller than 65 meshes for 2 times to obtain particles meeting the specification, wherein the yield of qualified particles is 91.0%.
Mixing the granules meeting the specification with the β -cyclodextrin inclusion compound obtained in the step 2) to obtain about 139.2kg of the granules for stopping bleeding and regulating menstruation, and subpackaging.
Example 2
Steps 1) to 4) of example 2 are the same as in example 1.
5) Pumping the extractive solution into a concentrator, concentrating to obtain extract with specific gravity of 1.35 (measured at 60 deg.C).
6) And (3) putting the extract into a baking pan for vacuum drying, uniformly spreading, controlling the temperature to be 60-80 ℃, controlling the vacuum degree to be-0.06-0.08 MPa, drying for 15h to obtain dry extract, and pulverizing to obtain dry extract powder with the particle size of 150-250 mu m and the water content of 6.0 wt%, wherein about 58kg of the dry extract powder is obtained.
7) Taking the ground dry extract powder, the donkey-hide gelatin powder and the sucrose powder, adding the astragalus superfine powder and the pregelatinized starch, uniformly mixing, pumping to a hopper of an LG200 type dry granulator through a vacuum feeder, and horizontally feeding at a rotating speed of 75 r/min; the pressure is 13MPa, the running speed of the compression roller is 15r/min, and the displacement of the compression roller is 3-4 mm; crushing by a crushing knife, sieving by a 10-mesh sieve, grading, wherein the grading rotating speed is 100r/min, then feeding to a sieving machine, and sieving by a 10-mesh sieve and a 65-mesh sieve to obtain particles with the granularity meeting the specification; and re-pressing the fine powder with the granularity smaller than 65 meshes for 2 times to obtain particles meeting the specification, wherein the yield of qualified particles is 91.8%.
Mixing the granules meeting the specification with the β -cyclodextrin inclusion compound obtained in the step 2) to obtain about 138.6kg of the granules for stopping bleeding and regulating menstruation, and subpackaging.
Example 3
Steps 1) to 4) of example 3 are the same as in example 1.
5) Pumping the extractive solution into a concentrator, concentrating to obtain extract with specific gravity of 1.30 (measured at 60 deg.C).
6) And (3) putting the extract into a baking pan for vacuum drying, uniformly spreading, controlling the temperature to be 60-80 ℃, controlling the vacuum degree to be-0.06-0.08 MPa, drying for 18h to obtain dry extract, and pulverizing to obtain dry extract powder with the average particle size of 150-180 mu m and the water content of 6.2 wt%, wherein about 61kg of the dry extract powder is obtained.
7) Taking the ground dry extract powder, the donkey-hide gelatin powder and the sucrose powder, adding the astragalus superfine powder and the pregelatinized starch, uniformly mixing, pumping to a hopper of an LG200 type dry granulator through a vacuum feeder, and horizontally feeding at a rotating speed of 70 r/min; the pressure is 9MPa, the running speed of the compression roller is 15r/min, and the displacement of the compression roller is 3-4 mm; crushing by a crushing knife, sieving by a 10-mesh sieve, grading, sieving at the rotating speed of 80r/min, sieving by a sieving machine, and sieving by a 10-mesh sieve and a 65-mesh sieve to obtain particles with the granularity meeting the specification; and re-pressing the fine powder with the granularity smaller than 65 meshes for 3 times to obtain the particles meeting the specification, wherein the yield of the qualified particles is 92.5 percent.
Mixing the granules meeting the specification with the β -cyclodextrin inclusion compound obtained in the step 2) to obtain about 142.5kg of the granules for stopping bleeding and regulating menstruation, and subpackaging.
Comparative example 1
Steps 1) to 4) of comparative example 1 are the same as in example 3.
5) Pumping the extractive solution into a concentrator, concentrating to obtain extract with specific gravity of 1.10 (measured at 60 deg.C).
6) Spray drying the extract at air inlet temperature of 180 deg.C and air outlet temperature of 85 deg.C to obtain dry extract powder (about 50 kg).
7) Taking dry extract powder, donkey-hide gelatin powder and sucrose powder, adding the superfine powder of the astragalus and pregelatinized starch, uniformly mixing, pumping to a hopper of an LG200 type dry-process granulator through a vacuum feeder, and horizontally feeding at a rotating speed of 70 r/min; the pressure is 9MPa, the running speed of the compression roller is 15r/min, and the displacement of the compression roller is 3-4 mm; crushing by a crushing knife, sieving by a 10-mesh sieve, grading, sieving at the rotating speed of 80r/min, sieving by a sieving machine, and sieving by a 10-mesh sieve and a 65-mesh sieve to obtain particles with the granularity meeting the specification; and re-pressing the fine powder with the granularity smaller than 65 meshes for 3 times to obtain the particles meeting the specification, wherein the yield of the qualified particles is 85%.
Mixing the granules meeting the specification with the β -cyclodextrin inclusion compound obtained in the step 2) to obtain about 121.6kg of the granules for stopping bleeding and regulating menstruation, and subpackaging.
Comparative example 1 the spray-dried powder was used, and the yield after drying was much lower than that of vacuum drying, since the spray-dried powder was liable to absorb moisture and to adhere to the inner wall of the spray-drying apparatus. In the dry granulation process, materials are easy to adhere to the inner wall of the dry granulator, a compression roller and a granulating screen due to moisture absorption, so that the operation of the dry granulator is influenced, the dry granulator needs to be cleaned in time, and the yield of qualified granules is influenced. The yield of the finished product is about 15-20 kg lower than that of the new process.
Comparative example 2
Steps 1) to 4) of comparative example 1 are the same as in example 3.
5) Pumping the extractive solution into a concentrator, concentrating to obtain extract with specific gravity of 1.15 (measured at 60 deg.C).
6) And (3) putting the extract into a baking pan for vacuum drying, uniformly spreading, controlling the temperature to be 60-80 ℃, controlling the vacuum degree to be-0.06-0.08 MPa, drying for 30h to obtain dry extract, and pulverizing to obtain dry extract powder with the average particle size of 150-250 mu m and the water content of 6.2 wt%, wherein about 62kg of the dry extract powder is obtained.
7) Taking dry extract powder, donkey-hide gelatin powder and sucrose powder, adding the superfine powder of the astragalus and pregelatinized starch, uniformly mixing, pumping to a hopper of an LG200 type dry-process granulator through a vacuum feeder, and horizontally feeding at a rotating speed of 70 r/min; the pressure is 9MPa, the running speed of the compression roller is 15r/min, and the displacement of the compression roller is 3-4 mm; crushing by a crushing knife, sieving by a 10-mesh sieve, grading, sieving at the rotating speed of 80r/min, sieving by a sieving machine, and sieving by a 10-mesh sieve and a 65-mesh sieve to obtain particles with the granularity meeting the specification; and re-pressing the fine powder with the granularity smaller than 65 meshes for 3 times to obtain the particles meeting the specification, wherein the yield of the qualified particles is 91.4%.
Mixing the granules meeting the specification with the β -cyclodextrin inclusion compound obtained in the step 2) to obtain the blood-stopping and menstruation-regulating granules, wherein the weight of the granules is about 141.7kg, and subpackaging.
Comparative example 2 adopts the extract with the specific gravity of 1.15 (measured at 60 ℃) to carry out vacuum drying for about 30 hours, and adopts the extract with the specific gravity of 1.25-1.35 (measured at 60 ℃) to carry out vacuum drying for about 18-20 hours, which obviously influences the production cycle, the drying time is prolonged by about 10 hours, and adopts a double-effect concentrator to concentrate the extract with the specific gravity of 1.15 to the extract with the specific gravity of 1.25-1.35 and concentrate for about 0.5-1 hour, so that the extract with the specific gravity of 1.25-1.35 (measured at 60 ℃) is obviously more economic, and the production efficiency is higher.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The preparation method of the particles for stopping bleeding and regulating menstruation is characterized by comprising the following steps:
according to the formula of the hemostatic and menstruation-regulating granule, astragalus mongholicus, donkey-hide gelatin, codonopsis pilosula, white paeony root, Chinese angelica, hairyvein agrimony, madder, fingered citron, teasel root and auxiliary materials are adopted;
mixing the angelica and the fingered citron, distilling and extracting, collecting volatile oil, and obtaining mixed water extract of the angelica and the fingered citron and mixed dregs of the angelica and the fingered citron, and clathrating the volatile oil with β -cyclodextrin to obtain β -cyclodextrin inclusion compound;
pulverizing the donkey-hide gelatin into donkey-hide gelatin powder; taking half amount of radix astragali, pulverizing, sieving to obtain radix astragali coarse powder and radix astragali fine powder, and pulverizing the radix astragali fine powder to obtain radix astragali superfine powder;
mixing the astragalus coarse powder, the other half of astragalus, the mixed dregs of angelica and fingered citron, codonopsis pilosula, white paeony root, hairyvein agrimony, madder and teasel root, carrying out water extraction and filtration to obtain a water extract, combining the water extract and the mixed water extract of angelica and fingered citron, and concentrating to obtain an extract with the specific gravity of 1.25-1.35;
carrying out vacuum drying treatment and crushing on the extract to obtain dry extract powder, wherein the water content of the dry extract powder is 3-7 wt%;
uniformly mixing the dry extract powder, the donkey-hide gelatin powder, the astragalus superfine powder and the auxiliary materials, performing dry granulation, and then adding the β -cyclodextrin inclusion compound for total mixing to obtain the particles for stopping bleeding and regulating menstruation;
wherein the dry granulation parameters are as follows: the feeding speed is 65r/min to 75r/min, the pressure of a compression roller is 6MPa to 17.5MPa, the running speed of the compression roller is 8r/min to 20r/min, the liquid inlet temperature of cooling liquid of the compression roller is 6 ℃ to 16.5 ℃, and the whole grain speed is 60r/min to 100 r/min.
2. The preparation method according to claim 1, wherein the temperature of the vacuum drying treatment is 60 ℃ to 80 ℃, the vacuum degree is-0.06 MPa to-0.08 MPa, and the drying time is 15h to 20 h.
3. The method of claim 1, wherein the dry extract powder has a particle size of 150 to 250 μm.
4. The preparation method according to claim 1, wherein the dry granulation is carried out by carrying out primary pressing and secondary pressing by using a dry granulator, wherein the material with the average particle size of less than 65 meshes and more than 10 meshes is subjected to the secondary pressing after the primary pressing, and dry granules with the average particle size of 10 meshes to 65 meshes are obtained after the secondary pressing.
5. The preparation method according to claim 4, wherein the pressure of the primarily pressed compression roller is 9MPa to 17MPa, and the liquid inlet temperature of the cooling liquid of the compression roller is 9 ℃ to 15 ℃;
the pressure of the re-pressing press roller is 10 MPa-16.5 MPa, and the liquid inlet temperature of the cooling liquid of the press roller is 9-12 ℃.
6. The preparation method according to claim 1, wherein the weight of the astragalus membranaceus ultrafine powder is 15-20% of the total weight of the astragalus membranaceus.
7. The preparation method according to claim 1, wherein the encapsulation is that the volatile oil is added into a mixture of β -cyclodextrin and water in an amount of 7-10 times of the volatile oil and is ground for 20-30 minutes.
8. The preparation method according to claim 1, wherein the coarse powder of radix astragali, the other half amount of radix astragali, the mixed dregs of radix Angelicae sinensis and fructus Citri Sarcodactylis, radix Codonopsis, radix Paeoniae alba, herba et Gemma Agrimoniae, radix Rubiae and radix Dipsaci are mixed and then extracted with water twice, 8-10 times of water is added for boiling extraction for 1-2 hours for the first time, 6-8 times of water is added for boiling extraction for 1-1.5 hours for the second time; and combining the extracting solutions obtained by the two water extractions, and filtering to obtain the water extracting solution.
9. The preparation method according to any one of claims 1 to 8, wherein the particles for stopping bleeding and regulating menstruation comprise the following raw materials in parts by weight: 45-50 parts of astragalus membranaceus, 45-50 parts of donkey-hide gelatin, 43-48 parts of codonopsis pilosula, 12-16 parts of white paeony root, 10-15 parts of angelica sinensis, 45-50 parts of hairyvein agrimony, 20-28 parts of madder, 12-16 parts of fingered citron, 12-16 parts of teasel root, 15-20 parts of pregelatinized starch and 25-30 parts of sucrose powder.
10. The preparation method according to claim 9, wherein the raw materials comprise, by weight, 48 parts of astragalus membranaceus, 48 parts of donkey-hide gelatin, 45 parts of codonopsis pilosula, 15 parts of radix paeoniae alba, 12 parts of angelica sinensis, 48 parts of agrimony, 24 parts of madder, 12 parts of fingered citron, 12 parts of teasel roots, 18 parts of pregelatinized starch and 27 parts of sucrose powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911153686.7A CN110801477A (en) | 2019-11-22 | 2019-11-22 | Preparation method of particles for stopping bleeding and regulating menstruation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911153686.7A CN110801477A (en) | 2019-11-22 | 2019-11-22 | Preparation method of particles for stopping bleeding and regulating menstruation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110801477A true CN110801477A (en) | 2020-02-18 |
Family
ID=69491141
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911153686.7A Pending CN110801477A (en) | 2019-11-22 | 2019-11-22 | Preparation method of particles for stopping bleeding and regulating menstruation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110801477A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113004975A (en) * | 2021-03-19 | 2021-06-22 | 湖南安邦制药股份有限公司 | Method for extracting mixed volatile oil of angelica and fingered citron |
| CN113712924A (en) * | 2021-10-09 | 2021-11-30 | 陕西健民制药有限公司 | Preparation method of traditional Chinese medicine granular preparation |
| CN114732099A (en) * | 2022-04-20 | 2022-07-12 | 湖南振兴中药有限公司 | Donkey-hide gelatin and red date solid beverage and preparation process thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1235029A (en) * | 1998-05-08 | 1999-11-17 | 湖南安邦制药有限公司 | Medicine for regulating menstruation and arresting bleeding and producing process therefor |
| CN108420795A (en) * | 2018-03-28 | 2018-08-21 | 湖南安邦制药有限公司 | The preparation method of blood-arresting catamenia-regulating particle |
-
2019
- 2019-11-22 CN CN201911153686.7A patent/CN110801477A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1235029A (en) * | 1998-05-08 | 1999-11-17 | 湖南安邦制药有限公司 | Medicine for regulating menstruation and arresting bleeding and producing process therefor |
| CN108420795A (en) * | 2018-03-28 | 2018-08-21 | 湖南安邦制药有限公司 | The preparation method of blood-arresting catamenia-regulating particle |
Non-Patent Citations (1)
| Title |
|---|
| 田守生等: "阿胶颗粒干法制粒工艺研究", 《中草药》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113004975A (en) * | 2021-03-19 | 2021-06-22 | 湖南安邦制药股份有限公司 | Method for extracting mixed volatile oil of angelica and fingered citron |
| CN113712924A (en) * | 2021-10-09 | 2021-11-30 | 陕西健民制药有限公司 | Preparation method of traditional Chinese medicine granular preparation |
| CN114732099A (en) * | 2022-04-20 | 2022-07-12 | 湖南振兴中药有限公司 | Donkey-hide gelatin and red date solid beverage and preparation process thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110801477A (en) | Preparation method of particles for stopping bleeding and regulating menstruation | |
| CN101433368B (en) | Method for producing shredded tobacco of cigarette using cabo | |
| CN104664539A (en) | Production method of ginseng solid beverage | |
| CN113499412A (en) | Preparation method of Jindan Fuyan granules | |
| CN108434104B (en) | Composite maltodextrin and preparation method and application thereof | |
| JPH0767379B2 (en) | Manufacturing method for producing nutritive substance and extracted substance from seeds of lupine plant | |
| CN109289032B (en) | Wind-cold common cold granules and preparation method thereof | |
| CN107496375A (en) | A kind of preparation method of herbal mixture granule | |
| CN106615600A (en) | Technology for separating protein from seabuckthorn seed meal by wet grinding method | |
| CN103059093A (en) | Method for preparing saponin by vacuum digestion | |
| CN104958328A (en) | Method for preparing poria cocos formula granules by using flash type extracting technology | |
| CN109464507A (en) | A kind of preparation method of hawthorn granule | |
| CN109464518A (en) | A kind of preparation method of stir-baking RADIX MORINDAE after sprinking salt solution day granule | |
| CN112807370B (en) | Preparation method and application of stomach nourishing granules | |
| CN107028895A (en) | A kind of LBP-X granule and preparation method thereof | |
| CN113995784A (en) | Preparation process of white peony root formula granules | |
| CN105461779B (en) | It is a kind of low cost Tea Saponin continuously extract raw material pretreatment process | |
| CN104095177A (en) | Health-care granule by using ginseng flower bud as the main raw material and preparation method thereof | |
| CN103039811A (en) | Pueraria, radix glehniae and radix ophiopogonis cake and preparation method thereof | |
| CN106727809B (en) | A kind of preparation method of ginseng ultra micro pure powder tablet | |
| CN110420286A (en) | A kind of Shengjing tablet for invigoration drying and moulding production method | |
| CN108578630B (en) | Preparation method of ginseng, poria cocos and bighead atractylodes rhizome granules | |
| CN115887579B (en) | Daydream granule and its preparation method | |
| CN103055121A (en) | Preparation method of clearing heat and relieving sore throat drug | |
| CN215724580U (en) | Vacuum drying equipment is used in production of cimetidine two contracts |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200218 |
|
| RJ01 | Rejection of invention patent application after publication |