CN112870322A - Preparation method and quality control method of astragalus and cassia twig five-ingredient decoction preparation - Google Patents

Preparation method and quality control method of astragalus and cassia twig five-ingredient decoction preparation Download PDF

Info

Publication number
CN112870322A
CN112870322A CN202110149648.5A CN202110149648A CN112870322A CN 112870322 A CN112870322 A CN 112870322A CN 202110149648 A CN202110149648 A CN 202110149648A CN 112870322 A CN112870322 A CN 112870322A
Authority
CN
China
Prior art keywords
peak
astragalus
cassia twig
decoction
preparation
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.)
Granted
Application number
CN202110149648.5A
Other languages
Chinese (zh)
Other versions
CN112870322B (en
Inventor
郭水柱
高松
王瑞娜
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zhongjing Wanxi Pharmaceutical Co ltd
Original Assignee
Zhongjing Wanxi Pharmaceutical Co ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Zhongjing Wanxi Pharmaceutical Co ltd filed Critical Zhongjing Wanxi Pharmaceutical Co ltd
Priority to CN202110149648.5A priority Critical patent/CN112870322B/en
Priority to CN202211154522.8A priority patent/CN116046916A/en
Publication of CN112870322A publication Critical patent/CN112870322A/en
Application granted granted Critical
Publication of CN112870322B publication Critical patent/CN112870322B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • 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
    • 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)
    • A61K36/54—Lauraceae (Laurel family), e.g. cinnamon or sassafras
    • 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)
    • A61K36/72—Rhamnaceae (Buckthorn family), e.g. buckthorn, chewstick or umbrella-tree
    • A61K36/725—Ziziphus, e.g. jujube
    • 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)
    • A61K36/88—Liliopsida (monocotyledons)
    • A61K36/906—Zingiberaceae (Ginger family)
    • A61K36/9068—Zingiber, e.g. garden ginger
    • 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
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/0087—Galenical forms not covered by A61K9/02 - A61K9/7023
    • A61K9/0095—Drinks; Beverages; Syrups; Compositions for reconstitution thereof, e.g. powders or tablets to be dispersed in a glass of water; Veterinary drenches
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P25/00—Drugs for disorders of the nervous system
    • A61P25/02—Drugs for disorders of the nervous system for peripheral neuropathies
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/30—Control of physical parameters of the fluid carrier of temperature
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/74—Optical detectors
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/86—Signal analysis
    • G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
    • 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, decoction
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30—Extraction of the material
    • A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30—Extraction of the material
    • A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50—Methods involving additional extraction steps
    • A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/30—Control of physical parameters of the fluid carrier of temperature
    • G01N2030/3007—Control of physical parameters of the fluid carrier of temperature same temperature for whole column
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
    • G01N2030/324—Control of physical parameters of the fluid carrier of pressure or speed speed, flow rate
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

Landscapes

  • Health & Medical Sciences (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Medicinal Chemistry (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Animal Behavior & Ethology (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Epidemiology (AREA)
  • Physics & Mathematics (AREA)
  • Immunology (AREA)
  • General Physics & Mathematics (AREA)
  • Pathology (AREA)
  • Biochemistry (AREA)
  • Analytical Chemistry (AREA)
  • Medical Informatics (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Biotechnology (AREA)
  • Botany (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Neurosurgery (AREA)
  • Neurology (AREA)
  • Biomedical Technology (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Library & Information Science (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention relates to a preparation method and a quality control method of an astragalus-cassia twig five-ingredient decoction preparation, which comprises the steps of establishing a preparation method and a characteristic map of the astragalus-cassia twig five-ingredient decoction preparation and a content determination method of 5 components. The invention introduces a flash extractor and a membrane filtration method into the preparation process of the radix astragali-cassia twig five-substance decoction preparation, so that the active ingredients of the medicine are retained to the maximum extent, and the content of the active ingredients is improved, wherein the radix astragali-cassia twig five-substance decoction preparation prepared by the method has the paeoniflorin content of not less than 175.72mg/g, the calycosin glucoside content of not less than 3.78mg/g, the cinnamic acid content of not less than 10.65mg/g, the 6-gingerol content of not less than 8.2mg/g, and the total volatile oil content of not less than 0.1% (ml/g). The characteristic map of the astragalus-cassia twig five-ingredient decoction preparation evaluates the chemical substance types and the contents of the astragalus-cassia twig five-ingredient decoction preparation on the whole.

Description

Preparation method and quality control method of astragalus and cassia twig five-ingredient decoction preparation
One, the technical field
The invention relates to the technical field of traditional Chinese medicines, in particular to a preparation method and a quality control method of an astragalus-cassia twig five-ingredient decoction preparation.
Second, background Art
The Huangqi Guizhi Wu Tang originates from Zhang Zhongjing which is a formula for resolving and cutting the diseases and symptoms of jin Kui Yao L.blood Bi deficiency and consumptive disease syndrome and is prepared from Jiang Zhi Tang which is twice as much as the raw material ginger, removed of the liquorice and added with the astragalus root. The original recipe is mainly indicated for blood arthralgia syndrome, benefiting qi temperature and meridian and dredging arthralgia. The Chinese medicinal preparation has exact curative effect, and is included in the ancient classical famous party directory (first batch) published in the country of 4 months in 2018, which shows that the Chinese medicinal preparation has high development and application values.
The astragalus-cassia twig five-ingredient decoction has wider clinical application range and also obtains satisfactory curative effect. The application in various clinical departments is not only limited to oral administration, but also achieves certain curative effect on external application, which shows that the compatibility of the recipe is accurate to a certain extent. The clinical application range of the astragalus-cassia twig five-ingredient decoction is further expanded in recent 15 years, and particularly the astragalus-cassia twig five-ingredient decoction has a remarkable curative effect on treating peripheral neuropathy. Although the scope of diseases treated by the astragalus-cassia twig five-ingredient decoction is wide, the qi deficiency, congealing cold and blood stasis are always taken as basic pathogenesis, and the principle of treating different diseases simultaneously in the traditional Chinese medicine is reflected. The astragalus-cassia twig five-ingredient decoction is widely applied in clinic, so that the traditional prescription and the modern medicine are organically combined, the clinic is better served, the cure rate of diseases is improved, the pain of patients is relieved, and the clinical requirement is met.
Modern pharmacological research finds that calycosin glucoside in astragalus is mainly used for improving immune function, enhancing antioxidation, radioresistance and anticancer effects, protecting cardiovascular and cerebrovascular, liver, kidney and lung, protecting brain cells, improving memory, relaxing vascular smooth muscle, achieving hormone-like effect, resisting bacteria, inhibiting virus, reducing blood fat, reducing blood sugar, reducing diabetic complications and the like; paeoniflorin in radix Paeoniae alba has effects of dilating blood vessel, relieving pain and tranquilizing, resisting inflammation and ulcer, relieving fever and spasm, and promoting diuresis; the organic acid component in the cassia twig is mainly cinnamic acid and has the effects of oxidation resistance, thrombus resistance and the like; 6-gingerol has antioxidant, anti-apoptosis and antiinflammatory effects; the polysaccharide has antioxidant, immunity enhancing, anticancer, and liver protecting effects.
Third, the invention
The technical problem to be solved by the invention is to provide a preparation method and a quality control method of the astragalus-cassia twig five-substance decoction preparation, wherein the preparation method of the astragalus-cassia twig five-substance decoction preparation can improve the contents of paeoniflorin, calycosin glucoside, cinnamic acid and 6-gingerol in the astragalus-cassia twig five-substance decoction preparation; the quality control method of the radix astragali and ramulus Cinnamomi five-substance decoction can simultaneously determine the contents of paeoniflorin, calycosin glucoside, cinnamic acid and 6-gingerol in the radix astragali and ramulus Cinnamomi five-substance decoction by high performance liquid chromatography; an HPLC characteristic map is established for the astragalus and cassia twig five-ingredient decoction preparation.
In order to achieve the purpose, the specific technical scheme of the invention is as follows: the preparation method of the radix astragali-cassia twig five-ingredient decoction preparation comprises the following raw material medicines in parts by weight: 2-4 parts of astragalus membranaceus, 2-4 parts of cassia twig, 2-4 parts of radix paeoniae alba, 4-8 parts of ginger and 3-6 parts of Chinese dates, wherein the preferable weight ratio of the raw materials is as follows: 3 parts of astragalus, 3 parts of cassia twig, 3 parts of white paeony root, 6 parts of ginger and 4 parts of Chinese date. The astragalus and cassia twig five-ingredient decoction preparation is prepared by the following method: (1) extracting radix astragali, ramulus Cinnamomi, radix Paeoniae alba, rhizoma Zingiberis recens and fructus Jujubae with distilled water for 2 times by flash extractor, wherein the water added for each extraction is 12-19 times of the total weight of radix astragali, ramulus Cinnamomi, radix Paeoniae alba, rhizoma Zingiberis recens and fructus Jujubae, the extraction time is 1.8-5.6min, the extraction temperature is 50 deg.C, filtering, and mixing filtrates to obtain residue I and filtrate A; adding 9.5 times of ethanol with volume concentration of 95% into the residue I, soaking for 4h, and filtering to obtain filtrate B; distilling filtrate A, collecting volatile oil, concentrating at 55 deg.C under reduced pressure to obtain extract with specific gravity of 1.05-1.21 to obtain volatile oil C and extract D; adding 7 times of beta-cyclodextrin into the volatile oil C, grinding and clathrating, freeze drying, and pulverizing into 100 mesh fine powder to obtain beta-cyclodextrin clathrate C; collecting filtrate B, recovering ethanol at 50 deg.C under reduced pressure, concentrating under reduced pressure to obtain extract E with specific gravity of 1.02-1.19, lyophilizing, pulverizing into extract superfine powder passing through 200 mesh sieve to obtain extract superfine powder A; filtering the extract D with a roll-up membrane with pore size of 10000 molecular weight, recovering solvent from the filtrate under reduced pressure, concentrating under reduced pressure to obtain extract with specific gravity of 1.13 at 25 deg.C, freeze drying, and pulverizing into extract superfine powder of 200 mesh sieve to obtain extract superfine powder B; mixing the extract superfine powder A, the extract superfine powder B and the beta-cyclodextrin inclusion compound C uniformly, and adding auxiliary materials to prepare the traditional Chinese medicine preparation.
The content of paeoniflorin in the prepared astragalus mongholicus and cassia twig five-material decoction preparation is not lower than 175.72mg/g (determined by an HPLC method), the content of calycosin glucoside is not lower than 3.78mg/g (determined by an HPLC method), the content of cinnamic acid is not lower than 10.65mg/g (determined by an HPLC method), the content of 6-gingerol is not lower than 8.2mg/g (determined by an HPLC method), and the content of total volatile oil is not lower than 0.1% (ml/g) (the content of the total volatile oil is determined by a volatile oil determination method B according to an 2015 edition, Chinese pharmacopoeia (four parts) appendix 2204).
2015 edition "Chinese pharmacopoeia (four parts) appendix 2204 method for volatile oil determination: taking about 300ml of water and a plurality of glass beads, placing the water and the glass beads in a flask, and connecting with a volatile oil tester. Water was added from the top of the apparatus to fill the scale and the flask was then overflowed, and then l ml of xylene was added by pipette and connected to a flow condenser. The flask contents were heated to boiling and distillation continued at a rate to maintain the middle of the condenser tube in a cooled state. Stopping heating after 30min, standing for more than 15 min, reading volume of xylene, and collecting appropriate amount of sample (corresponding to volatile oil)
Figure BDA0002932250820000022
) Weighing (accurate to 0.01g), placing in a flask, adding water
Figure BDA0002932250820000021
(or an appropriate amount) and glass beads, shaking and mixing, and connecting a volatile oil tester and a reflux condenser tube. Adding water from the upper end of the condensation tube to fill the scale part of the volatile oil tester and overflow into the flask. Placing in an electric heating jacket or slowly heating to boil by other suitable methods, and slightly boiling for about 5 hours until the oil amount is not increased, stopping heating, placing for a moment, starting a piston at the lower end of the measurement, slowly discharging water until the upper end of the oil layer reaches 5mm above the 0 line of the scale. Standing for more than 1 hr, opening the piston to lower the oil layer to the level where its upper end is aligned with 0 line of the scale, reading the volatile oil amount, subtracting the xylene amount from the oil layer amount to obtain the volatile oil amount, and calculating the volatile oil content (%) in the sample.
The invention establishes a characteristic map and a content determination method of 5 components aiming at an astragalus-cassia twig five-substance decoction preparation, wherein paeoniflorin, calycosin glucoside, cinnamic acid and 6-gingerol can be simultaneously determined by an HPLC method, and the method is characterized by comprising the following steps of:
step 1, preparing a test solution of an astragalus and cassia twig five-substance decoction preparation: taking a proper amount of the astragalus and cassia twig five-material decoction preparation sample, adding a proper amount of 70% methanol for dissolving, transferring to a 10ml volumetric flask, carrying out ultrasonic treatment (250w, 40KHz) for 30min, standing to room temperature, fixing the volume to the scale with 70% methanol, shaking up, filtering, and taking the subsequent filtrate to obtain the astragalus and cassia twig five-material decoction preparation.
Step 2, preparation of mixed reference solution: accurately weighing penoniflorin, calycosin glucoside, cinnamic acid and 6-gingerol reference substance, placing in a volumetric flask, adding methanol to desired volume to scale, shaking, and making into mixed reference substance solution.
Step 3, simultaneous determination and characteristic spectrum determination of the content of 4 components in the astragalus and cassia twig five-component decoction preparation: injecting the test solution of the astragalus and cassia twig five-substance decoction preparation prepared in the step 1 into HPLC for analysis, and determining the content and the characteristic map of 4 components in 15 batches of astragalus and cassia twig five-substance decoction preparation samples. The detection method for simultaneously measuring the characteristic spectrum and the 4 components of the astragalus-cassia twig five-component decoction preparation comprises the following liquid chromatography conditions: acetonitrile (a) -0.2% aqueous formic acid (B), gradient elution; detecting at 278nm, 30 deg.C, 1.0ml/min flow rate, and chromatographic column Thermo Syncronis C18And (3) a column.
As a preferred scheme, the detection method for simultaneously determining the characteristic map and the 4 components of the astragalus-cassia twig five-ingredient decoction preparation comprises the following gradient elution procedures:
Figure BDA0002932250820000031
the characteristic spectrum of the radix astragali and cassia twig five-material decoction substance standard and the preparation thereof and the detection method for simultaneously measuring 4 components have 12 common peaks in the established characteristic spectrum.
The invention has the advantages that:
1. a method for measuring the content of cinnamaldehyde in cassia twig recorded in China pharmacopoeia of 2020 edition is adopted, and a method for measuring the content of a related component, namely cinnamic acid, is not recorded. The method for determining the content of the cinnamic acid fills the gap that the prior pharmacopoeia lacks the determination of the content of the cinnamic acid of the cassia twig.
2. A method for simultaneously determining 4 components of paeoniflorin, calycosin glucoside, cinnamic acid and 6-gingerol in the radix astragali-cassia twig five-substance decoction is established, the defects of the prior art are made up, and the quality reference of the radix astragali-cassia twig five-substance decoction and the quality attributes of the preparation thereof are integrally controlled.
3. Establishing a characteristic map of the astragalus-cassia twig five-ingredient decoction preparation, and integrally evaluating the chemical substance types and the contents of the astragalus-cassia twig five-ingredient decoction preparation.
4. The preparation process of the astragalus-cassia twig five-ingredient decoction preparation furthest reserves volatile components in medicinal materials in a prescription.
Description of the drawings
FIG. 1 is a graph of a control sample containing paeoniflorin, calycosin glucoside, cinnamic acid and 6-gingerol
FIG. 2 is a reference characteristic spectrum of the astragalus and cassia twig five-herb decoction
FIG. 3 shows the characteristic maps of 15 random lots of the decoction of Astragalus and Cassia twig (No. 3 peak paeoniflorin (set as reference peak), No. 4 peak calycosin glucoside, No. 8 peak cinnamic acid, No. 12 peak 6-gingerol)
FIG. 4 shows the spectra of 12 common peaks in 15 batches of the five-herb decoction of astragalus and cassia twig
FIG. 5 is a comparison feature map of three batches of radix astragali and ramulus Cinnamomi decoction granules
FIG. 6 is a characteristic spectrum of three batches of radix astragali and cassia twig five-ingredient decoction granules
Fifth, detailed description of the invention
The following describes the preparation method of the astragalus-cassia twig five-ingredient decoction preparation in detail with reference to specific examples, but the scope of the invention is not limited thereto.
Example 1
The invention can be realized by the following method in specific implementation: the traditional Chinese medicine composition of the astragalus mongholicus-cassia twig five-ingredient decoction preparation is prepared from the following raw material medicines in parts by weight: 2 parts of astragalus, 2 parts of cassia twig, 2 parts of white paeony root, 4 parts of ginger and 3 parts of Chinese date, and the astragalus and cassia twig five-substance decoction preparation is prepared by the following method: (1) extracting radix astragali, ramulus Cinnamomi, radix Paeoniae alba, rhizoma Zingiberis recens and fructus Jujubae with distilled water for 2 times in a flash extractor, wherein the water amount added for each extraction is 12 times of the total weight of radix astragali, ramulus Cinnamomi, radix Paeoniae alba, rhizoma Zingiberis recens and fructus Jujubae, the extraction time is 1.8min, the extraction temperature is 50 deg.C, filtering, and mixing filtrates to obtain residue I and filtrate A; adding 9.5 times of ethanol with volume concentration of 95% into the residue I, soaking for 4h, and filtering to obtain filtrate B; distilling filtrate A, collecting volatile oil, concentrating at 55 deg.C under reduced pressure to obtain extract with specific gravity of 1.05 to obtain volatile oil C and extract D; adding 7 times of beta-cyclodextrin into the volatile oil C, grinding and clathrating, freeze drying, and pulverizing into 100 mesh fine powder to obtain beta-cyclodextrin clathrate C; collecting filtrate B, recovering ethanol at 50 deg.C under reduced pressure, concentrating under reduced pressure to obtain extract E with specific gravity of 1.02, lyophilizing, and pulverizing into extract superfine powder of 200 mesh sieve to obtain extract superfine powder A; filtering the extract D with a roll-up membrane with pore size of 10000 molecular weight, recovering solvent from the filtrate under reduced pressure, concentrating under reduced pressure to obtain extract with specific gravity of 1.13 at 25 deg.C, freeze drying, and pulverizing into extract superfine powder of 200 mesh sieve to obtain extract superfine powder B; mixing extract superfine powder A, extract superfine powder B, and beta-cyclodextrin clathrate C, adding adjuvant, and making into granule; the radix astragali-cassia twig five-material decoction granules prepared by the invention have the paeoniflorin content of not less than 175.72mg/g (determined by an HPLC method), the calycosin glucoside content of not less than 3.78mg/g (determined by an HPLC method), the cinnamic acid content of not less than 10.65mg/g (determined by an HPLC method), the 6-gingerol content of not less than 8.2mg/g (determined by an HPLC method) and the total volatile oil content of not less than 0.1% (ml/g) (the total volatile oil content is determined by a volatile oil determination method B according to an 2015 edition, Chinese pharmacopoeia (four parts) appendix 2204).
Example 2
The invention can be realized by the following method in specific implementation: the traditional Chinese medicine composition of the astragalus mongholicus-cassia twig five-ingredient decoction preparation is prepared from the following raw material medicines in parts by weight: 4 parts of astragalus, 24 parts of cassia twig, 4 parts of white paeony root, 8 parts of ginger and 6 parts of Chinese date, and the astragalus and cassia twig five-substance decoction preparation is prepared by the following method: (1) extracting radix astragali, ramulus Cinnamomi, radix Paeoniae alba, rhizoma Zingiberis recens and fructus Jujubae with distilled water for 2 times in a flash extractor, wherein the water amount added for each extraction is 19 times of the total weight of radix astragali, ramulus Cinnamomi, radix Paeoniae alba, rhizoma Zingiberis recens and fructus Jujubae, the extraction time is 5.6min, the extraction temperature is 50 deg.C, filtering, and mixing filtrates to obtain residue I and filtrate A; adding 9.5 times of ethanol with volume concentration of 95% into the residue I, soaking for 4h, and filtering to obtain filtrate B; distilling filtrate A, collecting volatile oil, concentrating at 55 deg.C under reduced pressure to obtain extract with specific gravity of 1.21 to obtain volatile oil C and extract D; adding 7 times of beta-cyclodextrin into the volatile oil C, grinding and clathrating, freeze drying, and pulverizing into 100 mesh fine powder to obtain beta-cyclodextrin clathrate C; collecting filtrate B, recovering ethanol at 50 deg.C under reduced pressure, concentrating under reduced pressure to obtain extract E with specific gravity of 1.19, lyophilizing, and pulverizing into extract superfine powder of 200 mesh sieve to obtain extract superfine powder A; filtering the extract D with a roll-up membrane with pore size of 10000 molecular weight, recovering solvent from the filtrate under reduced pressure, concentrating under reduced pressure to obtain extract with specific gravity of 1.13 at 25 deg.C, freeze drying, and pulverizing into extract superfine powder of 200 mesh sieve to obtain extract superfine powder B; mixing extract superfine powder A, extract superfine powder B, and beta-cyclodextrin clathrate C, adding adjuvant, and making into tablet; the content of paeoniflorin in the astragalus mongholicus and cassia twig five-ingredient decoction tablet prepared by the invention is not lower than 175.72mg/g (determined by an HPLC method), the content of calycosin glucoside is not lower than 3.78mg/g (determined by an HPLC method), the content of cinnamic acid is not lower than 10.65mg/g (determined by an HPLC method), the content of 6-gingerol is not lower than 8.2mg/g (determined by an HPLC method), and the content of total volatile oil is not lower than 0.1% (ml/g) (the content of the total volatile oil is determined by a volatile oil determination method B according to an 2015 edition, namely, Chinese pharmacopoeia (four parts) appendix 2204).
Example 3
The invention can be realized by the following method in specific implementation: the astragalus and cassia twig five-ingredient decoction preparation is prepared from the following raw material medicines in parts by weight: 3 parts of astragalus, 3 parts of cassia twig, 3 parts of white paeony root, 6 parts of ginger and 4 parts of Chinese date, and the astragalus and cassia twig five-substance decoction preparation is prepared by the following method: (1) extracting radix astragali, ramulus Cinnamomi, radix Paeoniae alba, rhizoma Zingiberis recens and fructus Jujubae with distilled water for 2 times in a flash extractor, wherein the water amount added for each extraction is 15 times of the total weight of radix astragali, ramulus Cinnamomi, radix Paeoniae alba, rhizoma Zingiberis recens and fructus Jujubae, the extraction time is 4.1min, the extraction temperature is 50 deg.C, filtering, and mixing filtrates to obtain residue I and filtrate A; adding 9.5 times of ethanol with volume concentration of 95% into the residue I, soaking for 4h, and filtering to obtain filtrate B; distilling filtrate A, collecting volatile oil, concentrating at 55 deg.C under reduced pressure to obtain extract with specific gravity of 1.13 to obtain volatile oil C and extract D; adding 7 times of beta-cyclodextrin into the volatile oil C, grinding and clathrating, freeze drying, and pulverizing into 100 mesh fine powder to obtain beta-cyclodextrin clathrate C; collecting filtrate B, recovering ethanol at 50 deg.C under reduced pressure, concentrating under reduced pressure to obtain extract E with specific gravity of 1.11, lyophilizing, and pulverizing into extract superfine powder of 200 mesh sieve to obtain extract superfine powder A; filtering the extract D with a roll-up membrane with pore size of 10000 molecular weight, recovering solvent from the filtrate under reduced pressure, concentrating under reduced pressure to obtain extract with specific gravity of 1.13 at 25 deg.C, freeze drying, and pulverizing into extract superfine powder of 200 mesh sieve to obtain extract superfine powder B; mixing the extract superfine powder A, the extract superfine powder B and the beta-cyclodextrin inclusion compound C uniformly, adding auxiliary materials and preparing into capsules; the content of paeoniflorin in the astragalus mongholicus and cassia twig five-ingredient decoction capsule prepared by the invention is not lower than 175.72mg/g (determined by an HPLC method), the content of calycosin glucoside is not lower than 3.78mg/g (determined by an HPLC method), the content of cinnamic acid is not lower than 10.65mg/g (determined by an HPLC method), the content of 6-gingerol is not lower than 8.2mg/g (determined by an HPLC method), and the content of total volatile oil is not lower than 0.1% (ml/g) (the content of the total volatile oil is determined by a volatile oil determination method B according to an 2015 edition, namely, Chinese pharmacopoeia (four parts) appendix 2204).
Example 4
The invention can be realized by the following method in specific implementation: the astragalus and cassia twig five-ingredient decoction preparation is prepared from the following raw material medicines in parts by weight: 4 parts of astragalus, 2 parts of cassia twig, 3 parts of white paeony root, 6 parts of ginger and 3 parts of Chinese date, and the astragalus and cassia twig five-substance decoction preparation is prepared by the following method: (1) extracting radix astragali, ramulus Cinnamomi, radix Paeoniae alba, rhizoma Zingiberis recens and fructus Jujubae with distilled water for 2 times in a flash extractor, wherein the water amount added for each extraction is 19 times of the total weight of radix astragali, ramulus Cinnamomi, radix Paeoniae alba, rhizoma Zingiberis recens and fructus Jujubae, the extraction time is 1.8min, the extraction temperature is 50 deg.C, filtering, and mixing filtrates to obtain residue I and filtrate A; adding 9.5 times of ethanol with volume concentration of 95% into the residue I, soaking for 4h, and filtering to obtain filtrate B; distilling filtrate A, collecting volatile oil, concentrating at 55 deg.C under reduced pressure to obtain extract with specific gravity of 1.13 to obtain volatile oil C and extract D; adding 7 times of beta-cyclodextrin into the volatile oil C, grinding and clathrating, freeze drying, and pulverizing into 100 mesh fine powder to obtain beta-cyclodextrin clathrate C; collecting filtrate B, recovering ethanol at 50 deg.C under reduced pressure, concentrating under reduced pressure to obtain extract E with specific gravity of 1.02, lyophilizing, and pulverizing into extract superfine powder of 200 mesh sieve to obtain extract superfine powder A; filtering the extract D with a roll-up membrane with pore size of 10000 molecular weight, recovering solvent from the filtrate under reduced pressure, concentrating under reduced pressure to obtain extract with specific gravity of 1.13 at 25 deg.C, freeze drying, and pulverizing into extract superfine powder of 200 mesh sieve to obtain extract superfine powder B; mixing extract superfine powder A, extract superfine powder B, and beta-cyclodextrin clathrate C, adding adjuvant, and making into pill; the content of paeoniflorin in the astragalus mongholicus and cassia twig five-material decoction pill prepared by the invention is not lower than 175.72mg/g (determined by an HPLC method), the content of calycosin glucoside is not lower than 3.78mg/g (determined by an HPLC method), the content of cinnamic acid is not lower than 10.65mg/g (determined by an HPLC method), the content of 6-gingerol is not lower than 8.2mg/g (determined by an HPLC method), and the content of total volatile oil is not lower than 0.1% (ml/g) (the content of the total volatile oil is determined by a volatile oil determination method B according to an 2015 edition, namely, appendix 2204 of Chinese pharmacopoeia (four parts)).
The quality control method of the astragalus mongholicus-cassia twig five-ingredient decoction preparation of the invention is explained in detail with reference to specific examples below.
1. Apparatus and materials
1.1 Experimental instruments
Waters e 2695 high performance liquid chromatograph-Waters 2998 diode array detector; KQ-500DE type double-frequency numerical control ultrasonic cleaner (wx-yfcs-002) (ultrasonic instruments, Inc. of Kunshan city); MS105 type electronic analytical balance (wx-yftp-001) (Metler-Torledo instruments (Shanghai) Co., Ltd.); UPT-II-10T ultra pure water machine (Chengdu ultra pure science and technology Co., Ltd.). .
1.2 Experimental reagents and materials
Water is ultrapure water, methanol and acetonitrile are chromatographically pure, formic acid is chromatographically pure, and other reagents are analytically pure. The standards used are as in table 1:
TABLE 1 Standard substance information
Figure BDA0002932250820000071
2. Method and results
2.1 preparation of Experimental drugs
15 batches of astragalus, cassia twig, white paeony root, ginger and Chinese date medicinal materials are respectively taken to prepare 15 batches of astragalus and cassia twig five-material decoction granules according to the embodiment 1 of the invention, and the granules are randomly numbered as SJ01-SJ 15.
TABLE 2 batches of herbs
Figure BDA0002932250820000072
2.2 chromatographic conditions
Establishing a characteristic spectrum and a content determination chromatographic condition of the astragalus-cassia twig five-substance decoction preparation, wherein the common chromatographic condition of the characteristic spectrum and the content determination is as follows: detecting at 278nm, 30 deg.C, 1.0ml/min flow rate, and chromatographic column Thermo Syncronis C18Column, acetonitrile (a) -0.2% aqueous formic acid (B), gradient elution, procedure:
TABLE 3 gradient elution Table
Figure BDA0002932250820000081
2.3 preparation of the solution
2.3.1 preparation of test solutions:
taking 2.1 prepared radix astragali and ramulus Cinnamomi five-substance decoction granules, adding appropriate amount of 70% methanol, treating with ultrasound (250W, 40KHz) for 30min, diluting to 10mL with 70% methanol, shaking, and filtering to obtain the final product.
2.3.2 preparation of Mixed control solutions:
accurately weighing paeoniflorin, calycosin glucoside, cinnamic acid and 6-gingerol reference substances, placing in a volumetric flask, adding methanol to constant volume to scale, shaking uniformly, and making into paeoniflorin, calycosin glucoside, cinnamic acid and 6-gingerol mixed reference substance solutions with concentrations of 3071.73 μ g/mL, 53.17248 μ g/mL, 81.7272 μ g/mL and 192.7072 μ g/mL respectively.
2.4 methodology investigation of Multi-index component content determination
2.4.1 Linear relationship
Sequentially diluting the 2.3.2 mixed reference substance solution by 1, 1.33, 2, 5, 6.67, 10 and 25 times to obtain mixed reference substance solutions with series concentrations, sequentially injecting HPLC, taking the concentration of the series reference substance as a horizontal coordinate X and the corresponding peak area as a vertical coordinate Y, performing linear regression analysis on each chemical component, and calculating a linear regression equation; the linear regression equation of paeoniflorin is as follows: 2029.8X-27765.0, R21.0000; the linear regression equation of calycosin glucoside is as follows: 39521.1X +28358.2, R20.9991; the cinnamic acid linear regression equation is: 175250.0X +22869.7, R20.9999; the linear regression equation of 6-gingerol is as follows: 10802.6X +5961.7, R2＝0.9999。
2.4.2 precision test
And taking the same sample solution, continuously injecting samples for 6 times, measuring peak areas, and calculating RSD. The data are shown in Table 4.
TABLE 4 precision data
Figure BDA0002932250820000091
The result shows that the RSD of each component peak area is less than or equal to 3.1 percent, and the instrument precision is good.
2.4.3. Stability test
Sampling the same sample solution for 0, 2, 4, 6, 8, 10, 12, 16, 20 and 24h respectively, measuring peak area, and calculating RSD. The data are shown in Table 5.
TABLE 5 stability data
Figure BDA0002932250820000092
The result shows that the peak areas RSD of the 4 components are less than or equal to 3.3 percent, and the test solution has good stability within 24 hours.
2.4.4 repeatability test
Respectively taking 6 parts of test solution, carrying out sample injection detection according to 2.2 chromatographic conditions, and calculating the RSD of the peak area. The repeatability data for the 4 components are shown in Table 6.
Table 6 repeatability data
Figure BDA0002932250820000093
Figure BDA0002932250820000101
The result shows that the RSD of the peak areas of the 4 components is less than 4.0 percent, which indicates that the repeatability of the method is good.
2.4.5 sample recovery test
Respectively taking 6 parts of test solution, respectively adding penoniflorin, calycosin glucoside, cinnamic acid and 6-gingerol mixed reference solution, preparing test solution according to item "2.3.1", measuring according to item "2.2" chromatographic condition, and calculating sample recovery rate. The recovery data for the four component samples are shown in tables 7-10.
TABLE 7 Paeoniflorin sample recovery data
Figure BDA0002932250820000102
TABLE 8 Calycosin glucoside sample recovery data
Figure BDA0002932250820000103
TABLE 9 cinnamic acid sample recovery data
Figure BDA0002932250820000104
TABLE 106 gingerol sample application recovery data
Figure BDA0002932250820000105
Figure BDA0002932250820000111
2.5 content determination of random 15 batches of samples
TABLE 11 results of measurements on random 15 batches of samples
Figure BDA0002932250820000112
2.6 methodological investigation of characteristic spectrum of Astragalus mongholicus-cassia twig five-ingredient decoction preparation
2.6.1 precision test
Taking the same sample solution, continuously sampling for 6 times under the chromatographic condition of '2.2', taking the No. 3 peak as a reference peak, and respectively keeping the relative retention time and the relative peak area RSD value of each common chromatographic peak less than 0.5% and 5.0%, which indicates that the precision of the instrument is good.
TABLE 12 precision vs. Retention time
Figure BDA0002932250820000113
Figure BDA0002932250820000121
TABLE 13 precision relative peak area
Figure BDA0002932250820000122
2.6.2 stability test
And taking the same sample solution, respectively injecting samples for 0, 2, 4, 6, 8, 10, 12, 16, 20 and 24 hours, taking the No. 3 peak as a reference peak, and respectively ensuring that the relative retention time of each common chromatographic peak and the RSD value of the relative peak area are less than 0.5 percent and 4.5 percent, thereby indicating that the sample solution has good stability in 24 hours.
TABLE 14 stability relative retention time
Figure BDA0002932250820000123
Figure BDA0002932250820000131
TABLE 15 stability relative peak area
Figure BDA0002932250820000132
2.6.3 repeatability test
Respectively taking 6 parts of test solution, determining according to 2.2 chromatographic conditions, preparing 6 parts of samples according to the test preparation method, performing determination analysis, taking the No. 8 peak as a reference peak, and respectively keeping the relative retention time of each common chromatographic peak and the RSD value of the relative peak area to be less than 0.4% and 11.0%, wherein the result shows that the test preparation method has good repeatability.
TABLE 16 repeatability versus retention time
Figure BDA0002932250820000133
Figure BDA0002932250820000141
TABLE 17 repeatability relative peak area
Figure BDA0002932250820000142
2.7 feature mapping and similarity evaluation
Taking 15 batches of radix astragali and ramulus Cinnamomi five-drug decoction granules, preparing a test solution according to a test solution preparation method, carrying out sample injection determination under the chromatographic condition of '2.2', and recording a chromatogram (see a figure 1-4). The method is introduced into software of a traditional Chinese medicine chromatogram fingerprint similarity evaluation system (2012 edition), a common mode control map is generated by adopting an automatic matching method, the determined 12 common characteristic peaks are sequentially numbered as 1-12 according to retention time, and the similarity is calculated. By comparing with the mixed reference solution, the peak 3 is marked as paeoniflorin, the peak 4 is marked as calycosin glucoside, the peak 8 is marked as cinnamic acid, and the peak 12 is marked as 6-gingerol. Wherein, the No. 3 peak (paeoniflorin) has higher response value, good separation degree and relatively stable retention time, and the No. 3 peak is selected as a reference peak.
TABLE 18 random 15 batches relative retention time
Figure BDA0002932250820000143
Figure BDA0002932250820000151
TABLE 19 random 15 batches of relative peak area
Figure BDA0002932250820000152
TABLE 20 results of similarity evaluation of random 15 lots
Figure BDA0002932250820000161
2.8 detection of characteristic chromatogram of radix astragali-cassia twig five-ingredient decoction particles
Taking 3 batches of the astragalus and cassia twig five-substance decoction granules, preparing a sample solution according to a sample solution preparation method, carrying out sample injection determination under the chromatographic condition of '2.2', and recording a chromatogram. Introducing into software of Chinese medicinal chromatogram fingerprint similarity evaluation system (2012 edition), and generating common mode control chromatogram by automatic matching method, as shown in FIGS. 5-6.
The above embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and the scope of the present invention is defined by the claims. Various modifications and equivalents may be made by those skilled in the art within the spirit and scope of the present invention, and such modifications and equivalents should also be considered as falling within the scope of the present invention.

Claims (6)

1. A preparation method and a quality control method of an astragalus-cassia twig five-ingredient decoction preparation are provided, wherein a traditional Chinese medicine composition of the astragalus-cassia twig five-ingredient decoction preparation is prepared from the following raw material medicines in parts by weight: 2-4 parts of astragalus, 2-4 parts of cassia twig, 2-4 parts of white peony root, 4-8 parts of ginger and 3-6 parts of Chinese date, and is characterized in that the astragalus and cassia twig five-substance decoction preparation is prepared by the following method: (1) extracting radix astragali, ramulus Cinnamomi, radix Paeoniae alba, rhizoma Zingiberis recens and fructus Jujubae with distilled water for 2 times by flash extractor, wherein the water added for each extraction is 12-19 times of the total weight of radix astragali, ramulus Cinnamomi, radix Paeoniae alba, rhizoma Zingiberis recens and fructus Jujubae, the extraction time is 1.8-5.6min, the extraction temperature is 50 deg.C, filtering, and mixing filtrates to obtain residue I and filtrate A; adding 9.5 times of ethanol with volume concentration of 95% into the residue I, soaking for 4h, and filtering to obtain filtrate B; distilling filtrate A, collecting volatile oil, concentrating at 55 deg.C under reduced pressure to obtain extract with specific gravity of 1.05-1.21 to obtain volatile oil C and extract D; adding 7 times of beta-cyclodextrin into the volatile oil C, grinding and clathrating, freeze drying, and pulverizing into 100 mesh fine powder to obtain beta-cyclodextrin clathrate C; collecting filtrate B, recovering ethanol at 50 deg.C under reduced pressure, concentrating under reduced pressure to obtain extract E with specific gravity of 1.02-1.19, lyophilizing, pulverizing into extract superfine powder passing through 200 mesh sieve to obtain extract superfine powder A; filtering the extract D with a roll-up membrane with pore size of 10000 molecular weight, recovering solvent from the filtrate under reduced pressure, concentrating under reduced pressure to obtain extract with specific gravity of 1.13 at 25 deg.C, freeze drying, and pulverizing into extract superfine powder of 200 mesh sieve to obtain extract superfine powder B; mixing the extract superfine powder A, the extract superfine powder B and the beta-cyclodextrin inclusion compound C uniformly, and adding auxiliary materials to prepare a traditional Chinese medicine preparation; the content of paeoniflorin in the Chinese medicinal preparation is not less than 175.72mg/g, the content of calycosin glucoside is not less than 3.78mg/g, the content of cinnamic acid is not less than 10.65mg/g, the content of 6-gingerol is not less than 8.2mg/g, and the content of total volatile oil is not less than 0.1%; the method for simultaneously measuring the characteristic map of the astragalus-cassia twig five-substance decoction preparation and the contents of 4 components of paeoniflorin, calycosin glucoside, cinnamic acid and 6-gingerol comprises the following steps: step 1, preparing a test solution of an astragalus and cassia twig five-substance decoction preparation: taking a proper amount of the astragalus and cassia twig five-material decoction preparation sample, adding a proper amount of 70% methanol for dissolving, transferring to a 10ml volumetric flask, carrying out ultrasonic treatment for 30min at 250w and 40KHz, standing to room temperature, fixing the volume to a scale with 70% methanol, shaking up, filtering, and taking a subsequent filtrate to obtain the astragalus and cassia twig five-material decoction preparation; step 2, preparation of mixed reference solution: accurately weighing penoniflorin, calycosin glucoside, cinnamic acid and 6-gingerol reference substance, placing in a volumetric flask, adding methanol to desired volume to scale, shaking to obtain mixed reference substance solution; step 3, simultaneous determination and characteristic spectrum determination of the content of 4 components in the astragalus and cassia twig five-component decoction preparation: injecting the test solution of the astragalus and cassia twig five-substance decoction preparation prepared in the step 1 into a high performance liquid chromatograph for analysis, and determining the content and the characteristic map of 4 components in the astragalus and cassia twig five-substance decoction preparation sample; the characteristic map of the astragalus-cassia twig five-substance decoction preparation is composed of 12 common peaks, a reference substance is used for comparison, a peak 3 is paeoniflorin, a peak 4 is calycosin glucoside, a peak 8 is cinnamic acid, a peak 12 is 6-gingerol, paeoniflorin is used as a reference substance, a peak 3 is used as a reference peak, the standard comparison characteristic map has 12 common characteristic peaks, a peak corresponding to the reference substance peak is used as an S peak, the relative retention time of each characteristic peak and the S peak is calculated, the relative retention time is within +/-5% of a specified value, and the specified value is peak 1: 0.28, peak 2: 0.56, peak 3: 1.00, peak 4: 1.19, peak 5: 1.35, peak 6: 1.52, peak 7: 1.76, peak 8: 2.36, peak 9: 2.39, peak 10: 2.61, peak 11: 2.87, peak 12: 3.00.
2. the preparation method and the quality control method of the astragalus mongholicus-cassia twig five-ingredient decoction preparation according to claim 1, wherein the traditional Chinese medicine composition of the astragalus mongholicus-cassia twig five-ingredient decoction preparation is prepared from the following raw material medicines in parts by weight: 2 parts of astragalus, 2 parts of cassia twig, 2 parts of white paeony root, 4 parts of ginger and 3 parts of Chinese date, and is characterized in that the astragalus and cassia twig five-substance decoction preparation is prepared by the following method: (1) extracting radix astragali, ramulus Cinnamomi, radix Paeoniae alba, rhizoma Zingiberis recens and fructus Jujubae with distilled water for 2 times in a flash extractor, wherein the water amount added for each extraction is 12 times of the total weight of radix astragali, ramulus Cinnamomi, radix Paeoniae alba, rhizoma Zingiberis recens and fructus Jujubae, the extraction time is 1.8min, the extraction temperature is 50 deg.C, filtering, and mixing filtrates to obtain residue I and filtrate A; adding 9.5 times of ethanol with volume concentration of 95% into the residue I, soaking for 4h, and filtering to obtain filtrate B; distilling filtrate A, collecting volatile oil, concentrating at 55 deg.C under reduced pressure to obtain extract with specific gravity of 1.05 to obtain volatile oil C and extract D; adding 7 times of beta-cyclodextrin into the volatile oil C, grinding and clathrating, freeze drying, and pulverizing into 100 mesh fine powder to obtain beta-cyclodextrin clathrate C; collecting filtrate B, recovering ethanol at 50 deg.C under reduced pressure, concentrating under reduced pressure to obtain extract E with specific gravity of 1.02, lyophilizing, and pulverizing into extract superfine powder of 200 mesh sieve to obtain extract superfine powder A; filtering the extract D with a roll-up membrane with pore size of 10000 molecular weight, recovering solvent from the filtrate under reduced pressure, concentrating under reduced pressure to obtain extract with specific gravity of 1.13 at 25 deg.C, freeze drying, and pulverizing into extract superfine powder of 200 mesh sieve to obtain extract superfine powder B; mixing extract superfine powder A, extract superfine powder B, and beta-cyclodextrin clathrate C, adding adjuvant, and making into granule; the content of paeoniflorin in the granules is not lower than 175.72mg/g, the content of calycosin glucoside is not lower than 3.78mg/g, the content of cinnamic acid is not lower than 10.65mg/g, the content of 6-gingerol is not lower than 8.2mg/g, and the content of total volatile oil is not lower than 0.1%; the method for simultaneously measuring the characteristic map of the astragalus-cassia twig five-material decoction granules and the contents of 4 components of paeoniflorin, calycosin glucoside, cinnamic acid and 6-gingerol comprises the following steps: step 1, preparing a test solution of astragalus mongholicus-cassia twig five-ingredient decoction granules: taking a proper amount of a sample of the astragalus and cassia twig five-material decoction granules, adding a proper amount of 70% methanol for dissolving, transferring the mixture into a 10ml volumetric flask, carrying out ultrasonic treatment on the mixture for 30min at 250w under 40KHz, placing the mixture to room temperature, fixing the volume to a scale with 70% methanol, shaking up, filtering, and taking a subsequent filtrate to obtain the astragalus and cassia twig five-material decoction granules; step 2, preparation of mixed reference solution: accurately weighing penoniflorin, calycosin glucoside, cinnamic acid and 6-gingerol reference substance, placing in a volumetric flask, adding methanol to desired volume to scale, shaking to obtain mixed reference substance solution; step 3, simultaneous determination and characteristic spectrum determination of the content of 4 components in the astragalus and cassia twig five-component decoction granules: injecting the test solution of the radix astragali and cassia twig five-substance decoction granule prepared in the step 1 into a high performance liquid chromatograph for analysis, and determining the content and the characteristic map of 4 components in the radix astragali and cassia twig five-substance decoction granule sample; the characteristic map of the astragalus-cassia twig five-ingredient decoction granules is composed of 12 common peaks, a reference substance is used for comparison, a peak 3 is paeoniflorin, a peak 4 is calycosin glucoside, a peak 8 is cinnamic acid, a peak 12 is 6-gingerol, paeoniflorin is used as a reference substance, a peak 3 is used as a reference peak, the standard comparison characteristic map has 12 common characteristic peaks, a peak corresponding to the reference substance peak is used as an S peak, the relative retention time of each characteristic peak and the S peak is calculated, the relative retention time is within +/-5% of a specified value, and the specified value is peak 1: 0.28, peak 2: 0.56, peak 3: 1.00, peak 4: 1.19, peak 5: 1.35, peak 6: 1.52, peak 7: 1.76, peak 8: 2.36, peak 9: 2.39, peak 10: 2.61, peak 11: 2.87, peak 12: 3.00.
3. the preparation method and the quality control method of the astragalus mongholicus-cassia twig five-ingredient decoction preparation according to claim 1, wherein the traditional Chinese medicine composition of the astragalus mongholicus-cassia twig five-ingredient decoction preparation is prepared from the following raw material medicines in parts by weight: 4 parts of astragalus, 24 parts of cassia twig, 4 parts of white paeony root, 8 parts of ginger and 6 parts of Chinese date, and is characterized in that the astragalus and cassia twig five-substance decoction preparation is prepared by the following method: (1) extracting radix astragali, ramulus Cinnamomi, radix Paeoniae alba, rhizoma Zingiberis recens and fructus Jujubae with distilled water for 2 times in a flash extractor, wherein the water amount added for each extraction is 19 times of the total weight of radix astragali, ramulus Cinnamomi, radix Paeoniae alba, rhizoma Zingiberis recens and fructus Jujubae, the extraction time is 5.6min, the extraction temperature is 50 deg.C, filtering, and mixing filtrates to obtain residue I and filtrate A; adding 9.5 times of ethanol with volume concentration of 95% into the residue I, soaking for 4h, and filtering to obtain filtrate B; distilling filtrate A, collecting volatile oil, concentrating at 55 deg.C under reduced pressure to obtain extract with specific gravity of 1.21 to obtain volatile oil C and extract D; adding 7 times of beta-cyclodextrin into the volatile oil C, grinding and clathrating, freeze drying, and pulverizing into 100 mesh fine powder to obtain beta-cyclodextrin clathrate C; collecting filtrate B, recovering ethanol at 50 deg.C under reduced pressure, concentrating under reduced pressure to obtain extract E with specific gravity of 1.19, lyophilizing, and pulverizing into extract superfine powder of 200 mesh sieve to obtain extract superfine powder A; filtering the extract D with a roll-up membrane with pore size of 10000 molecular weight, recovering solvent from the filtrate under reduced pressure, concentrating under reduced pressure to obtain extract with specific gravity of 1.13 at 25 deg.C, freeze drying, and pulverizing into extract superfine powder of 200 mesh sieve to obtain extract superfine powder B; mixing extract superfine powder A, extract superfine powder B, and beta-cyclodextrin clathrate C, adding adjuvant, and making into tablet; the content of paeoniflorin in the tablet is not lower than 175.72mg/g, the content of calycosin glucoside is not lower than 3.78mg/g, the content of cinnamic acid is not lower than 10.65mg/g, the content of 6-gingerol is not lower than 8.2mg/g, and the content of total volatile oil is not lower than 0.1%; the method for simultaneously measuring the characteristic map of the astragalus-cassia twig five-ingredient decoction tablet and the contents of 4 components of paeoniflorin, calycosin glucoside, cinnamic acid and 6-gingerol comprises the following steps: step 1, preparing a test solution of astragalus mongholicus-cassia twig five-ingredient decoction tablets: taking a proper amount of astragalus and cassia twig five-material decoction tablet samples, adding a proper amount of 70% methanol for dissolving, transferring to a 10ml volumetric flask, carrying out ultrasonic treatment for 30min at 250w and 40KHz, standing to room temperature, fixing the volume to a scale with 70% methanol, shaking up, filtering, and taking a subsequent filtrate to obtain the astragalus and cassia twig five-material decoction tablet; step 2, preparation of mixed reference solution: accurately weighing penoniflorin, calycosin glucoside, cinnamic acid and 6-gingerol reference substance, placing in a volumetric flask, adding methanol to desired volume to scale, shaking to obtain mixed reference substance solution; step 3, simultaneous determination and characteristic spectrum determination of the content of 4 components in the astragalus and cassia twig five-component decoction tablet: injecting the test solution of the astragalus and cassia twig five-substance decoction tablet prepared in the step 1 into a high performance liquid chromatograph for analysis, and determining the content and the characteristic map of 4 components in the astragalus and cassia twig five-substance decoction tablet sample; the characteristic map of the astragalus-cassia twig five-ingredient decoction tablet is composed of 12 common peaks, a reference substance is used for comparison, a peak 3 is paeoniflorin, a peak 4 is calycosin glucoside, a peak 8 is cinnamic acid, a peak 12 is 6-gingerol, paeoniflorin is used as a reference substance, a peak 3 is used as a reference peak, the standard comparison characteristic map has 12 common characteristic peaks, a peak corresponding to the reference substance peak is used as an S peak, the relative retention time of each characteristic peak and the S peak is calculated, the relative retention time is within +/-5% of a specified value, and the specified value is peak 1: 0.28, peak 2: 0.56, peak 3: 1.00, peak 4: 1.19, peak 5: 1.35, peak 6: 1.52, peak 7: 1.76, peak 8: 2.36, peak 9: 2.39, peak 10: 2.61, peak 11: 2.87, peak 12: 3.00.
4. the preparation method and the quality control method of the astragalus mongholicus-cassia twig five-ingredient decoction preparation according to claim 1, wherein the traditional Chinese medicine composition of the astragalus mongholicus-cassia twig five-ingredient decoction preparation is prepared from the following raw material medicines in parts by weight: 3 parts of astragalus, 3 parts of cassia twig, 3 parts of white paeony root, 6 parts of ginger and 4 parts of Chinese date, and is characterized in that the astragalus and cassia twig five-substance decoction preparation is prepared by the following method: (1) extracting radix astragali, ramulus Cinnamomi, radix Paeoniae alba, rhizoma Zingiberis recens and fructus Jujubae with distilled water for 2 times in a flash extractor, wherein the water amount added for each extraction is 15 times of the total weight of radix astragali, ramulus Cinnamomi, radix Paeoniae alba, rhizoma Zingiberis recens and fructus Jujubae, the extraction time is 4.1min, the extraction temperature is 50 deg.C, filtering, and mixing filtrates to obtain residue I and filtrate A; adding 9.5 times of ethanol with volume concentration of 95% into the residue I, soaking for 4h, and filtering to obtain filtrate B; distilling filtrate A, collecting volatile oil, concentrating at 55 deg.C under reduced pressure to obtain extract with specific gravity of 1.13 to obtain volatile oil C and extract D; adding 7 times of beta-cyclodextrin into the volatile oil C, grinding and clathrating, freeze drying, and pulverizing into 100 mesh fine powder to obtain beta-cyclodextrin clathrate C; collecting filtrate B, recovering ethanol at 50 deg.C under reduced pressure, concentrating under reduced pressure to obtain extract E with specific gravity of 1.11, lyophilizing, and pulverizing into extract superfine powder of 200 mesh sieve to obtain extract superfine powder A; filtering the extract D with a roll-up membrane with pore size of 10000 molecular weight, recovering solvent from the filtrate under reduced pressure, concentrating under reduced pressure to obtain extract with specific gravity of 1.13 at 25 deg.C, freeze drying, and pulverizing into extract superfine powder of 200 mesh sieve to obtain extract superfine powder B; mixing the extract superfine powder A, the extract superfine powder B and the beta-cyclodextrin inclusion compound C uniformly, adding auxiliary materials and preparing into capsules; the content of paeoniflorin in the capsule is not lower than 175.72mg/g, the content of calycosin glucoside is not lower than 3.78mg/g, the content of cinnamic acid is not lower than 10.65mg/g, the content of 6-gingerol is not lower than 8.2mg/g, and the content of total volatile oil is not lower than 0.1%; the method for simultaneously measuring the characteristic map of the astragalus-cassia twig five-material decoction capsule and the contents of 4 components of paeoniflorin, calycosin glucoside, cinnamic acid and 6-gingerol comprises the following steps: step 1, preparing a test solution of astragalus mongholicus-cassia twig five-substance decoction capsule: taking a proper amount of astragalus and cassia twig five-material decoction capsule samples, adding a proper amount of 70% methanol for dissolving, transferring to a 10ml volumetric flask, carrying out ultrasonic treatment for 30min at 250w and 40KHz, standing to room temperature, fixing the volume to a scale with 70% methanol, shaking up, filtering, and taking a subsequent filtrate to obtain the astragalus and cassia twig five-material decoction capsule; step 2, preparation of mixed reference solution: accurately weighing penoniflorin, calycosin glucoside, cinnamic acid and 6-gingerol reference substance, placing in a volumetric flask, adding methanol to desired volume to scale, shaking to obtain mixed reference substance solution; step 3, simultaneous determination and characteristic spectrum determination of the content of 4 components in the astragalus and cassia twig five-component decoction capsule: injecting the test solution of the astragalus and cassia twig five-substance decoction capsule prepared in the step 1 into a high performance liquid chromatograph for analysis, and determining the content and the characteristic map of 4 components in the astragalus and cassia twig five-substance decoction capsule sample; the characteristic map of the astragalus-cassia twig five-substance soup capsule is composed of 12 common peaks, a reference substance is used for comparison, a peak 3 is paeoniflorin, a peak 4 is calycosin glucoside, a peak 8 is cinnamic acid, a peak 12 is 6-gingerol, paeoniflorin is used as a reference substance, a peak 3 is used as a reference peak, the standard comparison characteristic map has 12 common characteristic peaks, a peak corresponding to the reference substance peak is used as an S peak, the relative retention time of each characteristic peak and the S peak is calculated, the relative retention time is within +/-5% of a specified value, and the specified value is peak 1: 0.28, peak 2: 0.56, peak 3: 1.00, peak 4: 1.19, peak 5: 1.35, peak 6: 1.52, peak 7: 1.76, peak 8: 2.36, peak 9: 2.39, peak 10: 2.61, peak 11: 2.87, peak 12: 3.00.
5. the preparation method and the quality control method of the astragalus mongholicus-cassia twig five-ingredient decoction preparation according to claim 1, wherein the traditional Chinese medicine composition of the astragalus mongholicus-cassia twig five-ingredient decoction preparation is prepared from the following raw material medicines in parts by weight: 4 parts of astragalus, 2 parts of cassia twig, 3 parts of white paeony root, 6 parts of ginger and 3 parts of Chinese date, and is characterized in that the astragalus and cassia twig five-substance decoction preparation is prepared by the following method: (1) extracting radix astragali, ramulus Cinnamomi, radix Paeoniae alba, rhizoma Zingiberis recens and fructus Jujubae with distilled water for 2 times in a flash extractor, wherein the water amount added for each extraction is 19 times of the total weight of radix astragali, ramulus Cinnamomi, radix Paeoniae alba, rhizoma Zingiberis recens and fructus Jujubae, the extraction time is 1.8min, the extraction temperature is 50 deg.C, filtering, and mixing filtrates to obtain residue I and filtrate A; adding 9.5 times of ethanol with volume concentration of 95% into the residue I, soaking for 4h, and filtering to obtain filtrate B; distilling filtrate A, collecting volatile oil, concentrating at 55 deg.C under reduced pressure to obtain extract with specific gravity of 1.13 to obtain volatile oil C and extract D; adding 7 times of beta-cyclodextrin into the volatile oil C, grinding and clathrating, freeze drying, and pulverizing into 100 mesh fine powder to obtain beta-cyclodextrin clathrate C; collecting filtrate B, recovering ethanol at 50 deg.C under reduced pressure, concentrating under reduced pressure to obtain extract E with specific gravity of 1.02, lyophilizing, and pulverizing into extract superfine powder of 200 mesh sieve to obtain extract superfine powder A; filtering the extract D with a roll-up membrane with pore size of 10000 molecular weight, recovering solvent from the filtrate under reduced pressure, concentrating under reduced pressure to obtain extract with specific gravity of 1.13 at 25 deg.C, freeze drying, and pulverizing into extract superfine powder of 200 mesh sieve to obtain extract superfine powder B; mixing extract superfine powder A, extract superfine powder B, and beta-cyclodextrin clathrate C, adding adjuvant, and making into pill; the content of paeoniflorin in the pill is not lower than 175.72mg/g, the content of calycosin glucoside is not lower than 3.78mg/g, the content of cinnamic acid is not lower than 10.65mg/g, the content of 6-gingerol is not lower than 8.2mg/g, and the content of total volatile oil is not lower than 0.1%; the method for simultaneously measuring the characteristic map of the astragalus-cassia twig five-material decoction pill and the contents of 4 components of paeoniflorin, calycosin glucoside, cinnamic acid and 6-gingerol comprises the following steps: step 1, preparing a test solution of astragalus mongholicus-cassia twig five-ingredient decoction pills: taking a proper amount of astragalus and cassia twig five-material decoction pill sample, adding a proper amount of 70% methanol for dissolving, transferring to a 10ml volumetric flask, carrying out ultrasonic treatment for 30min at 250w and 40KHz, standing to room temperature, fixing the volume to a scale with 70% methanol, shaking up, filtering, and taking a subsequent filtrate to obtain the traditional Chinese medicine preparation; step 2, preparation of mixed reference solution: accurately weighing penoniflorin, calycosin glucoside, cinnamic acid and 6-gingerol reference substance, placing in a volumetric flask, adding methanol to desired volume to scale, shaking to obtain mixed reference substance solution; step 3, simultaneous determination and characteristic spectrum determination of the content of 4 components in the astragalus and cassia twig five-component decoction pill: injecting the test solution of the astragalus and cassia twig five-substance decoction pill prepared in the step 1 into a high performance liquid chromatograph for analysis, and determining the content and the characteristic map of 4 components in the astragalus and cassia twig five-substance decoction pill sample; the characteristic map of the astragalus-cassia twig five-ingredient decoction pill consists of 12 common peaks, a reference substance is used for comparison, a peak 3 is paeoniflorin, a peak 4 is calycosin glucoside, a peak 8 is cinnamic acid, a peak 12 is 6-gingerol, paeoniflorin is used as a reference substance, a peak 3 is used as a reference peak, the standard comparison characteristic map has 12 common characteristic peaks, a peak corresponding to the reference substance peak is used as an S peak, the relative retention time of each characteristic peak and the S peak is calculated, the relative retention time is within +/-5% of a specified value, and the specified value is peak 1: 0.28, peak 2: 0.56, peak 3: 1.00, peak 4: 1.19, peak 5: 1.35, peak 6: 1.52, peak 7: 1.76, peak 8: 2.36, peak 9: 2.39, peak 10: 2.61, peak 11: 2.87, peak 12: 3.00.
6. the preparation method and quality control method of the astragalus and cassia twig five-ingredient decoction preparation according to any one of claims 1 to 5, wherein the characteristic spectrum of the astragalus and cassia twig five-ingredient decoction preparation and the liquid chromatography conditions of the detection method for simultaneously measuring 4 components are as follows: acetonitrile (a) -0.2% aqueous formic acid (B), gradient elution; detection wavelength of 278nm, column temperatureChromatography column Thermo Syncronis C at 30 deg.C and flow rate of 1.0ml/min18Column, gradient elution procedure:
0-5 minutes, the mobile phase A is 4%, and the mobile phase B is 96%;
5-10 minutes, the mobile phase A is 4% -5%, and the mobile phase B is 96% -95%;
10-15 minutes, the mobile phase A is 5% -8%, and the mobile phase B is 95% -92%;
for 15-20 minutes, the mobile phase A is 8% -12%, and the mobile phase B is 92% -88%;
20-25 minutes, the mobile phase A is 12% -16%, and the mobile phase B is 88% -84%;
25-65 minutes, the mobile phase A is 16-20 percent, and the mobile phase B is 84-80 percent;
65-70 minutes, the mobile phase A is 20% -27%, the mobile phase B is 80% -73%;
70-80 minutes, the mobile phase A is 27% -29%, and the mobile phase B is 73% -71%;
80-85 minutes, the mobile phase A is 29-32%, and the mobile phase B is 71-68%;
85-95 minutes, the mobile phase A is 32-50 percent, and the mobile phase B is 68-50 percent;
95-110 minutes, the mobile phase A is 50% -90%, and the mobile phase B is 50% -10%; wherein, the proportion of the mobile phase A and the proportion of the mobile phase B are volume percentage.
CN202110149648.5A 2021-02-03 2021-02-03 Preparation method and quality control method of astragalus and cassia twig five-substance decoction preparation Active CN112870322B (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN202110149648.5A CN112870322B (en) 2021-02-03 2021-02-03 Preparation method and quality control method of astragalus and cassia twig five-substance decoction preparation
CN202211154522.8A CN116046916A (en) 2021-02-03 2021-02-03 Quality control method of astragalus and cassia twig five-ingredient decoction preparation

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110149648.5A CN112870322B (en) 2021-02-03 2021-02-03 Preparation method and quality control method of astragalus and cassia twig five-substance decoction preparation

Related Child Applications (1)

Application Number Title Priority Date Filing Date
CN202211154522.8A Division CN116046916A (en) 2021-02-03 2021-02-03 Quality control method of astragalus and cassia twig five-ingredient decoction preparation

Publications (2)

Publication Number Publication Date
CN112870322A true CN112870322A (en) 2021-06-01
CN112870322B CN112870322B (en) 2022-10-21

Family

ID=76057012

Family Applications (2)

Application Number Title Priority Date Filing Date
CN202211154522.8A Pending CN116046916A (en) 2021-02-03 2021-02-03 Quality control method of astragalus and cassia twig five-ingredient decoction preparation
CN202110149648.5A Active CN112870322B (en) 2021-02-03 2021-02-03 Preparation method and quality control method of astragalus and cassia twig five-substance decoction preparation

Family Applications Before (1)

Application Number Title Priority Date Filing Date
CN202211154522.8A Pending CN116046916A (en) 2021-02-03 2021-02-03 Quality control method of astragalus and cassia twig five-ingredient decoction preparation

Country Status (1)

Country Link
CN (2) CN116046916A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115480011A (en) * 2022-09-20 2022-12-16 广州白云山潘高寿药业股份有限公司 Method for detecting contents of six components in astragalus and cassia twig five-component decoction material standard
CN116448899A (en) * 2023-01-12 2023-07-18 内蒙古壹善药业有限公司 Radix astragali preparation fingerprint detection method

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1279943A (en) * 2000-06-29 2001-01-17 赵国林 Concentrated granule medicine of famous decoction formulation and its preparation
CN102430102A (en) * 2011-12-07 2012-05-02 哈药集团中药二厂 Preparation method for huangqi-guizhi-wuwu granule
CN106265531A (en) * 2016-08-31 2017-01-04 赵国林 The fresh medicine in a kind of soup side is condensed into corpuscular medicament and preparation method thereof

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU2000272667A1 (en) * 2000-09-13 2002-04-29 Jiangsu Kanion Pharmaceutical Co. Pharmaceutical composition treating gynecological blood stasis diseases, cardio and cerebral vascular diseases, respiratory diseases and the like
CN1293092C (en) * 2005-04-26 2007-01-03 沈颜新 Method for separating lacti-streptocin from fermentation liquid of lacti-galactococcus
CN109172635B (en) * 2018-05-16 2021-08-27 上海中医药大学 Preparation method of traditional Chinese medicine composition containing cassia twig
CN112114056A (en) * 2019-06-21 2020-12-22 好医生药业集团有限公司 UPLC-MS method for identifying main effective components in cassia twig, peony and rhizoma anemarrhenae decoction

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1279943A (en) * 2000-06-29 2001-01-17 赵国林 Concentrated granule medicine of famous decoction formulation and its preparation
CN102430102A (en) * 2011-12-07 2012-05-02 哈药集团中药二厂 Preparation method for huangqi-guizhi-wuwu granule
CN106265531A (en) * 2016-08-31 2017-01-04 赵国林 The fresh medicine in a kind of soup side is condensed into corpuscular medicament and preparation method thereof

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
肖旭霖: "《轻工科技兴农》", 30 September 2000, 中国轻工业出版社 *
谭睿: "《天然药物化学实验》", 31 July 2011, 西南交通大学出版社 *
陈革豫等: "经方黄芪桂枝五物汤复方颗粒剂的成型工艺研究", 《现代中药研究与实践》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115480011A (en) * 2022-09-20 2022-12-16 广州白云山潘高寿药业股份有限公司 Method for detecting contents of six components in astragalus and cassia twig five-component decoction material standard
CN116448899A (en) * 2023-01-12 2023-07-18 内蒙古壹善药业有限公司 Radix astragali preparation fingerprint detection method

Also Published As

Publication number Publication date
CN112870322B (en) 2022-10-21
CN116046916A (en) 2023-05-02

Similar Documents

Publication Publication Date Title
CN109709251B (en) Detection method of fingerprint of poria, cassia, rhizoma atractylodis and licorice decoction
CN112870322B (en) Preparation method and quality control method of astragalus and cassia twig five-substance decoction preparation
CN111999423B (en) Establishment method and application of neck pain granule fingerprint spectrum
CN106226440A (en) The method of quality control of SHENGMA GEGEN TANG compositions
CN109172635B (en) Preparation method of traditional Chinese medicine composition containing cassia twig
CN106290599B (en) Content determination method of traditional Chinese medicine composition
CN112903867A (en) Quality control method of poria cocos, cassia twig, rhizoma atractylodis and rhizoma glycyrrhizae decoction substance reference
CN113759035B (en) Construction method of Xiaoqidecoction fingerprint
CN113281439B (en) Quality control detection method of Shenbao tablets
CN112526014B (en) Jinyinliang oral liquid fingerprint spectrum and establishing method thereof
CN110806457B (en) Detection method of fingerprint of Sijun manna drink
CN111879884A (en) Quality control method of Chinese medicinal preparation
CN112881540A (en) Method for detecting bupleurum chinense and vinegar bupleurum chinense formula granules
CN113917002B (en) Construction method of ophiopogon decoction characteristic spectrum
CN113447596B (en) Method for measuring 3 active ingredients in pharmaceutical preparation
CN113281428B (en) Preparation method of jade girl decoction reference substance and fingerprint detection method
CN113759011B (en) Method for establishing characteristic spectrum of starwort root and preparation thereof
CN107894466B (en) Determination method of HPLC fingerprint of Jinsangqi antitoxic preparation and quality control method of Jinsangqi antitoxic preparation
CN110967415B (en) Method for measuring verbascoside in serum-nourishing brain water extract
CN113484429A (en) Method for establishing reference of peach pit qi-bearing soup substance
CN114689776B (en) Construction method of high-efficiency liquid-phase characteristic spectrum of lindera root decoction
CN112362774B (en) Method for measuring content of various effective components in menstruation-regulating and nourishing soup
CN113484428B (en) Construction method of peach pit qi-bearing decoction characteristic spectrum
Qian et al. Simultaneous determination of gallic acid and cinnamic acid content in rhubarb by HPLC.
CN113219095B (en) Construction method of fingerprint of Fukean tablet and fingerprint thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant