CN106177024A - The preparation method of XINKESHU JIAONANG - Google Patents

The preparation method of XINKESHU JIAONANG Download PDF

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Publication number
CN106177024A
CN106177024A CN201610743425.0A CN201610743425A CN106177024A CN 106177024 A CN106177024 A CN 106177024A CN 201610743425 A CN201610743425 A CN 201610743425A CN 106177024 A CN106177024 A CN 106177024A
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radix
time
preparation
salviae miltiorrhizae
thick paste
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张四岩
赵国强
王建允
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HEBEI GOGIN PHARMACEUTICAL CO Ltd
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HEBEI GOGIN PHARMACEUTICAL CO Ltd
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    • 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)
    • A61K36/53—Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
    • A61K36/537—Salvia (sage)
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/25—Araliaceae (Ginseng family), e.g. ivy, aralia, schefflera or tetrapanax
    • A61K36/258—Panax (ginseng)
    • 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)
    • A61K36/28—Asteraceae or Compositae (Aster or Sunflower family), e.g. chamomile, feverfew, yarrow or echinacea
    • A61K36/285—Aucklandia
    • 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
    • A61K36/488—Pueraria (kudzu)
    • 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
    • A61K36/734—Crataegus (hawthorn)
    • 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
    • A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/4841—Filling excipients; Inactive ingredients
    • 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
    • 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
    • A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization

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  • Health & Medical Sciences (AREA)
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Abstract

The invention belongs to the preparation of Chinese patent medicine, particularly relate to the preparation method of a kind of XINKESHU JIAONANG.Including getting the raw materials ready, Radix Notoginseng, the micronizing of the Radix Aucklandiae, the preparation of mixing thick paste, the preparation of Radix Salviae Miltiorrhizae thick paste, it is vacuum dried, makes the processing steps such as capsule.The present invention efficiently solves production cycle length present in prior art, energy consumption is high, efficiency is low, the feature of environmental protection is poor, pelletization is complicated, intermediate products are difficult to store, be prone to the problems such as microbiological contamination, the advantage such as have that active ingredient loses less, technological process is short, production cost is low, energy consumption is low, intermediate products easily store and microbiological contamination rate is low.

Description

The preparation method of XINKESHU JIAONANG
Technical field
The invention belongs to the preparation of Chinese patent medicine, particularly relate to the preparation method of a kind of XINKESHU JIAONANG.
Background technology
XINKESHU JIAONANG is made up of Chinese medicine of the five flavours such as Radix Salviae Miltiorrhizae, Fructus Crataegi, the Radix Aucklandiae, Radix Puerariae, Radix Notoginseng, has blood circulation promoting and blood stasis dispelling, circulation of qi promoting Pain relieving.Uncomfortable in chest, the angina pectoris, hypertension, dizziness, headache, neck pain and the rhythm of the heart that cause for qi stagnation and blood stasis type coronary heart disease lose Often, the disease such as hyperlipidemia.The performance of herbal mixture drug effect is the coefficient result of multicomponent, in order to better control in said preparation Radix Salviae Miltiorrhizae, the Radix Aucklandiae, Radix Puerariae, the content of Radix Notoginseng, be optimized for the preparation technology of XINKESHU JIAONANG and have necessity.
Quality standard of Xinkeshu excludes in " Chinese Pharmacopoeia ", records in ministry standard Traditional Chinese medicine historical preparation the 15th Volume WS3-B-2856-98。
Fructus Crataegi has the effect such as blood fat reducing, blood pressure, heart tonifying, arrhythmia, be also simultaneously spleen benefiting and stimulating the appetite, relieving dyspepsia, The good medicine of phlegm reduction of blood circulation promoting, the disease such as, hernia, blood stasis full to chest and diaphragm spleen, amenorrhea has good curative effect.Flavone compound in Fructus Crataegi Vitexin, is the medicine that a kind of antitumaous effect is stronger, and its extract is equal to suppressing internal growth of cancer cells, propagation and infiltration metastasis Have certain effect.
The Radix Aucklandiae is the dry root of the feverfew Radix Aucklandiae, has antibacterial hepatoprotective, promoting the circulation of QI to relieve pain, soothing the liver, the spleen invigorating of regulating the flow of vital energy disappears stagnant, anti- Bacterium antiinflammatory etc. act on.
Radix Salviae Miltiorrhizae is dry root and the rhizome of labiate Radix Salviae Miltiorrhizae Salvia miltiorrhiza Bge..Having invigorates blood circulation dispels The stasis of blood, inducing menstruation to relieve menalgia, clear away heart-fire relieving restlessness, effect of removing heat from blood eliminating carbuncle.For obstruction of qi in the chest and cardialgia, gastral cavity abdomen hypochondriac pain, abdominal mass abdominal mass gathers, pyretic arthralgia pain, Dysphoria and insomnia, menoxenia, dysmenorrhea amenorrhea, skin infection swells and ache.
Radix Notoginseng has another name called Radix Notoginseng, for Umbellales Araliaceae, is distributed mainly on the ground such as Yunnan, Guangxi, Jiangxi, Sichuan.In Medical material Radix Notoginseng is using its root as medicinal effects, has dissipating blood stasis hemostasis, effect of subduing swelling and relieving pain.Cure mainly spitting of blood, spit blood, nosebleed Blood, has blood in stool, metrorrhagia, traumatic hemorrhage, chest and abdomen twinge, and tumbling down swells and ache.
Radix Puerariae is the dry root of legume pueraria lobata, practises and claims Herba Gelsemii Elegantis.Autumn, season in winter two excavate, and take advantage of fresh-cut and become sheet or fritter； It is dried.Sweet, pungent, cool.There are expelling pathogenic factors from muscles for reducing heat, rash, promoting the production of body fluid to quench thirst, the merit of yang invigorating antidiarrheal.It is usually used in exterior syndrome to generate heat, stiff nape and back, Measles without adequate eruption, calentura is thirsty, and the deficiency of YIN is quenched one's thirst, diarrhea of heat type hematodiarrhoea, diarrhea due to hypofunction of the spleen.
The modernization of Chinese medicine produces and is a complexity and the system engineering of arduousness, relates to many industries and research.The most domestic Enterprise produces the technique of this kind and is substantially the same, and concrete preparation method is: take Radix Notoginseng, Radix Aucklandiae powder is broken into fine powder；Fructus Crataegi, Radix Puerariae add 60% Ethanol warm macerating heating and refluxing extraction secondary, merges alcohol extract, decompression recycling ethanol, is concentrated into relative density 1.35 (20 DEG C)；Red Participating in soak by water secondary, collecting decoction, filter, filtrate is concentrated into relative density 1.35 (20 DEG C)；By above-mentioned two kinds of thick pastes in 80 Dry, pulverize into fine powder and Radix Notoginseng, the mixing of Radix Aucklandiae fine powder at DEG C, make granule, be dried, to obtain final product.
Though existing production technology reasonable, but in the case of the market competitiveness gradually fierceness, above-mentioned existing production work Skill gradually manifests the drawbacks such as production cycle length, energy consumption is high, efficiency is low, the feature of environmental protection is poor, and one is concentration employing one in existing technique As concentration method, in concentration process, loss of effective components is big, and moisture is the most volatile；Two is to filter to use general Filtration, i.e. extracts Gauze directly crossed by liquid or extractum, thus easily block because of insoluble substance gauze hole, time-consuming long, filter thoroughly, waste is big Reason, causes the defects such as effective ingredient loss is big, labor intensity is high；Three is to there is cycle length, effect in wet cream dry run The defects such as rate is low, energy consumption is high, be prone to microbiological contamination, production cost is high；Four is that (content only reaches owing to active constituent content is the most on the low side The lower limit of country's statutory standards limit), patient's medication dose is bigger than normal and medicining cycle is long.
Applicant, through finding the retrieval of domestic patent database, is confined in laboratory in domestic patent documentation mostly Groping of process conditions, and the production technology of mass is not illustrated, thus add XINKESHU JIAONANG mass production Technical study difficulty.
In laboratory, process conditions can not reflect industrial practical situation comprehensively, mainly from the size of material treating capacity Great disparity, equipment performance (as sealing, dispel the heat, manipulation etc.), the factor such as production cost considers, it can thus be appreciated that laboratory result is not It will be apparent that be not directly applicable the big production of mechanization.
Notification number be CN101138373B patent documentation in disclose a kind of compound tea buccal tablets and preparation method thereof, it is public Open following technical scheme: green tea equivalent extract in the present invention, used in vacuum belt-type dryer and be dried to dry extract.This technical side Case is reasonable in design, simple, convenient, and production cost is relatively low.It is green that the compound tea buccal tablets of preparation contains natural bacteriostatic active component Ortho acid, is conducive to keeping oral hygiene, and the tea flavour of tea buccal tablet is dense, in good taste, many containing nutritional labeling, good health care effect.
Notification number be CN103385510B patent documentation in disclose the preparation of a kind of Radix Puerariae mulberry compounded anti-alcoholism beverage Method, it is disclosed that following technical solution: the invention discloses the preparation side of a kind of Radix Puerariae mulberry compounded anti-alcoholism beverage Method, including centrifugal filtration.In the Radix Puerariae that the present invention prepares, puerarin purity is higher, and utilization rate is higher；The present invention prepares drink Material color and luster clarification, transparent, uniformity, aubergine, invariant color；Giving off a strong fragrance, entrance is salubrious, soft persistently, aftertaste is sweet, nothing Abnormal flavour and precipitation, feed liquid is limpid, is visible by naked eyes precipitated impurities.
Above-mentioned patent documentation is discussed respectively for vacuum belt type drying, centrifugal filtration technique, asks present in it Vacuum belt type drying, centrifugal filtration technique etc. are not used the advanced modernization preparation method having a high potential to combine by topic Close research, it is impossible to represent the huge advantage that modernization preparation method plays in specific product.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of XINKESHU JIAONANG.
The overall technology design of the present invention is:
The preparation method of XINKESHU JIAONANG, comprises the technical steps that:
A, get the raw materials ready
Carry out Radix Salviae Miltiorrhizae, Fructus Crataegi, the Radix Aucklandiae, Radix Puerariae, Radix Notoginseng respectively choosing, clean, cutting, drying；
B, Radix Notoginseng, the micronizing of the Radix Aucklandiae
After processing in step a, Radix Notoginseng, the Radix Aucklandiae make Radix Notoginseng fine powder, Radix Aucklandiae fine powder through micronizing；
C, the preparation of mixing thick paste
After Fructus Crataegi after processing in step a, Radix Puerariae add ethanol warm macerating, heating and refluxing extraction, by alcohol extract high speed centrifugation Filtering, decompression recycling ethanol, concentrating and making temperature is that at 20 DEG C, relative density is the mixing thick paste of 1.35；
D, the preparation of Radix Salviae Miltiorrhizae thick paste
Radix Salviae Miltiorrhizae boiling after processing in step a, by decocting liquid centrifugal filtration, filtrate reduced in volume is made temperature and is At 20 DEG C, relative density is the Radix Salviae Miltiorrhizae thick paste of 1.35；
E, vacuum drying
By the most vacuum dried for the Radix Salviae Miltiorrhizae thick paste made in the mixing thick paste made in step c and step d make mixed Close dried cream powder and Radix Salviae Miltiorrhizae extracts dried cream powder；
F, make capsule
The mixing dried cream powder made in step e, Radix Salviae Miltiorrhizae are extracted Radix Notoginseng fine powder, the wood made in dried cream powder and step b Fragrant fine powder mix homogeneously, adds ethanol and makes soft material, makes after screen cloth granulation, airpillow-dry, granulate, inspection, capsule are filled XINKESHU JIAONANG.
XINKESHU JIAONANG prepared by the method for the present invention because prescription proportioning does not change, applicant to each crude drug and The consumption of adjuvant repeats no more.Micronizing in step b uses existing commercial equipment to complete, and applicant is to its technique mistake Journey and relevant parameter repeat no more.
The concrete technology design of the present invention also has:
For making the effective ingredient of medicine be fully dissolved out by alcohol extraction, reaching more preferable extraction effect, preferred technology realizes Mode is, the ethanol warm macerating that in described step c, Fructus Crataegi, Radix Puerariae select percent by volume to be 60% 30 minutes, is heated to reflux carrying Taking twice, the time is 2.5 hours for the first time, and the time is 2 hours for the second time.For quickly removing the impurity in alcohol extract, it is ensured that from Filter effect after the heart, avoids high temperature to concentrate the loss of lower effective ingredient as far as possible, realizes the quick volatilization of ethanol simultaneously, excellent The technical implementation way of choosing is, the rotating speed that described step c high speed is centrifuged is 12000-15000 rev/min, and the time is 15- 20 minutes；The process conditions of decompression recycling ethanol are that temperature is 50-55 DEG C, and pressure is 0.05-0.10 MPa, and the time is that 6-10 is little Time.
It is fully dissolved out for making the effective ingredient of medicine be carried by water, reaches more preferable extraction effect, avoid height the most as far as possible Temperature concentrates the loss of lower effective ingredient, it is achieved the quick volatilization of moisture, preferred technical implementation way is, described step Radix Salviae Miltiorrhizae boiling twice in d, the time is 2 hours for the first time, and the time is 1.5 hours for the second time, and centrifugal rotating speed is 10000- 13000 revs/min, the time is 10-20 minute.The process conditions of concentrating under reduced pressure are that temperature is 60-80 DEG C, and pressure is 0.05- 0.07 MPa, the time is 6-12 hour.
Preferably vacuum drying mode is, the vacuum drying in described step e uses vacuum belt drier, and vacuum is done Dry process conditions are: pressure 0.001-0.005 MPa, temperature 45-50 DEG C, 40-60 minute time, charging rate 50-60 thousand Grams Per Hour, crawler track speeds 3-8 cm per minute.
Substantive distinguishing features and significant technological progress acquired by the present invention are:
1, concentrate under reduced pressure at low temperature, centrifugal filtration and vacuum drying technique are applied to XINKESHU JIAONANG production technology by the present invention In, overcoming loss of effective components in existing technique, extractum is difficult to problems such as being dried；Improve product inherent quality, and have medicine Effect ingredient degradation loss is less, indirectly makes product drug effect improve, has saved drug resource, effective ingredient in prepared product The XINKESHU JIAONANG prepared apparently higher than common process.
2, the state-of-the-art technology such as centrifugal filtration, vacuum belt type drying is applied in industrialized production by the present invention, so that Chinese medicine can better adapt to modernize big production, and prepared XINKESHU JIAONANG meets national standard.
3, use centrifugation technique can be effectively prevented the loss of Effective Component of Chinese Medicine, preserve the activity of medicine to greatest extent Composition, shortened process.
4, in process of vacuum drying, need not add any adjuvant, the granule of dried gained has a certain degree of crystallization effect Should, from microstructure, there is micropore inside simultaneously.After being directly crushed to required particle diameter, the mobility of granule is fine, by Have the open structure of microcosmic in granule, instant capacity is fabulous, and capsule is filled and disintegration all has clear improvement.
5, the present invention uses dried cream powder granule, thus preferably improves the stability of product, not only maintains Chinese medicine The performance of " genuine ", and do not destroy effective ingredient, in the case of crude drug amount and taking dose are constant, medicine effectively becomes Content is divided all to improve a lot.Effectively prevent that microbiological contamination during extractum stores is rotten, the defect of the waste energy, dry cream stores Time limit is longer and steady quality, and production environment is clean, it is possible to significantly Improving The Quality of Products stability and curative effect.
Accompanying drawing explanation
Fig. 1 is protocatechualdehyde thin layer chromatography comparison figure.
In Fig. 1, band from left to right is followed successively by: protocatechualdehyde reference substance；Use product prepared by the method for the present invention； Applicant uses product prepared by former technique；Comparison producer sample.
Fig. 2 is ursolic acid thin layer chromatography comparison figure.
In Fig. 1, band from left to right is followed successively by: use product prepared by the method for the present invention；Applicant uses former technique The product produced；Radix Aucklandiae control medicinal material；Ursolic acid reference substance；Comparison producer XINKESHU JIAONANG sample.
Fig. 3 is XINKESHU JIAONANG puerarin reference substance high-efficient liquid phase chromatogram.
Fig. 4 is that the puerarin content of the XINKESHU JIAONANG using former technique to produce measures high-efficient liquid phase chromatogram.
Fig. 5 is that the puerarin content of the product using the method for the present invention to produce measures high-efficient liquid phase chromatogram.
Fig. 6 is that fertile China board XINKESHU JIAONANG puerarin content measures high-efficient liquid phase chromatogram.
It can be seen that the spot colors using the product prepared of method of the present invention corresponding is deep from Fig. 1-2；Pueraria lobota in Fig. 5 Clear and the content that root element composition separates is high.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described further, but should not be construed as limitation of the invention, the present invention The content recorded with claim of protection domain be as the criterion, any equivalent technical elements made according to description is replaced, all Without departing from protection scope of the present invention.
Embodiment 1
The preparation method of XINKESHU JIAONANG, comprises the technical steps that:
A, get the raw materials ready
Carry out Radix Salviae Miltiorrhizae, Fructus Crataegi, the Radix Aucklandiae, Radix Puerariae, Radix Notoginseng respectively choosing, clean, cutting, drying；
B, Radix Notoginseng, the micronizing of the Radix Aucklandiae
After processing in step a, Radix Notoginseng, the Radix Aucklandiae make Radix Notoginseng fine powder, Radix Aucklandiae fine powder through micronizing；
C, the preparation of mixing thick paste
After Fructus Crataegi after processing in step a, Radix Puerariae add ethanol warm macerating, heating and refluxing extraction, by alcohol extract high speed centrifugation Filtering, decompression recycling ethanol, concentrating and making temperature is that at 20 DEG C, relative density is the mixing thick paste of 1.35；
D, the preparation of Radix Salviae Miltiorrhizae thick paste
Radix Salviae Miltiorrhizae boiling after processing in step a, by decocting liquid centrifugal filtration, filtrate reduced in volume is made temperature and is At 20 DEG C, relative density is the Radix Salviae Miltiorrhizae thick paste of 1.35；
E, vacuum drying
By the most vacuum dried for the Radix Salviae Miltiorrhizae thick paste made in the mixing thick paste made in step c and step d make mixed Close dried cream powder and Radix Salviae Miltiorrhizae extracts dried cream powder；
F, make capsule
The mixing dried cream powder made in step e, Radix Salviae Miltiorrhizae are extracted Radix Notoginseng fine powder, the wood made in dried cream powder and step b Fragrant fine powder mix homogeneously, adds ethanol and makes soft material, makes after screen cloth granulation, airpillow-dry, granulate, inspection, capsule are filled XINKESHU JIAONANG.
XINKESHU JIAONANG prepared by the method for the present embodiment because prescription proportioning do not change, applicant to each crude drug with And the consumption of adjuvant repeats no more.Micronizing in step b uses existing commercial equipment to complete, and applicant is to its technique Process and relevant parameter repeat no more.
The ethanol warm macerating that in described step c, Fructus Crataegi, Radix Puerariae select percent by volume to be 60% 30 minutes, is heated to reflux carrying Taking twice, the time is 2.5 hours for the first time, and the time is 2 hours for the second time, is merged by alcohol extract and uses high speed centrifugation, high The rotating speed that speed is centrifuged is 12000 revs/min, and the time is 15 minutes；The process conditions of decompression recycling ethanol be temperature be 50 DEG C, pressure Power is 0.05 MPa, and the time is 10 hours.
Radix Salviae Miltiorrhizae boiling twice in described step d, the time is 2 hours for the first time, and the time is 1.5 hours for the second time, Centrifugal rotating speed is 10000 revs/min, and the time is 20 minutes.The process conditions of concentrating under reduced pressure be temperature be 60 DEG C, pressure is 0.05 MPa, the time is 12 hours.
Vacuum drying in described step e uses vacuum belt drier, and vacuum drying process conditions are: pressure 0.001 MPa, temperature 45 C, 60 minutes time, charging rate 50 kgs/hr, crawler track speeds 3 cm per minute.
Embodiment 2
The present embodiment is with the difference of embodiment 1:
The rotating speed that described step c high speed is centrifuged is 15000 revs/min, and the time is 15 minutes；Decompression recycling ethanol Process conditions be temperature be 55 DEG C, pressure is 0.10 MPa, and the time is 6 hours.
The rotating speed that described step d high speed is centrifuged is 13000 revs/min, and the time is 10 minutes.The technique of concentrating under reduced pressure Condition be temperature be 80 DEG C, pressure is 0.07 MPa, and the time is 6 hours.
Vacuum drying in described step e uses vacuum belt drier, and vacuum drying process conditions are: pressure 0.005 MPa, temperature 50 C, 40 minutes time, charging rate 60 kgs/hr, crawler track speeds 8 cm per minute.
Remaining content is same as in Example 1.
Embodiment 3
The present embodiment is with the difference of embodiment 1:
The rotating speed that described step c high speed is centrifuged is 13500 revs/min, and the time is 18 minutes；Decompression recycling ethanol Process conditions be temperature be 53 DEG C, pressure is 0.07 MPa, and the time is 8 hours.
The rotating speed that described step d high speed is centrifuged is 12000 revs/min, and the time is 15 minutes.The technique of concentrating under reduced pressure Condition be temperature be 70 DEG C, pressure is 0.06 MPa, and the time is 9 hours.
Vacuum drying in described step e uses vacuum belt drier, and vacuum drying process conditions are: pressure 0.003 MPa, temperature 48 DEG C, 50 minutes time, charging rate 55 kgs/hr, crawler track speeds 6 cm per minute.
Remaining content is same as in Example 1.
Embodiment 4
The present embodiment is with the difference of embodiment 1:
The rotating speed that described step c high speed is centrifuged is 14000 revs/min, and the time is 18 minutes；Decompression recycling ethanol Process conditions be temperature be 54 DEG C, pressure is 0.06 MPa, and the time is 9 hours.
The rotating speed that described step d high speed is centrifuged is 11000 revs/min, and the time is 18 minutes.The technique of concentrating under reduced pressure Condition be temperature be 65 DEG C, pressure is 0.055 MPa, and the time is 7.5 hours.
Vacuum drying in described step e uses vacuum belt drier, and vacuum drying process conditions are: pressure 0.002 MPa, temperature 46.5 DEG C, 55 minutes time, charging rate 52.5 kgs/hr, crawler track speeds 7 cm per minute.
Remaining content is same as in Example 1.
Embodiment 5
The present embodiment is with the difference of embodiment 1:
The rotating speed that described step c high speed is centrifuged is 12500 revs/min, and the time is 16 minutes；Decompression recycling ethanol Process conditions be temperature be 52 DEG C, pressure is 0.06 MPa, and the time is 7 hours.
The rotating speed that described step d high speed is centrifuged is 11000 revs/min, and the time is 13 minutes.The technique of concentrating under reduced pressure Condition be temperature be 75 DEG C, pressure is 0.065 MPa, and the time is 10.5 hours.
Vacuum drying in described step e uses vacuum belt drier, and vacuum drying process conditions are: pressure 0.004 MPa, temperature 46 DEG C, 45 minutes time, charging rate 57.5 kgs/hr, crawler track speeds 4 cm per minute.
Remaining content is same as in Example 1.
For verifying the technique effect of the present invention, the product that the method using embodiment 1-5 is produced by applicant, former technique side Sell on the product of method production and marketFertile China board XINKESHU JIAONANGProperty indices detected, and to detection knot Fruit is contrasted, and the product that former process produces is the product (lot number: 6601201 that applicant produces；Specification: every dress 0.3g),Fertile China board XINKESHU JIAONANG(lot number: 0560206；Specification: every dress 0.3g).
One, its character, discriminating, moisture, disintegration, content uniformity etc. are carried out comparison and detection
The factors such as appearance character, moisture, disintegration, content uniformity directly affect curative effect and the matter of herbal mixture capsule Amount.
(1) experiment place: Hebei Gogin Pharmaceutical Co., Ltd.'s laboratory.
(2) experimental technique: with reference to " Chinese Pharmacopoeia " version in 2015 four.
(3) experimental period: on February 20th, 2016.
(4) participant: Wang Jianyun, Meng Xiangyun, Xu Jiantao.
(5) result such as table 1.
Table 1 related check item contrast table
As known from Table 1, use product that the product prepared of method of embodiment 1-5 prepared with former process andFertile China board XINKESHU JIAONANGContrast, find use embodiment 1-5 method prepare the character of product, moisture (9.0% must not be crossed), The result of the related check items such as content uniformity (± 10%), disintegration (must not spend 30 minutes) all meets regulation.
Two, comparison and detection is carried out for hygroscopicity percentage rate
Modern Chinese medicine preparation is that effective component extracting is made, including natural medicinal plants system from Chinese crude drug mostly Agent.The hygroscopicity of Chinese medicine ingredients is stronger than Western medicine, and the material after moisture absorption can show the bad features such as poor fluidity, stickiness are strong, this Bring bigger difficulty not only to Chinese medicine preparation preparation process, also affect Chinese medicine preparation stability.
(1) experiment place: Hebei Gogin Pharmaceutical Co., Ltd.'s laboratory.
(2) experimental technique: in sample deposits in 25 DEG C, relative humidity is the stability test case under the conditions of 75%, detection Method measures with reference to " Chinese Pharmacopoeia " four aquametries of version in 2015 (general rule 0832).
(3) experimental period: on February 22nd, 2016.
(4) participant: Wang Jianyun, Meng Xiangyun, Xu Jiantao.
(5) result such as table 2.
Table 2 moisture absorption contrast table (%)
It is not difficult to find out by the result in above-mentioned table 1,2, uses the product prepared of method of embodiment 1-5 and former technique Product prepared by method carries out detection contrast, and the product quality using the method for embodiment 1-5 to prepare is more excellent, is difficult to the moisture absorption.
Three, contrast is differentiated
Method under item is differentiated, product prepared by the method using embodiment 1-5 and former in ministry standard XINKESHU JIAONANG Product prepared by process andFertile China board XINKESHU JIAONANGCarry out detection contrast.
(1) reference substance
Ursolic acid: lot number 110742-201220, Nat'l Pharmaceutical & Biological Products Control Institute.
Protocatechualdehyde: lot number 110810-201007, Nat'l Pharmaceutical & Biological Products Control Institute.
(2) reagent
Ether, ethanol, hexamethylene, chloroform, methanol, toluene, ethyl acetate, formic acid, phloroglucinol, sulphuric acid.
(3) experiment place: Hebei Gogin Pharmaceutical Co., Ltd.'s laboratory.
(4) experimenter: Xu Jiantao.
(5) experimental period: on February 24th, 2016.
(6) the results are shown in Table 3.
Table 3 identification result table
It can be seen that use standby two kinds of products of product and other of method of embodiment 1-5 the most aobvious from table 3 and Fig. 1-2 Show speckle, but the product spot colors using the method for embodiment 1-5 standby is deeper.
Four, index composition contrast
Puerarin is one of principle active component of Radix Puerariae, for having raising immunity, strengthens myocardial contraction, protects the heart Myocyte, reduces blood pressure, and has the effects such as antiplatelet aggregation.Radix Puerariae is as one of XINKESHU JIAONANG prescription medical material, puerarin The number of content directly affects drug effect.
(1) chromatographic condition and system suitability
Being filler with octadecylsilane chemically bonded silica, methanol-water (20:80) is flowing phase, and detection wavelength is 250nm, number of theoretical plate is calculated by puerarin peak should be not less than 1500.
(2) preparation of reference substance solution
Precision weighs puerarin reference substance 30% ethanol dilution and becomes every 1ml solution containing 20 μ g, to obtain final product.
(3) preparation of need testing solution
Take content, finely ground, take 0.3g, put in tool plug conical flask, the accurate 30% ethanol 50ml that adds, close plug is weighed heavy Amount, supersound process 30 minutes, let cool, weighed weight.Supply the weight of less loss with 30% ethanol, shake up, filter, discard initial filter Liquid, takes subsequent filtrate as need testing solution.
(4) algoscopy
Precision draws reference substance solution and each 20 μ l of need testing solution respectively, injects chromatograph of liquid, by external standard method, Obtain.
(5) reagent
Methanol, ethanol.
(6) reference substance
Puerarin: lot number 110752-200912, Nat'l Pharmaceutical & Biological Products Control Institute.
(7) instrument
High performance liquid chromatography liquid: Beijing North divides analysis of spectrum instrument Technology Co., Ltd. of China, model S6000.
(8) experiment place: Hebei Gogin Pharmaceutical Co., Ltd.'s laboratory.
(9) experimental period: on February 26th, 2016.
(10) experimenter: Meng Xiangyun, Xu Jiantao.
(11) result such as table 4.
Table 4 active constituent content table
It can be seen that use in the standby product of method of embodiment 1-5 puerarin content higher than former from table 4 and Fig. 4-6 Product prepared by process and fertile China board XINKESHU JIAONANG.
Five, content of microorganisms contrast
(1) aerobe, the mensuration of yeast and mold quantity
Method: with reference to four (general rule 1105) non-sterile product limit test of microbe of " Chinese Pharmacopoeia " version in 2015: micro- Biological counting method.
(2) bile tolerance gram-negative bacteria, escherichia coli and the mensuration of salmonella quantity
Method: with reference to four (general rule 1106) non-sterile product limit test of microbe of " Chinese Pharmacopoeia " version in 2015: control Bacterium inspection technique processed.
(3) experiment place: Hebei Gogin Pharmaceutical Co., Ltd.'s laboratory.
(4) experimenter: Fu Lijuan.
(5) experimental period: on February 20th, 2016.
(6) result such as table 5.
Table 5 microorganism detection Comparative result table
Conclusion: use the product prepared of method of embodiment 1-5 and content of microorganisms in other two kinds of products all meet " in State's pharmacopeia " four oral solid formulation limitation standard in microbes regulations of 2015 years versions, but utilize embodiment of the present invention 1-5 method In the product produced, content of microorganisms is significantly lower than other two kinds.
Seven, clinical comparison test
(1) method
The product that the method using embodiment 1-5 is prepared by applicant has carried out clinical comparison test, particularly as follows:
Dissimilar patient is carried out clinical verification, looks for patient 350 example suffering from coronary heart disease, be equally divided into 7 groups, first 5 groups Illustratively take the product using the method for embodiment 1-5 to prepare, illustratively take applicant for the 6th group and prepare by former process Product (lot number: 6601201；Specification: every dress 0.3g), take fertile China board XINKESHU JIAONANG (lot number: 0560206 for the 7th group； Specification: every dress 0.3g).
(2) curative effect determinate standard: take effect and start to take a turn for the better for symptom, continue drug administration symptom and alleviate.
(3) test site: Shijiazhuang safety hospital.
(4) testing crew: Wang Jianyun, Tao Jun.
(5) test period: on February 25th, 2016.
(6) result such as table 6.
Table 6 Comparison of therapeutic table
Conclusion: take and use that the obvious responding time of product prepared of method of embodiment 1-5 is fast, treatment cycle is short, take Amount is few.
The product using the method for embodiment 1-5 to prepare by above test comparative descriptions is evident in efficacy, and the present invention is permissible It is applied in XINKESHU JIAONANG production technology；The product color using the method for the present invention to prepare is consistent, and good airproof performance, without the moisture absorption And the phenomenons such as adhesion of luming, indices all meets the 15th WS of ministry standard3-B-2856-98 specifies.
About pharmacology and the problem of toxicological experiment of the product utilizing the method for the present invention to prepare, because using the present invention's The reason that product prepared by method and existing XINKESHU JIAONANG do not change in prescription proportioning, composition, clinical trial, application People does not reoffer the result of basal animal and toxicity test.

Claims (6)

1. the preparation method of XINKESHU JIAONANG, it is characterised in that comprise the technical steps that:
A, get the raw materials ready
Carry out Radix Salviae Miltiorrhizae, Fructus Crataegi, the Radix Aucklandiae, Radix Puerariae, Radix Notoginseng respectively choosing, clean, cutting, drying；
B, Radix Notoginseng, the micronizing of the Radix Aucklandiae
After processing in step a, Radix Notoginseng, the Radix Aucklandiae make Radix Notoginseng fine powder, Radix Aucklandiae fine powder through micronizing；
C, the preparation of mixing thick paste
After Fructus Crataegi after processing in step a, Radix Puerariae add ethanol warm macerating, heating and refluxing extraction, by alcohol extract high speed centrifugation, Decompression recycling ethanol, concentrating and making temperature is that at 20 DEG C, relative density is the mixing thick paste of 1.35；
D, the preparation of Radix Salviae Miltiorrhizae thick paste
Radix Salviae Miltiorrhizae boiling after processing in step a, by decocting liquid centrifugal filtration, it is 20 DEG C that filtrate reduced in volume makes temperature Lower relative density is the Radix Salviae Miltiorrhizae thick paste of 1.35；
E, vacuum drying
To make mixing dry by the most vacuum dried for the Radix Salviae Miltiorrhizae thick paste made in the mixing thick paste made in step c and step d Cream powder and Radix Salviae Miltiorrhizae extract dried cream powder；
F, make capsule
The mixing dried cream powder made in step e, Radix Salviae Miltiorrhizae are extracted the Radix Notoginseng fine powder made in dried cream powder and step b, the Radix Aucklandiae thin Powder mix homogeneously, adds ethanol and makes soft material, and making the heart after screen cloth granulation, airpillow-dry, granulate, inspection, capsule are filled can Relieving capsule.
The preparation method of XINKESHU JIAONANG the most according to claim 1, it is characterised in that Fructus Crataegi, Pueraria lobota in described step c The ethanol warm macerating that root selects percent by volume to be 60% 30 minutes, heating and refluxing extraction twice, the time is 2.5 hours for the first time, Time is 2 hours for the second time, is merged by alcohol extract and uses high speed centrifugation.
3. according to the preparation method of the XINKESHU JIAONANG according to any one of claim 1 or 2, it is characterised in that described step The rotating speed that c high speed is centrifuged is 12000-15000 rev/min, and the time is 15-20 minute；The process conditions of decompression recycling ethanol Being that temperature is 50-55 DEG C, pressure is 0.05-0.10 MPa, and the time is 6-10 hour.
The preparation method of XINKESHU JIAONANG the most according to claim 1, it is characterised in that in described step d, Radix Salviae Miltiorrhizae adds water Decocting twice, the time is 2 hours for the first time, and the time is 1.5 hours for the second time, and centrifugal rotating speed is 10000-13000 rev/min Clock, the time is 10-20 minute.
5. according to the preparation method of the XINKESHU JIAONANG described in claim 1 or 4, it is characterised in that described step d reduces pressure The process conditions concentrated are that temperature is 60-80 DEG C, and pressure is 0.05-0.07 MPa, and the time is 6-12 hour.
The preparation method of XINKESHU JIAONANG the most according to claim 1, it is characterised in that the described vacuum in step e is done Dry employing vacuum belt drier, vacuum drying process conditions are: pressure 0.001-0.005 MPa, temperature 45-50 DEG C, time Between 40-60 minute, charging rate 50-60 kg/hr, crawler track speeds 3-8 cm per minute.
CN201610743425.0A 2016-08-29 2016-08-29 The preparation method of XINKESHU JIAONANG Pending CN106177024A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1714836A (en) * 2004-06-30 2006-01-04 天津天士力制药股份有限公司 Use of medicine in preparing medicine for treating anti-aspirin
CN101036707A (en) * 2006-03-13 2007-09-19 北京奇源益德药物研究所 Pill for easing heart and the method for preparing the same

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1714836A (en) * 2004-06-30 2006-01-04 天津天士力制药股份有限公司 Use of medicine in preparing medicine for treating anti-aspirin
CN101036707A (en) * 2006-03-13 2007-09-19 北京奇源益德药物研究所 Pill for easing heart and the method for preparing the same

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Application publication date: 20161207