CN103784505B - 'Chuan Xiong Tea ' - Google Patents
'Chuan Xiong Tea ' Download PDFInfo
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- CN103784505B CN103784505B CN201410076023.0A CN201410076023A CN103784505B CN 103784505 B CN103784505 B CN 103784505B CN 201410076023 A CN201410076023 A CN 201410076023A CN 103784505 B CN103784505 B CN 103784505B
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Abstract
The present invention relates to 'Chuan Xiong Tea '.Specifically, the present invention relates to a kind of 'Chuan Xiong Tea ', said preparation is by including that following medical material is made: Rhizoma Chuanxiong, the Radix Angelicae Dahuricae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae, Radix Saposhnikoviae, Herba Asari, Herba Menthae, Herba Schizonepetae.The invention still further relates to the preparation method of this 'Chuan Xiong Tea '.The 'Chuan Xiong Tea ' of the present invention can be used for treating dispelling wind and relieving, or can treat ailment said due to cold or exposure headache, or have aversion to cold, generate heat, have a stuffy nose.
Description
Technical field
The invention belongs to technical field of Chinese medicines, relate to 'Chuan Xiong Tea ' especially 'Chuan Xiong Tea ', further relate to the preparation side of this 'Chuan Xiong Tea '
Method.
Background technology
Song's " formulary of peaceful benevolent dispensary " is come from Chuan Xiong Tea granular raw side, has dispelling wind and relieving effect, for ailment said due to cold or exposure have a headache, or have aversion to cold,
Heating, nasal obstruction.This side mainly by Rhizoma Chuanxiong, Herba Schizonepetae, Radix Saposhnikoviae, Herba Asari, the Radix Angelicae Dahuricae, Rhizoma Et Radix Notopterygii, Herba Menthae, Radix Glycyrrhizae form (see, Lin Xiaolan. Rhizoma Chuanxiong
Tea adjusts granule clinical practice situation analysis [J]. Beijing traditional Chinese medical science, and 2004,23 (3): 190-192), its determined curative effect.It is believed that Chuan Xiong Tea granule has
Anti-platelet aggregation, alleviates small blood vessel spasm, improves heart and brain tissues blood supply oxygen supply, thus reach blood circulation promoting and blood stasis dispelling, active promote blood circulation, dispelling wind and relieving it
Effect.It is applicable to various headaches and migraine that vascular, nerve, tonicity, cervical spondylosis etc. cause；Be applicable to anemofrigid cold, aversion to cold,
The diseases such as heating, nasal obstruction and sinusitis.Prevention cerebral hemorrhage outbreak, cerebral thrombosis and improve sequal of cerebrovascular diseases.
Chinese Pharmacopoeia version in 2010 one the 472-274 page has included Chuan Xiong Tea ball and two kinds of Traditional Chinese medicine historical preparations of Chuanxiong Chatiao San respectively, and it is joined
Side is Rhizoma Chuanxiong 120g, Radix Angelicae Dahuricae 60g, Rhizoma Et Radix Notopterygii 60g, Herba Asari 30g, Radix Saposhnikoviae 45g, Herba Schizonepetae 120g, Herba Menthae 240g, Radix Glycyrrhizae 60g.Chuan Xiong Tea
Ball is to make each pulverizing medicinal materials mix after becoming fine powder, makes with water pill；Chuanxiong Chatiao San is then to make each pulverizing medicinal materials directly mix after becoming fine powder.
CN1739612A (Chinese Patent Application No.: 200510032127.2, publication date: 2006-03-01, denomination of invention: the Chinese medicine of dispelling wind and relieving
Preparation and preparation method thereof and method of quality control) to disclose the composition that mainly comprises for dispelling wind and relieving be Rhizoma Chuanxiong, the Radix Angelicae Dahuricae, Rhizoma Et Radix Notopterygii, Herba Asari, anti-
Wind, Herba Menthae, Herba Schizonepetae, the Expellin extract pill of Radix Glycyrrhizae or micropill or pellet capsule or capsule or soft capsule, the preparation method of these preparations is: river
Rhizome of chuanxiong, the Radix Angelicae Dahuricae, Rhizoma Et Radix Notopterygii, Herba Asari, Radix Saposhnikoviae, Radix Glycyrrhizae boiling, filter；Herba Menthae, Herba Schizonepetae are extracted its aqueous solution after volatile oil and filter, filtrate with
Above-mentioned medicinal liquid merges, and is concentrated into thick paste, is dried, and mixing after adding suitable adjuvant, sprays into Herba Menthae, Herba Schizonepetae volatile oil, makes drop pill or micropill
Or pellet capsule or capsule or soft capsule.In an example of this invention, this Chinese medicine composition and proportioning and two kinds of Rhizoma Chuanxiongs described in Chinese Pharmacopoeia
Tea modulator is identical, and its preparation process includes: (1) Rhizoma Chuanxiong, the Radix Angelicae Dahuricae, Rhizoma Et Radix Notopterygii, Herba Asari, Radix Saposhnikoviae, Radix Glycyrrhizae boiling 2 times, and each 1.5
Hour, collecting decoction, filter, medicinal liquid is standby；(2) Herba Menthae, Herba Schizonepetae extract volatile oil, standby；Its aqueous solution filters, filtrate and step (1)
Gained medicinal liquid merges, and is concentrated into thick paste, dry, pulverize, obtains fine drug powder, standby；(3) take step (2) gained fine drug powder, spray into step (2)
Gained Herba Menthae, Herba Schizonepetae volatile oil, mixing, obtain hybrid medicine, standby；Then step (3) gained hybrid medicine is prepared as through conventional formulation technique
Drop pill, micropill, capsule, soft capsule etc..Additionally, CN1739612A has also stated that the preparation method of existing Chuan Xiong Tea granule, its step
Suddenly: take Rhizoma Chuanxiong, the Radix Angelicae Dahuricae, Rhizoma Et Radix Notopterygii, Herba Asari, Radix Saposhnikoviae, Radix Glycyrrhizae boiling, decocting liquid filters；After Herba Menthae, Herba Schizonepetae extraction volatile oil, it is water-soluble
Liquid filters, and filtrate merges with above-mentioned medicinal liquid, is concentrated into clear paste, pelletizes, and is dried, sprays into Herba Menthae, Herba Schizonepetae volatile oil, and mixing to obtain final product.
Chinese traditional compound medicine is many because of its medicament composing prescription, the complex chemical composition related to, and every taste medical material would generally be with its typical chemical component table
Levy.For oral solid formulation, medicine stability generally from the standpoint of physical stability and chemical stability two, and as granule this
Planting pharmaceutical preparation, its physical stability is generally easier to reach the requirement of general pharmaceutical preparation, but the most often makes for chemical stability
Those skilled in the art are challenged.
Those skilled in the art need nonetheless remain for effective method and obtain the pharmaceutical preparation such as 'Chuan Xiong Tea ' with superperformance, such as, expect
This 'Chuan Xiong Tea ' has good physical stability and/or chemical stability.
Summary of the invention
It is an object of the invention to provide a kind of new 'Chuan Xiong Tea ', particularly expect that this 'Chuan Xiong Tea ' has good performance and such as has
Good physical stability and/or chemical stability.The inventors discovered that, adding some specific pharmaceutical auxiliaries in 'Chuan Xiong Tea ' substantially has
Help improve the physical stability of medicine and/or chemical stability, or the active substance being favorably improved in granular preparation.The present inventor is based on this
Find and be accomplished.
To this end, first aspect present invention provides a kind of 'Chuan Xiong Tea ', said preparation is by including that following medical material is made: Rhizoma Chuanxiong, the Radix Angelicae Dahuricae, Qiang
Work, Radix Glycyrrhizae, Radix Saposhnikoviae, Herba Asari, Herba Menthae, Herba Schizonepetae.
In one embodiment of the invention, described 'Chuan Xiong Tea ' is Chuan Xiong Tea granular preparation.
'Chuan Xiong Tea ' according to a first aspect of the present invention, the raw medicinal material composition of said preparation includes:
'Chuan Xiong Tea ' according to a first aspect of the present invention, the raw medicinal material composition of said preparation includes:
'Chuan Xiong Tea ' according to a first aspect of the present invention, the raw medicinal material composition of said preparation includes:
'Chuan Xiong Tea ' according to a first aspect of the present invention, the raw medicinal material composition of said preparation includes:
'Chuan Xiong Tea ' according to a first aspect of the present invention, wherein said Rhizoma Chuanxiong, the Radix Angelicae Dahuricae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae, Radix Saposhnikoviae, Herba Asari Six-element medicine be with
The form of its water extract adds.
'Chuan Xiong Tea ' according to a first aspect of the present invention, wherein said Herba Menthae, Herba Schizonepetae are to obtain to extract through vapor distillation together both it
Volatile oil and water extract two parts add.
'Chuan Xiong Tea ' according to a first aspect of the present invention, it is substantially prepared by the method for following steps:
A Rhizoma Chuanxiong, the Radix Angelicae Dahuricae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae, Radix Saposhnikoviae, the medicinal water extract of Herba Asari Six-element are obtained aqueous extract by ()；
B Herba Menthae, both Herba Schizonepetae are extracted the volatile oil and aqueous extract two parts obtained by () with vapor distillation；
C step (a) gained Aqueous extracts is merged by () with step (b) gained Aqueous extracts, concentrate, be dried to obtain extract powder；
D step (b) gained volatile oil and optional pharmaceutic adjuvant are joined in step (c) gained extract powder by (), prepare granule, to obtain final product.
'Chuan Xiong Tea ' according to a first aspect of the present invention, the most also comprises maltodextrin (its English name maltodextrin, CAS registration number
9050-36-6)。
'Chuan Xiong Tea ' according to a first aspect of the present invention, the most also comprises maltodextrin, in terms of the Ligusticum chuanxiong Hort of every 120 weight portions, and wheat
The amount of bud magma essence is 1～30 weight portions.
'Chuan Xiong Tea ' according to a first aspect of the present invention, the most also comprises maltodextrin, in terms of the Ligusticum chuanxiong Hort of every 120 weight portions, and wheat
The amount of bud magma essence is 2～25 weight portions.
'Chuan Xiong Tea ' according to a first aspect of the present invention, the most also comprises maltodextrin, in terms of the Ligusticum chuanxiong Hort of every 120 weight portions, and wheat
The amount of bud magma essence is 5～20 weight portions.
'Chuan Xiong Tea ' according to a first aspect of the present invention, wherein said maltodextrin is in the extracted extraction obtained of described each raw medicinal material
Liquid adds and is condensed into dry extract together with described extracting solution.
'Chuan Xiong Tea ' according to a first aspect of the present invention, wherein said maltodextrin is by addition to described merging in described step (c)
Aqueous extract in mode add.
Owing to the aqueous extract of merging being obtained extract powder through conventional concentration, dry run in step (c), this concentrates, dry run needs
To carry out by the way of heating.It has been unexpectedly discovered that concentration, dry run add appropriate maltose in aqueous extract at this
Dextrin contributes to obtaining the dried object with higher amount glycyrrhizic acid, i.e. by using maltodextrin during concentrate drying so that product
There is the yield of higher glycyrrhizic acid.Additionally it has also been unexpectedly found that, than the extract obtained in the method being not added with maltodextrin or
The Chuan Xiong Tea granular preparation that the most existing method of preparation being prepared as by it is prepared as is compared, extract of the present invention or the Chuan Xiong Tea being made from
Granular preparation has higher stability such as chemical stability, the particularly chemical stability in terms of glycyrrhizic acid and/or the hygroscopic physics of material
Stability.
In view of essence of the invention is that by add maltodextrin make extract of the present invention or be made from Chuan Xiong Tea granular preparation institute in
Existing beat all beneficial effect, and the extract of the present invention substantially can be not added with other adjuvant and directly prepare pharmaceutical preparation such as granule
Agent, can also add some nonactive pharmaceutic adjuvants again for the purpose of dilution, therefore, and Chuan Xiong Tea granule according to a first aspect of the present invention
Preparation, it can be the most only to comprise above-mentioned 8 kinds of Chinese crude drugs to extract extract obtained, i.e. described in above-mentioned steps (d), by step (b) gained
Volatile oil joins in step (c) gained extract powder, the granule (not adding other adjuvant) prepared；Or by step (b) gained volatile oil and
Pharmaceutic adjuvant joins in step (c) gained extract powder, the granule (adding other adjuvant) prepared.
Thus, 'Chuan Xiong Tea ' according to a first aspect of the present invention, the most also include pharmaceutically acceptable adjuvant.
'Chuan Xiong Tea ' according to a first aspect of the present invention, wherein said adjuvant is selected from: sucrose, dextrin, lactose, starch, pregelatinized Starch,
Microcrystalline Cellulose, and combinations thereof.
'Chuan Xiong Tea ' according to a first aspect of the present invention, wherein in terms of the Ligusticum chuanxiong Hort of 120 weight portions that often feed intake, the amount of described adjuvant is to make
The final weight obtaining described Chuan Xiong Tea granule is 300～1000 weight portions.As well known to those skilled in the art, for Chinese medicine preparation, Chinese medicine
Material is extracted, concentrate, the extraction ratio of dry extract that is dried to obtain would generally be in the range of 5～30%, and such as 100 grams medical materials are extracted, dense
Contracting, the dry extract weight being dried to obtain are generally up to 5～30 grams.And for fixing Chinese medicine rate of charge, allow between batches there are
Certain difference；But in order to make final preparation weight between batches consistent, above-mentioned difference can be balanced by adding appropriate adjuvant,
Thus may insure that the concordance of final weight of formulation and the crude drug weight that feeds intake between batches.Therefore, from the angle of above-mentioned production practical operation
Degree is said, the amount of adjuvant can not make concrete restriction, and can be by that above-mentioned " amount of described adjuvant is so that the final of described Chuan Xiong Tea granule
Weight is 300～1000 weight portions " or similar Description Method state.
'Chuan Xiong Tea ' according to a first aspect of the present invention, wherein in terms of the Ligusticum chuanxiong Hort of 120 weight portions that often feed intake, the amount of described adjuvant is to make
The final weight obtaining described Chuan Xiong Tea granule is 350～900 weight portions.
'Chuan Xiong Tea ' according to a first aspect of the present invention, wherein in terms of the Ligusticum chuanxiong Hort of 120 weight portions that often feed intake, the amount of described adjuvant is to make
The final weight obtaining described Chuan Xiong Tea granule is 375～800 weight portions.
'Chuan Xiong Tea ' according to a first aspect of the present invention, wherein said adjuvant is sucrose and dextrin combination.
'Chuan Xiong Tea ' according to a first aspect of the present invention, wherein said adjuvant is sucrose with both dextrin with 1:0.2～the combination of 5 weight ratios.
'Chuan Xiong Tea ' according to a first aspect of the present invention, wherein said adjuvant is lactose and dextrin combination.
'Chuan Xiong Tea ' according to a first aspect of the present invention, wherein said adjuvant is lactose with both dextrin with 1:0.2～the combination of 5 weight ratios,
E.g. lactose and both dextrin are with 1:0.5～the combination of 2 weight ratios.
In the 'Chuan Xiong Tea ' of the present invention, can also add sucrose without sucrose.Benefit without sucrose is to go for
Some special patient such as diabetics, and the benefit adding sucrose be than in use lactose production cost low.
Thus, 'Chuan Xiong Tea ' according to a first aspect of the present invention, it is sugar type granules preparation or sugar-containing type granular preparation.
'Chuan Xiong Tea ' according to a first aspect of the present invention, it is sugar type granules preparation.
'Chuan Xiong Tea ' according to a first aspect of the present invention, it is sugar-containing type granular preparation.
In the present invention, term " sugar type granules preparation " or similar terms, refer to that not comprising sucrose etc. in described granular preparation may use in impact
The adjuvant of medicine person's change of blood sugar.In the present invention, term " sugar-containing type granular preparation " or similar terms, refer to described granular preparation comprises sugarcane
Sugar etc. may affect the adjuvant of medication person's change of blood sugar.
'Chuan Xiong Tea ' according to a first aspect of the present invention, it is unit dose package preparation.Described unit dose package preparation can be composite membrane
Packed, plastic bottle or the packaging of other form.
'Chuan Xiong Tea ' according to a first aspect of the present invention, it is the unit dose package preparation that composite membrane is packed.
'Chuan Xiong Tea ' according to a first aspect of the present invention, it is the unit dose package preparation that composite membrane is packed, and the granule comprised in every bag is with river
Rhizome of chuanxiong medical material is calculated as 1.0～1.5g, the most such as 1.1～1.3g, the most such as 1.15～1.25g, the most e.g., from about 1.2g.Typically, often
The weight of the particulate matter in Dai is 2-10g, such as 3-8g.
Further, second aspect present invention provides and prepares 'Chuan Xiong Tea ' (the such as Rhizoma Chuanxiong described in first aspect present invention any embodiment
Tea modulator) method, said preparation is by including that following medical material is made: Rhizoma Chuanxiong, the Radix Angelicae Dahuricae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae, Radix Saposhnikoviae, Herba Asari, Herba Menthae, Herba Schizonepetae,
The method comprises the following steps:
A Rhizoma Chuanxiong, the Radix Angelicae Dahuricae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae, Radix Saposhnikoviae, the medicinal water extract of Herba Asari Six-element are obtained aqueous extract by ()；
B Herba Menthae, both Herba Schizonepetae are extracted the volatile oil and aqueous extract two parts obtained by () with vapor distillation；
C step (a) gained Aqueous extracts is merged by () with step (b) gained Aqueous extracts, concentrate, be dried to obtain extract powder；
D step (b) gained volatile oil and optional pharmaceutic adjuvant are joined in step (c) gained extract powder by (), prepare granule, to obtain final product.
Method according to a second aspect of the present invention, the raw medicinal material composition of wherein said preparation includes:
Method according to a second aspect of the present invention, the raw medicinal material composition of wherein said preparation includes:
Method according to a second aspect of the present invention, the raw medicinal material composition of wherein said preparation includes:
Method according to a second aspect of the present invention, the raw medicinal material composition of wherein said preparation includes:
Method according to a second aspect of the present invention, the most also Aqueous extracts of the merging in described step (c) are added maltodextrin.Added
Maltodextrin concentrates together with described Aqueous extracts, is dried.
Method according to a second aspect of the present invention, wherein in terms of the Ligusticum chuanxiong Hort of every 120 weight portions, the amount of maltodextrin is 1～30 weight portions.
Method according to a second aspect of the present invention, wherein in terms of the Ligusticum chuanxiong Hort of every 120 weight portions, the amount of maltodextrin is 2～25 weight portions.
Method according to a second aspect of the present invention, wherein in terms of the Ligusticum chuanxiong Hort of every 120 weight portions, the amount of maltodextrin is 5～20 weight portions.
Method according to a second aspect of the present invention, also includes pharmaceutically acceptable adjuvant in wherein obtained 'Chuan Xiong Tea '.
Method according to a second aspect of the present invention, wherein said adjuvant is selected from: sucrose, dextrin, lactose, starch, pregelatinized Starch, crystallite fibre
Dimension element, and combinations thereof.
Method according to a second aspect of the present invention, wherein in terms of the Ligusticum chuanxiong Hort of 120 weight portions that often feed intake, the amount of described adjuvant is so that described river
Rhizome of chuanxiong tea adjusts the final weight of granule to be 300～1000 weight portions.
Method according to a second aspect of the present invention, wherein in terms of the Ligusticum chuanxiong Hort of 120 weight portions that often feed intake, the amount of described adjuvant is so that described river
Rhizome of chuanxiong tea adjusts the final weight of granule to be 350～900 weight portions.
Method according to a second aspect of the present invention, wherein in terms of the Ligusticum chuanxiong Hort of 120 weight portions that often feed intake, the amount of described adjuvant is so that described river
Rhizome of chuanxiong tea adjusts the final weight of granule to be 375～800 weight portions.
Method according to a second aspect of the present invention, wherein in terms of the Ligusticum chuanxiong Hort of 120 weight portions that often feed intake, the amount of described adjuvant is so that described river
Rhizome of chuanxiong tea adjusts the final weight of granule to be 400 weight portions or 780 weight portions.
Method according to a second aspect of the present invention, wherein said adjuvant is sucrose and dextrin combination.
Method according to a second aspect of the present invention, wherein said adjuvant is sucrose with both dextrin with 1:0.2～the combination of 5 weight ratios.
Method according to a second aspect of the present invention, wherein said adjuvant is lactose and dextrin combination.
Method according to a second aspect of the present invention, wherein said adjuvant is lactose with both dextrin with 1:0.2～the combination of 5 weight ratios, e.g. breast
Sugar and both dextrin are with 1:0.5～the combination of 2 weight ratios.
Method according to a second aspect of the present invention, its obtained 'Chuan Xiong Tea ' is sugar type granules preparation (i.e. without sucrose) or sugar-containing type
Grain preparation (i.e. containing sucrose).
Method according to a second aspect of the present invention, its obtained 'Chuan Xiong Tea ' is sugar type granules preparation.
Method according to a second aspect of the present invention, its obtained 'Chuan Xiong Tea ' is sugar-containing type granular preparation.
Known Chuan Xiong Tea granule is the dosage changing form preparation of Chuan Xiong Tea ball or Chuanxiong Chatiao San, its existing national drug standards available to execute,
I.e. standard No. WS3-B-0887-91-2011 is contained.Its [function cures mainly] is dispelling wind and relieving, for ailment said due to cold or exposure have a headache, or have aversion to cold, heating,
Nasal obstruction.
The Chuan Xiong Tea granule of the present invention using the inventive method to obtain has excellent properties as described herein, and therefore, third aspect present invention carries
Supply the Chuan Xiong Tea that method described in 'Chuan Xiong Tea ' described in any one of first aspect present invention or any one of second aspect present invention prepares
Preparation purposes in preparation is used for the medicine of dispelling wind and relieving.
Or, third aspect present invention provides 'Chuan Xiong Tea ' described in any one of first aspect present invention or any one of second aspect present invention
The 'Chuan Xiong Tea ' that described method prepares is had a headache for ailment said due to cold or exposure in preparation, or have aversion to cold, generate heat, purposes in the medicine had a stuffy nose.
Arbitrary technical characteristic in any embodiment of either side of the present invention can combine with other embodiment of this aspect, or can be with
Any embodiment combination of other side, as long as this combination does not haves contradiction.Whole documents that the present invention quotes are incorporated herein by.
Rhizoma Chuanxiong used by the present invention is the dry rhizome of samphire Rhizoma Chuanxiong Ligustiucum chuanxiong Hort..Summer is when the joint dish on stem
Notable prominent, and excavate during purplish, remove silt, shine post-drying, then remove fibrous root.This product meets " Chinese Pharmacopoeia " 2010 editions one 38
Specify under page Rhizoma Chuanxiong item.
The Radix Angelicae Dahuricae used by the present invention is samphire Radix Angelicae Dahuricae Angelica dahurica (Fisch.ex Hoffm.) Benth.et Hook.f. or Radix angelicae dahuricae
The dry root of Angelica dahurica (Fisch.ex Hoffm.) Benth.et Hook.f.var.formosana (Boiss.) Shan et yuan.Leaf between summer, autumn
Excavate time yellow, remove fibrous root and silt, dry or cold drying；This product meets regulation under " Chinese Pharmacopoeia " 2010 editions page 97 Radix Angelicae Dahuricae items.
Rhizoma Et Radix Notopterygii used by the present invention is samphire Rhizoma Et Radix Notopterygii Notopterygium incisum Ting exH.T.Chang or Radix et Rhizoma Notopterygii
The dry rhizome of Notopterygium franchetii H.de Boiss. and root.Spring, season in autumn two excavate, and remove fibrous root and silt, dry.This product accords with
Close and specify under " Chinese Pharmacopoeia " 2010 editions page 170 Rhizoma Et Radix Notopterygii items.
Herba Asari used by the present invention is aristolochiaceae plant Herba Asari Asarum heterotropoides Fr.Schmidt
Var.mandshuricum (Maxim.) Kitag., Seoul Herba Asari Asarum sieboldii Miq.var.seoulense Nakai or China Herba Asari Asarum
The dry root of sieboldii Miq. and rhizome.The first two is planted to practise and claims " Herba Asari ".Summer, fructescence or excavate early autumn, Ex-all aerial parts and silt, cloudy
Dry.This product meets regulation under " Chinese Pharmacopoeia " 2010 editions page 214 Herba Asari items.
Radix Saposhnikoviae used by the present invention: for the dry root of umbelliferae Saposhnikovia divaricata Saposhnikovia divaricata (Turcz.) Schischk..Spring, autumn two
Excavate the root not taking out scape plant season, remove fibrous root and silt, dry.This product meets under " Chinese Pharmacopoeia " 2010 editions page 140 Radix Saposhnikoviae items
Regulation.
Herba Schizonepetae used by the present invention is the dry aerial parts of labiate Herba Schizonepetae Schizonepeta tenuifolia Briq..Summer, season in autumn two, the flowers are in blossom
Tap time green to top, fringe, remove impurity, dry.This product meets regulation under " Chinese Pharmacopoeia " 2010 editions page 216 Herba Schizonepetae items.
Herba Menthae used by the present invention is the dry aerial parts of labiate Herba Menthae Mentha haplocalyx Briq..Summer, season in autumn two stem and leaf luxuriant
Or when the flowers are in blossom to three-wheel, select fine day, tap by several times, dry or dry in the shade.This product meets under " Chinese Pharmacopoeia " 2010 editions page 354 Herba Menthae items
Regulation.
Radix Glycyrrhizae used by the present invention is glycyrrhizic legume Glycyrrhiza uralensis Fisch., Glycyrrhiza inflata Bat. Glycyrrhiza inflata Bat. or light
The really dry root of Radix Glycyrrhizae Glycyrrhiza glabra L. and rhizome.Spring, season in autumn two excavate, and remove fibrous root, dry.This product meets " Chinese Pharmacopoeia "
Specify under 2010 editions page 80 Radix Glycyrrhizae items.
Detailed description of the invention
The present invention can be conducted further description by the following examples, but, the scope of the present invention is not limited to following embodiment.This
Practitioners will appreciate that of field, on the premise of without departing substantially from the spirit and scope of the present invention, can carry out various change and modification to the present invention.
The present invention to test used in material and test method carry out generality and/or concrete description.Although being made by realizing the object of the invention
Many materials and operational approach be it is known in the art that but the present invention still describe in detail as far as possible at this.
Some test instrunments used in the present invention include with reagent: Agilent1100 high performance liquid chromatograph；Diamonisil (R) diamond C18
Chromatographic column (250mm × 4.6mm, 5 μm)；Ferulic acid (purchased from Nat'l Pharmaceutical & Biological Products Control Institute, lot number 110773-200611)；Ammonium glycyrrhizinate (is purchased
From Nat'l Pharmaceutical & Biological Products Control Institute, lot number 110731-201116).In tests below, when relating to weight portion, if not otherwise indicated, each
Weight portion unit is 0.1kg.In following preparation example and comparison preparation example, if not otherwise indicated, the yield of extract (including volatile oil part) all exists
Between 15～25% (based on medical material gross weight).When preparing Chuan Xiong Tea (granule) preparation below, the most all by obtained granule with often
The granule comprised in Dai is calculated as 1.2g with Ligusticum chuanxiong Hort, is sub-packed in aluminum-plastic composite membrane bag, preserves or detection for long-term.
A, the quality investigation method of Chuan Xiong Tea granule
The quality investigation method that this part provides, may be used for investigation present invention acquisition does not adds the auxiliary granular preparation made, it is also possible to be used for investigating
What the present invention obtained adds the auxiliary granular preparation (including sugar-containing type and Sugarless type) made；These granular preparations are investigated in the operation of method below,
All it is properly termed as this product or test sample.These quality investigation methods and the index limit being directed to are basically identical with existing product standard.
Investigation method example 1: the discriminating of granular preparation
Differential method 1:Take this product 4g, finely ground, put in tool plug conical flask, add diethyl ether 20ml, close plug, shaking, supersound process 20 points in ice bath
Clock, filters, and filtrate is waved to about 1ml, as need testing solution.Separately take Mentholum reference substance appropriate, add ethanol and make every 1ml containing 0.5mg's
Solution, as reference substance solution.Test according to thin layer chromatography (Chinese Pharmacopoeia one annex VI B of version in 2010), draw above two solution each
10 μ l, put respectively on the same silica gel g thin-layer plate with sodium carboxymethyl cellulose as adhesive, with toluene-ethyl acetate (17:3) as developing solvent,
Launching, take out, dry, spray, with 5% vanillin-sulfuric acid solution, is heated to spot development at 105 DEG C clear.In test sample chromatograph, with compare
On the corresponding position of product chromatograph, the speckle of aobvious same color.
Differential method 2:Taking this product 8g, finely ground, the 100ml that adds water makes dissolving, centrifugal, takes supernatant, extracts 2 times with ether shaking, each 30ml,
Merge ether solution, be concentrated into about 1ml, as need testing solution.Separately taking Rhizoma Chuanxiong control medicinal material 0.3g, add diethyl ether 20ml, close plug, supersound process
20 minutes, filtering, filtrate is waved to about 1ml, as control medicinal material solution.According to thin layer chromatography (Chinese Pharmacopoeia one annex VI B of version in 2010)
Test, draws each 10 μ l of above two solution, puts respectively on the same silica gel g thin-layer plate with sodium carboxymethyl cellulose as adhesive, with hexamethylene
Alkane-ethyl acetate (9:1) is developing solvent, launches, and takes out, dries, put and inspect under ultra-violet lamp (365nm).In test sample chromatograph, with compare
On the corresponding position of medical material chromatograph, a fluorescence principal spot of aobvious same color.
Differential method 3:Taking Rhizoma Et Radix Notopterygii control medicinal material 0.5g, add water 50ml, decocts 20 minutes, lets cool, centrifugal, takes supernatant, shakes with ether
Extract 2 times, each 20ml, merge ether solution, wave to about 1ml, as control medicinal material solution.According to thin layer chromatography (Chinese Pharmacopoeia 2010
One annex VI B of version) test, draw the need testing solution under differential method 2 and each 15 μ l of above-mentioned control medicinal material solution, put respectively in same with
Sodium carboxymethyl cellulose is on the silica gel g thin-layer plate of adhesive, with cyclohexane-ethyl acetate (8:2) as developing solvent, launches, takes out, dry,
Spraying with 10% ethanol solution of sulfuric acid, 85 DEG C are heated about 5 minutes, put and inspect under ultra-violet lamp (365nm).In test sample chromatograph, with compare medicine
Wood color is composed on corresponding position, the fluorescence principal spot of aobvious same color.
Differential method 4:Take this product 8g, finely ground, add acetone 50ml, supersound process 20 minutes, filter, filtrate is evaporated, and residue adds methanol 1ml
Make dissolving, by neutral alumina column (100～200 mesh, internal diameter 1cm, 2g), with 80% methanol solution 5ml eluting, collect eluent, steam
Dry, residue adds methanol 0.5ml makes dissolving, as need testing solution.Separately take Radix Saposhnikoviae control medicinal material 1g, add acetone 10ml, be made in the same way of comparison medicine
Material solution.Take cimicifugoside reference substance again and 5-O-methyl-visamminol reference substance is appropriate, add methanol respectively and make every 1ml respectively containing 1mg
Solution, as reference substance solution.Test according to thin layer chromatography (Chinese Pharmacopoeia one annex VI B of version in 2010), absorption need testing solution 20 μ l,
Reference substance solution and each 10 μ l of control medicinal material solution, put respectively on the same silica GF254 lamellae with sodium carboxymethyl cellulose as adhesive,
With methylene chloride-methanol (4:1) as developing solvent, launch, take out, dry, put and inspect under ultra-violet lamp (254nm).In test sample chromatograph, with
On the corresponding position of control medicinal material chromatograph, the principal spot of aobvious same color, on position corresponding with reference substance chromatograph, the speckle of aobvious same color.
Differential method 5:Taking this product 8g, finely ground, add diethyl ether 40ml, is heated to reflux 30 minutes, lets cool, and filters, discards filtrate, and filtering residue volatilizes
Ether, adds methanol 30ml, is heated to reflux 1 hour, lets cool, and filters, and filtrate is evaporated, and the residue 40ml that adds water makes dissolving, with water saturated just
Butanol shaking is extracted 2 times, and each 20ml merges n-butyl alcohol liquid, with the water 50ml washing that n-butyl alcohol is saturated, discards water liquid, and n-butyl alcohol liquid steams
Dry, residue adds methanol 1ml makes dissolving, as need testing solution.Another extracting liquorice control medicinal material 1g, add diethyl ether 20ml, is made in the same way of comparison medicine
Material solution.Test according to thin layer chromatography (Chinese Pharmacopoeia one annex VI B of version in 2010), draw each 10 μ l of above two solution, put respectively in same
On one silica gel g thin-layer plate with sodium carboxymethyl cellulose as adhesive, with acetic ether-methanoic acid-glacial acetic acid-water (15:1:1:2) as developing solvent,
Launching, take out, dry, spray, with 10% ethanol solution of sulfuric acid, is heated to spot development at 105 DEG C clear.In test sample chromatograph, with compare
On the corresponding position of medical material chromatograph, aobvious identical yellow principal spot.
Differential method 6:Taking this product 4g, add water 50ml, supersound process 10 minutes, centrifugal, takes supernatant, with dilute hydrochloric acid regulation pH value to 2～
3, extract 2 times with dichloromethane shaking, each 20ml, combined dichloromethane liquid, be evaporated, residue adds methanol 1ml makes dissolving, as examination
Product solution.Separately take Radix Angelicae Dahuricae control medicinal material 1g, be made in the same way of control medicinal material solution.According to thin layer chromatography (Chinese Pharmacopoeia one annex of version in 2010
VI B) test, draw each 10 μ l of above two solution, put respectively on the same silica gel g thin-layer plate with sodium carboxymethyl cellulose as adhesive,
With petroleum ether (30～60 DEG C)-ether (12:7) as developing solvent, launch, take out, dry, put and inspect under ultra-violet lamp (254nm).Test sample color
In spectrum, on position corresponding with control medicinal material chromatograph, the fluorescence principal spot of aobvious same color.
Investigation method example 2: the assay of granular preparation
Determination 1: measure Rhizoma Chuanxiong, the content of Rhizoma Et Radix Notopterygii
(lucifuge operation) is measured according to high performance liquid chromatography (Chinese Pharmacopoeia one annex VI D of version in 2010)
Chromatographic condition and system suitability: with octadecylsilane chemically bonded silica as filler；With acetonitrile-2% glacial acetic acid solution (10:90)
For flowing phase；Detection wavelength is 323nm.Number of theoretical plate is calculated by ferulic acid peak should be not less than 8000.
The preparation of reference substance solution: take ferulic acid reference substance appropriate, accurately weighed, add 45% ethanol-glacial acetic acid (20:1) mixed solution and make often
The 1ml solution containing 10 μ g, to obtain final product.
The preparation of need testing solution: take this product under content uniformity item, finely ground, take about 1.5g, accurately weighed, precision adds 45% ethanol-ice vinegar
Acid (20:1) mixed solution 25ml, weighed weight, heating and refluxing extraction 30 minutes, let cool, more weighed weight, with 45% ethanol-glacial acetic acid (20:
1) mixed solution supplies the weight of less loss, shakes up, centrifugal (4000 revs/min) 10 minutes, takes supernatant, to obtain final product.
Algoscopy: precision draws reference substance solution and each 10 μ l of need testing solution respectively, injects chromatograph of liquid, measures, to obtain final product.
Typically, it is desirable to this product every bag in terms of ferulic acid (C10H10O4), must not be less than 0.39mg containing Rhizoma Chuanxiong and Rhizoma Et Radix Notopterygii.
Determination 2: measure the content of Radix Glycyrrhizae
Measure according to high performance liquid chromatography (Chinese Pharmacopoeia one annex VI D of version in 2010)
Chromatographic condition and system suitability: with octadecylsilane chemically bonded silica as filler；With acetonitrile-0.5% phosphoric acid solution (containing 1mmol/L
Ammonium acetate) (33:67) for flowing phase；Detection wavelength is 254nm.Number of theoretical plate is calculated by ammonium glycyrrhizinate peak should be not less than 4000.
The preparation of reference substance solution: extracting liquorice acid ammonium reference substance is appropriate, accurately weighed, adds methanol dissolving and makes every 1ml containing ammonium glycyrrhizinate 50 μ g (folding
Close glycyrrhizic acid be 48.975 μ g) solution, to obtain final product.
The preparation of need testing solution: take this product under content uniformity item, finely ground, take about 1g, accurately weighed, to put in tool plug conical flask, precision adds
70% ethanol solution 20ml, weighed weight, supersound process (power 500W, frequency 53kHz) 30 minutes, let cool, more weighed weight, with 70%
Ethanol solution supplies the weight of less loss, shakes up, and filters, takes subsequent filtrate, to obtain final product.
Algoscopy: precision draws reference substance solution and each 20 μ l of need testing solution respectively, injects chromatograph of liquid, measures, to obtain final product.
Typically, it is desirable to this product every bag in terms of glycyrrhizic acid (C42H62O16), must not be less than 4.0mg containing Radix Glycyrrhizae.
B, the 'Chuan Xiong Tea ' of the preparation present invention
Preparation example 1:
Raw medicinal material forms:
Preparation method:
A (), by Rhizoma Chuanxiong, the Radix Angelicae Dahuricae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae, Radix Saposhnikoviae, the medicinal water extract of Herba Asari Six-element, i.e. boiling secondary, adds 8 times amount for the first time
Water, decocts 1.5 hours, and second time adds 6 times amount water, decocts 1 hour, and decocting liquid filters, and filtrate merges, and obtains aqueous extract；
B Herba Menthae, both Herba Schizonepetae are added 8 times amount water by (), vapor distillation extracts volatile oil 2.5 hours, obtains volatile oil and aqueous extract (filtration)
Two parts；
C step (a) gained Aqueous extracts is merged by () with step (b) gained Aqueous extracts, add the maltodextrin of 10 weight portions, be concentrated into relative density
For the extractum of 1.12-1.16 (80 DEG C), it is spray-dried (intake air temperature 230 DEG C, air outlet temperature 110 DEG C), obtains extract powder；
D step (b) gained volatile oil and appropriate lactose, dextrin (the two uses with weight ratio 1:1 ratio) are joined step (c) gained extractum by ()
In powder, making material always weigh 400 weight portions, prepare granule, every 4g granule is equivalent to 1.2g Ligusticum chuanxiong Hort, uses compound membrane bag subpackage, to obtain final product,
Sample is designated as Ex1.
Glycyrrhizic acid yield algoscopy:
The Radix Glycyrrhizae (60 weight portion) of formula ratio is extracted according to step (a) method and obtains aqueous extract, measure in this aqueous extract sweet with determination 2
The amount (being calculated as W0) of oxalic acid, the amount of the glycyrrhizic acid that this amount obtains after extracted by the Radix Glycyrrhizae that fed intake, it is not affected by subsequent technique；
Further, measure the content of glycyrrhizic acid in the granular preparation sample Ex1 that this preparation example prepares, calculate by the Radix Glycyrrhizae of formula inventory through carrying
Take, preparation processing obtains the amount (being calculated as W1) of the glycyrrhizic acid in final granule, the Radix Glycyrrhizae of W0 amount in this amount reflection step (a) gained aqueous extract
The glycyrrhizic acid amount that acid is remaining after subsequent technique processes；
Glycyrrhizic acid yield with following formula calculating preparation example 1 granular preparation: glycyrrhizic acid yield (%)=(W1/W0) × 100%.Result preparation example 1 granule
The glycyrrhizic acid yield of preparation is 98.2%, shows the preparation that the inventive method obtains, and its glycyrrhizic acid acquisition rate is at a relatively high.
Glycyrrhizic acid stability determination method:
The chemical stability that this law characterizes with glycyrrhizic acid for the granular preparation of the present invention investigated in dry granular preparation form, HPLC algoscopy is adopted
Carry out with determination 2；
The granular preparation sample Ex1 that this preparation example packed by compound membrane bag prepares is placed in 45 DEG C of calorstats placement and (in the present invention may be used for 4 months
Referred to as high-temperature treatment or high temperature is disposed or is similar to appellation April), measure sample before this high-temperature treatment wherein glycyrrhizic acid content (represent with M0,
Unit represents with the mg amount of glycyrrhizic acid in every gram of granule, i.e. mg/g), and measure sample postpone at this high temperature April wherein glycyrrhizic acid content (with
M1 represents, unit represents with the mg amount of glycyrrhizic acid in every gram of granule, i.e. mg/g)；
The remaining rate postponed at the method with glycyrrhizic acid in following formula calculating sample: remaining rate (%)=(M1/M0) × 100%.Result preparation example 1
It is 98.6% that the glycyrrhizic acid remnants of grain preparation lead, and shows the preparation that the inventive method obtains, the most preferable with the chemical stability that glycyrrhizic acid characterizes.
Melting investigation method:
This law is carried out with reference to Chinese Pharmacopoeia annex IC granule [melting] method in 2010, for investigating in dry granular preparation form
Granular preparation of the present invention dissolve performance；
Take 1 bag of granular preparation (its amount is calculated as 1.2g with Ligusticum chuanxiong Hort), add hot water 200ml, stir 5 minutes, observe melting immediately, with all
Dissolve 5 points, all dissolve but have little cloudy obtain 4 points, the most entirely dissolve have suspended matter obtain 3 points, the most entirely dissolve have precipitate obtain 2 points, no
Energy fine dispersion obtains the evaluation criterion of dissolving of 1 point, and the test of every batch sample is averaged for 5 times, calculates melting score；
For same batch to be tested, test high temperature mentioned above and dispose the melting score of forward and backward sample April, be designated as T0 and T1 respectively, under using
Formula calculates sample and dissolves speed after high-temperature treatment: dissolve speed (%)=(T1/T0) × 100%.
This dissolves speed is to show when 100% that melting speed is the most unchanged after high-temperature treatment, shows that granular preparation is through height when this value is more than 100%
Melting speed is postponed slack-off, when dissolving speed < in the range of 150% the most acceptable, this parameter characterization granular preparation of the present invention is molten at Wen
Physical stability in terms of solution property.After measured, the speed of dissolving of preparation example 1 granular preparation is 118%, shows the preparation that the inventive method obtains
Physical stability in terms of dissolubility is the most preferable.
Preparation example 2:
Raw medicinal material forms:
Preparation method: substantially identical with preparation example 1, but step (c) uses the maltodextrin of 7.5 weight portions, lactose, dextrin two in step (d)
Person uses with weight ratio 1:0.5 ratio and adds and makes material always weigh 375 weight portions in right amount.Gained sample is designated as Ex2.With reference in preparation example 1
It is 98.7% that glycyrrhizic acid yield algoscopy measures the glycyrrhizic acid yield of this preparation example gained granular preparation sample.Steady with reference to the glycyrrhizic acid in preparation example 1
Qualitative assay measures this preparation example gained granular preparation sample glycyrrhizic acid remnants after high-temperature treatment and leads is 98.1%.With reference in preparation example 1
Melting is investigated method and measured this preparation example gained granular preparation sample speed of dissolving after high-temperature treatment is 96%.
Preparation example 3:
Raw medicinal material forms:
Preparation method: substantially identical with preparation example 1, but step (c) uses the maltodextrin of 15 weight portions, lactose, dextrin two in step (d)
Person uses with weight ratio 1:2 ratio and adds and makes material always weigh 450 weight portions in right amount.Gained sample is designated as Ex3.With reference in preparation example 1
It is 98.2% that glycyrrhizic acid yield algoscopy measures the glycyrrhizic acid yield of this preparation example gained granular preparation sample.Steady with reference to the glycyrrhizic acid in preparation example 1
Qualitative assay measures this preparation example gained granular preparation sample glycyrrhizic acid remnants after high-temperature treatment and leads is 99.1%.With reference in preparation example 1
Melting is investigated method and measured this preparation example gained granular preparation sample speed of dissolving after high-temperature treatment is 106%.
Preparation example 4: preparation does not include the extract of volatile oil
Raw medicinal material forms:
Preparation method:
A (), by Rhizoma Chuanxiong, the Radix Angelicae Dahuricae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae, Radix Saposhnikoviae, the medicinal water extract of Herba Asari Six-element, i.e. boiling secondary, adds 6 times amount for the first time
Water, decocts 1.5 hours, and second time adds 7 times amount water, decocts 2 hours, and decocting liquid filters, and filtrate merges, and obtains aqueous extract；
B Herba Menthae, both Herba Schizonepetae are added 6 times amount water by (), vapor distillation extracts volatile oil 3 hours, obtains volatile oil and aqueous extract (filtration) two
Part；
C step (a) gained Aqueous extracts is merged by () with step (b) gained Aqueous extracts, add the maltodextrin of 5 weight portions, is concentrated into relative density and is
The extractum of 1.12-1.16 (80 DEG C), is spray-dried (intake air temperature 230 DEG C, air outlet temperature 110 DEG C), obtains extract powder；
D step (b) gained volatile oil and appropriate sucrose, dextrin (the two uses with weight ratio 1:0.2 ratio) are joined the leaching of step (c) gained by ()
In cream powder, making material always weigh 780 weight portions, prepare granule, every 7.8g granule is equivalent to 1.2g Ligusticum chuanxiong Hort, uses compound membrane bag subpackage, i.e.
, sample is designated as Ex4.The glycyrrhizic acid yield of this preparation example gained granular preparation sample is measured with reference to the glycyrrhizic acid yield algoscopy in preparation example 1
It is 98.1%.This preparation example gained granular preparation sample Radix Glycyrrhizae after high-temperature treatment is measured with reference to the glycyrrhizic acid stability determination method in preparation example 1
The remaining rate of acid is 98.6%.Investigate method with reference to the melting in preparation example 1 and measure this preparation example gained granular preparation sample after high-temperature treatment
Dissolving speed is 124%.
Preparation example 5
Raw medicinal material forms:
Preparation method:
A (), by Rhizoma Chuanxiong, the Radix Angelicae Dahuricae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae, Radix Saposhnikoviae, the medicinal water extract of Herba Asari Six-element, i.e. boiling secondary, adds 7 times amount for the first time
Water, decocts 1.5 hours, and second time adds 6 times amount water, decocts 1.5 hours, and decocting liquid filters, and filtrate merges, and obtains aqueous extract；
B Herba Menthae, both Herba Schizonepetae are added 6 times amount water by (), vapor distillation extracts volatile oil 2 hours, obtains volatile oil and aqueous extract (filtration) two
Part；
C step (a) gained Aqueous extracts is merged by () with step (b) gained Aqueous extracts, add the maltodextrin of 20 weight portions, be concentrated into relative density
For the extractum of 1.12-1.16 (80 DEG C), it is spray-dried (intake air temperature 230 DEG C, air outlet temperature 110 DEG C), obtains extract powder；
D step (b) gained volatile oil and appropriate sucrose, dextrin (the two uses with weight ratio 1:5 ratio) are joined the leaching of step (c) gained by ()
In cream powder, making material always weigh 600 weight portions, prepare granule, every 6g granule is equivalent to 1.2g Ligusticum chuanxiong Hort, uses compound membrane bag subpackage, i.e.
, sample is designated as Ex5.The glycyrrhizic acid yield of this preparation example gained granular preparation sample is measured with reference to the glycyrrhizic acid yield algoscopy in preparation example 1
It is 99.5%.This preparation example gained granular preparation sample Radix Glycyrrhizae after high-temperature treatment is measured with reference to the glycyrrhizic acid stability determination method in preparation example 1
The remaining rate of acid is 97.9%.Investigate method with reference to the melting in preparation example 1 and measure this preparation example gained granular preparation sample after high-temperature treatment
Dissolving speed is 91%.
Preparation example 6
Formula and preparation method with reference to example 1 to preparation example 5 prepared as above are carried out respectively, but except for the difference that, are not added with adjuvant lactose (or sugarcane in step (d)
Sugar) and dextrin, but pelletize after directly volatile oil being mixed with extract powder.Obtain 5 samples, be designated as respectively Ex61, Ex62, Ex63, Ex64,
Ex65.The glycyrrhizic acid yield measuring this preparation example gained granular preparation sample with reference to the glycyrrhizic acid yield algoscopy in preparation example 1 all exists
In the range of 97.4～99.2%.This preparation example gained granular preparation sample is measured through high-temperature treatment with reference to the glycyrrhizic acid stability determination method in preparation example 1
After glycyrrhizic acid remnants lead all in the range of 97.1～99.3%.Investigate method with reference to the melting in preparation example 1 and measure this preparation example gained granule system
Agent sample dissolves speed all in the range of 90～125% after high-temperature treatment.
The maltodextrin added during feeding intake by the whole samples obtained by calculating example 1 to preparation example 6 made above and final material
Weight, can be informed in the maltodextrin fed intake in preparation process increases in the final granular preparation of the present invention as adjuvant.I.e. Fructus Hordei Germinatus
Magma essence is a kind of pharmaceutic adjuvant added in the middle process stage.
Reference examples 1
With reference to formula and the preparation method of preparation example 1, use 0,1,2.5,5,7.5,15,20,25,30,50 or 100 the most respectively
The maltodextrin of weight portion, obtains 11 granular preparation samples.They maltodextrin consumptions (weight portion) and numbered list are as follows:
| Maltodextrin amount | 0 | 1 | 2.5 | 5 | 7.5 | 15 | 20 | 25 | 30 | 50 | 100 |
| Sample number into spectrum | D101 | D102 | D103 | D104 | D105 | D106 | D107 | D108 | D109 | D110 | D111 |
The glycyrrhizic acid yield of this reference examples gained each granular preparation sample, result display wheat is measured with reference to the glycyrrhizic acid yield algoscopy in preparation example 1
Bud magma essence consumption, and shows less than the glycyrrhizic acid yield of three samples (D101 to D103) equal to 2.5 weight portions in the range of 43～71%
Maltodextrin consumption the lowest glycyrrhizic acid yield is the lowest；And maltodextrin consumption is more than or equal to the glycyrrhizic acid yield of remaining sample of 5 weight portions
In the range of 96～99%.
This reference examples gained each granular preparation sample glycyrrhizic acid after high-temperature treatment is measured residual with reference to the glycyrrhizic acid stability determination method in preparation example 1
Remaining rate, result shows, maltodextrin consumption leads less than or equal to the glycyrrhizic acid remnants of three samples (D101 to D103) of 2.5 weight portions
In the range of 71.7～84.8%, and show that the least stability with glycyrrhizic acid content sign of maltodextrin consumption is the lowest；And maltodextrin consumption
Lead all in the range of 95.4～98.3% more than or equal to the glycyrrhizic acid remnants of remaining sample of 5 weight portions, have unexpectedly shown that maltodextrin is this
Conventional pharmaceutic adjuvant is favorably improved the chemical stability of glycyrrhizic acid.
Investigate method with reference to the melting in preparation example 1 to measure this reference examples gained each granular preparation sample and dissolve speed after high-temperature treatment, knot
Really maltodextrin consumption dissolves speed less than or equal to 8 samples of 25 weight portions and is respectively less than 133%, shows that they are respectively provided with good solute
Reason stability；And maltodextrin consumption more than or equal to 30 weight portions 3 samples dissolve speed all in the range of 195～343%, and Fructus Hordei Germinatus
It is the biggest that magma essence consumption dissolves the most greatly rate value, has unexpectedly shown that this conventional pharmaceutic adjuvant of maltodextrin can cause when adding excess
Deteriorating of granular preparation physical stability of the present invention.
Reference examples 2
With reference to formula and the preparation method of reference examples 1, except for the difference that change lactose therein into equivalent sucrose, obtain 11 granular preparation samples.They
Maltodextrin consumption (weight portion) and numbered list are as follows:
| Maltodextrin amount | 0 | 1 | 2.5 | 5 | 7.5 | 15 | 20 | 25 | 30 | 50 | 100 |
| Sample number into spectrum | D201 | D202 | D203 | D204 | D205 | D206 | D207 | D208 | D209 | D210 | D211 |
The glycyrrhizic acid yield of this reference examples gained each granular preparation sample, result display wheat is measured with reference to the glycyrrhizic acid yield algoscopy in preparation example 1
Bud magma essence consumption, and shows less than the glycyrrhizic acid yield of three samples (D201 to D203) equal to 2.5 weight portions in the range of 46～73%
Maltodextrin consumption the lowest glycyrrhizic acid yield is the lowest；And maltodextrin consumption is more than or equal to the glycyrrhizic acid yield of remaining sample of 5 weight portions
In the range of 95～99%.
This reference examples gained each granular preparation sample glycyrrhizic acid after high-temperature treatment is measured residual with reference to the glycyrrhizic acid stability determination method in preparation example 1
Remaining rate, result shows, maltodextrin consumption leads less than or equal to the glycyrrhizic acid remnants of three samples (D201 to D203) of 2.5 weight portions
In the range of 74.3～82.2%, and show that the least stability with glycyrrhizic acid content sign of maltodextrin consumption is the lowest；And maltodextrin consumption
Lead all in the range of 96.3～98.9% more than or equal to the glycyrrhizic acid remnants of remaining sample of 5 weight portions, have unexpectedly shown that maltodextrin is this
Conventional pharmaceutic adjuvant is favorably improved the chemical stability of glycyrrhizic acid.
Investigate method with reference to the melting in preparation example 1 to measure this reference examples gained each granular preparation sample and dissolve speed after high-temperature treatment, knot
Really maltodextrin consumption dissolves speed less than or equal to 8 samples of 25 weight portions and is respectively less than 142%, shows that they are respectively provided with good solute
Reason stability；And maltodextrin consumption more than or equal to 30 weight portions 3 samples dissolve speed all in the range of 207～3363%, and wheat
It is the biggest that bud magma essence consumption dissolves the most greatly rate value, has unexpectedly shown that this conventional pharmaceutic adjuvant of maltodextrin can draw when adding excess
Play deteriorating of granular preparation physical stability of the present invention.
Reference examples 3
With reference to formula and the preparation method of reference examples 1, in step (d), except for the difference that it is not added with adjuvant lactose and dextrin, but directly by volatile oil and extractum
Pelletize after powder mixing, obtain 11 granular preparation samples.They maltodextrin consumptions (weight portion) and numbered list are as follows:
| Maltodextrin amount | 0 | 1 | 2.5 | 5 | 7.5 | 15 | 20 | 25 | 30 | 50 | 100 |
| Sample number into spectrum | D301 | D302 | D303 | D304 | D305 | D306 | D307 | D308 | D309 | D310 | D311 |
The glycyrrhizic acid yield of this reference examples gained each granular preparation sample, result display wheat is measured with reference to the glycyrrhizic acid yield algoscopy in preparation example 1
Bud magma essence consumption, and shows less than the glycyrrhizic acid yield of three samples (D301 to D303) equal to 2.5 weight portions in the range of 46～69%
Maltodextrin consumption the lowest glycyrrhizic acid yield is the lowest；And maltodextrin consumption is more than or equal to the glycyrrhizic acid yield of remaining sample of 5 weight portions
In the range of 97～100%.
This reference examples gained each granular preparation sample glycyrrhizic acid after high-temperature treatment is measured residual with reference to the glycyrrhizic acid stability determination method in preparation example 1
Remaining rate, result shows, maltodextrin consumption leads less than or equal to the glycyrrhizic acid remnants of three samples (D301 to D303) of 2.5 weight portions
In the range of 73.5～85.3%, and show that the least stability with glycyrrhizic acid content sign of maltodextrin consumption is the lowest；And maltodextrin consumption
Lead all in the range of 96.6～98.8% more than or equal to the glycyrrhizic acid remnants of remaining sample of 5 weight portions, have unexpectedly shown that maltodextrin is this
Conventional pharmaceutic adjuvant is favorably improved the chemical stability of glycyrrhizic acid.
Investigate method with reference to the melting in preparation example 1 to measure this reference examples gained each granular preparation sample and dissolve speed after high-temperature treatment, knot
Really maltodextrin consumption dissolves speed less than or equal to 8 samples of 25 weight portions and is respectively less than 130%, shows that they are respectively provided with good solute
Reason stability；And maltodextrin consumption more than or equal to 30 weight portions 3 samples dissolve speed all in the range of 188～314%, and Fructus Hordei Germinatus
It is the biggest that magma essence consumption dissolves the most greatly rate value, has unexpectedly shown that this conventional pharmaceutic adjuvant of maltodextrin can cause when adding excess
Deteriorating of granular preparation physical stability of the present invention.
Reference examples 4
In the Chuan Xiong Tea granule national drug standards that reference standard number is WS3-B-0887-91-2011, the method under [preparation method] item prepares Rhizoma Chuanxiong tea
Adjust granule.In this preparation process, measure the Radix Glycyrrhizae of this reference examples gained granular preparation sample with reference to the glycyrrhizic acid yield algoscopy in preparation example 1
Acid yield is 65.4%.This reference examples gained granular preparation sample is measured after high-temperature treatment with reference to the glycyrrhizic acid stability determination method in preparation example 1
Glycyrrhizic acid remnants to lead be 91.2%.Investigate method with reference to the melting in preparation example 1 and measure this reference examples gained granular preparation sample at high temperature
The speed of dissolving postponed is 196%.
Reference examples 5
Prepare with reference to formula described in CN 102579576A (Chinese Patent Application No. 2,012 1,004 4712.4) description preparation example 8 and method and include waving
The extract (dry product) of hair oil, this dry extract is not added with other adjuvant and directly prepares 'Chuan Xiong Tea ', method particularly includes: (1) take Rhizoma Chuanxiong,
The Radix Angelicae Dahuricae, Rhizoma Et Radix Notopterygii, Herba Asari, Radix Saposhnikoviae, Radix Glycyrrhizae, boiling 2 times, use medical material 8 times amount decocting 1.5 hours for the first time, second time medical material 6
Times amount decocting 1 hour, decocting liquid filters, and medicinal liquid is standby；(2) Herba Menthae, Herba Schizonepetae extract volatile oil, standby；Its aqueous solution filters, filtrate and step
(1) gained medicinal liquid merges；(3) step (2) gained merging medicinal liquid use organic membrane SMN-130A2350054 is crossed film nanofiltration, filtration temperature 36 DEG C,
Filter pressure 17bar, nanofiltration concentrated solution relative density is 1.21 (36 DEG C) (after nanofiltration, cleaning NF membrane with abluent 1% sodium polyphosphate),
Abandoning dialysis solution, the concentrated solution obtained is spray-dried, and makes extract powder, step (2) gained volatile oil is sprayed to the extract powder that step (3) gained is dried
In, mix homogeneously, it is extract prepared by this reference examples, it is not added with other adjuvant and is directly prepared as granular preparation.
In above-mentioned preparation process, measure the glycyrrhizic acid of this reference examples gained granular preparation sample with reference to the glycyrrhizic acid yield algoscopy in preparation example 1
Yield is 69.4%.This reference examples gained granular preparation sample is measured after high-temperature treatment with reference to the glycyrrhizic acid stability determination method in preparation example 1
It is 90.2% that glycyrrhizic acid remnants lead.Result shows, although the method described in CN102579576A uses NF membrane, dialysis concentrates significantly to subtract
The chance of few material thermo-contact, but the most not there is the effect of the high glycyrrhizic acid response rate, point out maltodextrin of the present invention to improve glycyrrhizic acid and reclaim
The mechanism of rate is not simply to improve the mode of glycyrrhizic acid heat stability.It addition, it is right to measure this with reference to the melting investigation method in preparation example 1
Gained granular preparation sample speed of dissolving after high-temperature treatment is 226% as usual.
Reference examples 6
The formula of six samples of D103 to D108 of reference reference examples 1 of the present invention and preparation method, except for the difference that change into maltodextrin therein
Amount maltose (Maltose, anhydride, CAS registration number 69-79-4) or maltose alcohol (Maltitol, anhydride, CAS registration number 585-88-6),
Obtain 12 granular preparation samples.The Radix Glycyrrhizae of this reference examples gained each granular preparation sample is measured with reference to the glycyrrhizic acid yield algoscopy in preparation example 1
Acid yield, result shows that the glycyrrhizic acid yield of 12 samples in whole maltose and maltose alcohol amount ranges is all in the range of 46～73%.Table
As bright use and maltodextrins, adjuvant but can not realize the effect obtained such as the present invention.
Reference examples 7
Take commercially available Chuan Xiong Tea granule (traditional Chinese medicines quasi-word Z11020995, every bagged granules 7.8g, be calculated as 1.2g with Rhizoma Chuanxiong crude drug containing active component).Ginseng
Measure the granular preparation sample of this reference examples glycyrrhizic acid remnants after high-temperature treatment lead according to the glycyrrhizic acid stability determination method in preparation example 1 and be
90.6%。
C, the quality investigation of Chuan Xiong Tea granule
According to above, the method in " A, the quality investigation method of Chuan Xiong Tea granule ", investigates the granule of preparation example 1 to preparation example 6 gained of the present invention
Obtained by preparation and reference examples 1 to reference examples 3, there is the granular preparation D104 to D107 of feature of present invention, D204 to D207, D304
To D307, result shows that these samples all meet set quota requirement in " A, the quality investigation method of Chuan Xiong Tea granule ".
Claims (20)
1. a 'Chuan Xiong Tea ', the raw medicinal material preparing said preparation consists of:
Rhizoma Chuanxiong 120 weight portion, the Radix Angelicae Dahuricae 45 ~ 75 weight portion,
Rhizoma Et Radix Notopterygii 45 ~ 75 weight portion, Radix Glycyrrhizae 45 ~ 75 weight portion,
Radix Saposhnikoviae 33 ~ 56 weight portion, Herba Asari 22 ~ 38 weight portion,
Herba Menthae 180 ~ 300 weight portion, Herba Schizonepetae 90 ~ 150 weight portion；
Said preparation is to be prepared by the method for following steps:
A Rhizoma Chuanxiong, the Radix Angelicae Dahuricae, Rhizoma Et Radix Notopterygii, Radix Glycyrrhizae, Radix Saposhnikoviae, the medicinal water extraction of Herba Asari Six-element are obtained aqueous extract by ()；
B volatile oil that Herba Menthae, both Herba Schizonepetae are obtained by () with water vapour distillation and aqueous extract two parts；
C step (a) gained Aqueous extracts is merged by () with step (b) gained Aqueous extracts, add maltodextrin 2 ~ 25 weight portion, dense
Contract, be dried to obtain extract powder；
D step (b) gained volatile oil and optional pharmaceutic adjuvant are joined in step (c) gained extract powder by (), preparation
Grain, to obtain final product.
'Chuan Xiong Tea ' the most according to claim 1, the raw medicinal material preparing said preparation consists of:
Rhizoma Chuanxiong 120 weight portion, the Radix Angelicae Dahuricae 48 ~ 72 weight portion,
Rhizoma Et Radix Notopterygii 48 ~ 72 weight portion, Radix Glycyrrhizae 48 ~ 72 weight portion,
Radix Saposhnikoviae 36 ~ 54 weight portion, Herba Asari 24 ~ 36 weight portion,
Herba Menthae 192 ~ 288 weight portion, Herba Schizonepetae 96 ~ 144 weight portion.
'Chuan Xiong Tea ' the most according to claim 1, the raw medicinal material preparing said preparation consists of:
Rhizoma Chuanxiong 120 weight portion, the Radix Angelicae Dahuricae 54 ~ 66 weight portion,
Rhizoma Et Radix Notopterygii 54 ~ 66 weight portion, Radix Glycyrrhizae 54 ~ 66 weight portion,
Radix Saposhnikoviae 33 ~ 56 weight portion, Herba Asari 27 ~ 33 weight portion,
Herba Menthae 216 ~ 264 weight portion, Herba Schizonepetae 108 ~ 132 weight portion.
'Chuan Xiong Tea ' the most according to claim 1, the raw medicinal material preparing said preparation consists of:
Rhizoma Chuanxiong 120 weight portion, the Radix Angelicae Dahuricae 60 weight portion,
Rhizoma Et Radix Notopterygii 60 weight portion, Radix Glycyrrhizae 60 weight portion,
Radix Saposhnikoviae 45 weight portion, Herba Asari 30 weight portion,
Herba Menthae 240 weight portion, Herba Schizonepetae 120 weight portion.
'Chuan Xiong Tea ' the most according to claim 1, wherein in terms of the Ligusticum chuanxiong Hort of every 120 weight portions, maltodextrin
Amount is 5 ~ 20 weight portions.
'Chuan Xiong Tea ' the most according to claim 1, the described adjuvant of step (d) is selected from: sucrose, dextrin, lactose, starch, pre-
Gelling starch, microcrystalline Cellulose, and combinations thereof.
'Chuan Xiong Tea ' the most according to claim 6, wherein in terms of the Ligusticum chuanxiong Hort of 120 weight portions that often feed intake, described adjuvant
Amount be so that the final weight of obtained granule is 300 ~ 1000 weight portions.
'Chuan Xiong Tea ' the most according to claim 6, wherein in terms of the Ligusticum chuanxiong Hort of 120 weight portions that often feed intake, described adjuvant
Amount be so that the final weight of obtained granule is 350 ~ 900 weight portions.
'Chuan Xiong Tea ' the most according to claim 6, wherein in terms of the Ligusticum chuanxiong Hort of 120 weight portions that often feed intake, described adjuvant
Amount be so that the final weight of obtained granule is 375 ~ 800 weight portions.
'Chuan Xiong Tea ' the most according to claim 6, wherein said adjuvant is sucrose with both dextrin with 1:0.2 ~ 5 weight
The combination of ratio.
11. 'Chuan Xiong Tea 's according to claim 6, wherein said adjuvant is lactose with both dextrin with 1:0.2 ~ 5 weight
The combination of ratio.
12. 'Chuan Xiong Tea 's according to claim 6, wherein said adjuvant is lactose with both dextrin with 1:0.5 ~ 2 weight
The combination of ratio.
13. 'Chuan Xiong Tea 's according to claim 1, it is unit dose package preparation.
14. 'Chuan Xiong Tea 's according to claim 1, it is the unit dose package preparation that composite membrane is packed.
15. 'Chuan Xiong Tea 's according to claim 14, the granule comprised in its every bag is calculated as 1.0 ~ 1.5g with Ligusticum chuanxiong Hort.
16. 'Chuan Xiong Tea 's according to claim 14, the granule comprised in its every bag is calculated as 1.1 ~ 1.3g with Ligusticum chuanxiong Hort.
17. 'Chuan Xiong Tea 's according to claim 14, the granule comprised in its every bag with Ligusticum chuanxiong Hort be calculated as 1.15 ~
1.25g。
18. 'Chuan Xiong Tea 's according to claim 14, the granule comprised in its every bag is calculated as 1.2g with Ligusticum chuanxiong Hort.
19. 'Chuan Xiong Tea 's according to claim 1, it is the unit dose package preparation that composite membrane is packed, in every bag
The weight of grain thing is 2-10g.
20. 'Chuan Xiong Tea 's according to claim 19, the weight of the particulate matter in its every bag is 3-8g.
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| CN104940431A (en) * | 2015-06-23 | 2015-09-30 | 湖南安邦制药有限公司 | Ligusticum wallichii tea modulating agent |
| CN108478626A (en) * | 2016-06-01 | 2018-09-04 | 湖南安邦制药有限公司 | A kind of extraction process of volatile oil |
| CN106692288A (en) * | 2016-12-22 | 2017-05-24 | 广州肇基生物科技有限公司 | Compound tea with functions of clearing away internal heat, calming liver, nourishing blood and dispelling wind and preparation method of compound tea |
| CN110772605A (en) * | 2019-11-15 | 2020-02-11 | 王同庆 | Traditional Chinese medicine for cervical spondylosis and preparation method thereof |
| CN113552276B (en) * | 2021-07-06 | 2022-07-19 | 贵州健兴药业有限公司 | Detection method of ligusticum wallichii and tea blending dropping pill |
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| CN1739612A (en) * | 2005-09-08 | 2006-03-01 | 王衡新 | Wind dispelling and pain relieving Chinese medicine prepn and its prepn process and quality control method |
| CN101313936A (en) * | 2007-06-01 | 2008-12-03 | 北京亚东生物制药有限公司 | Medicament composition for dispelling wind and relieving pain, preparation method and quality control method thereof |
| CN102579576A (en) * | 2012-02-27 | 2012-07-18 | 贵州威门药业股份有限公司 | Preparation methods of Chuanxiongchatiao granule extracts and preparations thereof |
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| CN1739612A (en) * | 2005-09-08 | 2006-03-01 | 王衡新 | Wind dispelling and pain relieving Chinese medicine prepn and its prepn process and quality control method |
| CN101313936A (en) * | 2007-06-01 | 2008-12-03 | 北京亚东生物制药有限公司 | Medicament composition for dispelling wind and relieving pain, preparation method and quality control method thereof |
| CN102579576A (en) * | 2012-02-27 | 2012-07-18 | 贵州威门药业股份有限公司 | Preparation methods of Chuanxiongchatiao granule extracts and preparations thereof |
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