CN107854312A - A kind of preparation technology of Chinese medicine preparation - Google Patents
A kind of preparation technology of Chinese medicine preparation Download PDFInfo
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- CN107854312A CN107854312A CN201711009683.7A CN201711009683A CN107854312A CN 107854312 A CN107854312 A CN 107854312A CN 201711009683 A CN201711009683 A CN 201711009683A CN 107854312 A CN107854312 A CN 107854312A
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Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61J—CONTAINERS SPECIALLY ADAPTED FOR MEDICAL OR PHARMACEUTICAL PURPOSES; DEVICES OR METHODS SPECIALLY ADAPTED FOR BRINGING PHARMACEUTICAL PRODUCTS INTO PARTICULAR PHYSICAL OR ADMINISTERING FORMS; DEVICES FOR ADMINISTERING FOOD OR MEDICINES ORALLY; BABY COMFORTERS; DEVICES FOR RECEIVING SPITTLE
- A61J3/00—Devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
Abstract
The invention discloses a kind of preparation technology of Chinese medicine preparation, its step is：Choose through examining qualified high-quality pharmaceutical decocting piece, mixed in prescription ratio, after soaking 30 minutes by a certain percentage, heating is boiled, and keep boiling 10~60 minutes with small fire, sieving, impurity and macromolecular substances is removed by centrifugation in filtrate, the extract solution clarified, extract solution is concentrated by depressurizing low temperature, it is concentrated to certain relative density, concentrate is added into a certain proportion of auxiliary material or is not added with auxiliary material, mix, by being spray-dried rapid draing into powder, powder is prepared into granule, global quality control is carried out to the granule of acquisition, using standard decoction as according to the fingerprint control method for establishing feature, overall monitor is carried out to product quality.The clinic that the invention changes tcm prescription takes mode, has the advantages that steady quality, easy to carry, long shelf-life, has preferable clinical value and market popularization value.
Description
Technical field
The present invention relates to a kind of preparation technology of Chinese medicine preparation, and in particular to the industry of the classics recipe decoction such as Xiao Chaihu Tang
Change preparation technology.
Background technology
Chinese medicine turns into the primary armament that the traditional Chinese medical science treats disease for thousands of years, classics recipe is the traditional Chinese medical science as our national treasure
Clinical the most frequently used prescription, it is as good and quality-high and inexpensive in floated drum, security that it is imitated, deep to be liked by numerous traditional Chinese physicians and patient.From
Used till today since Shang dynasty Yi Yin initiative soup,《Soup passes through》、《The Treatise on Fevrile Diseases》、《Synopsis Golden Chamber》、《Qianjin Yao Fang》、《Boudoir is secret
Hide》Deng recorded in classical works it is substantial amounts of examined by clinical practice, side curative for effect, that there is obvious characteristic and advantage
Agent.This is the marrow and elite of TCM Culture, and constantly succession and development, makes for the medical treatment ＆ health of the Chinese nation for thousands of years
Great contribution.
Chinese patent medicine preparation generally existing alcohol precipitation, long-time high temperature drying etc. in production technology destroys the main thing of decoction at present
Often larger difference be present with traditional decoction decoction, be embodied in and face in the processing step on matter basis, the Quality of Chinese Traditional Proprietary Medicine of listing
Often curative effect is had a greatly reduced quality on bed, and here it is patent medicine defect sex chromosome mosaicism.This few use that is clinician's preference using slice decoction
One of the main reason for Chinese patent drug.
The key problem of Chinese medicine classics recipe industrialization is that modern production technique exists with the product that traditional handicraft is obtained
On material base whether being consistent property.Alcohol after the water extraction or alcohol extracting, concentration that are generally used in the big production of Chinese patent drug at present
Heavy, high temperature drying, crush, the technological process such as shaping, this conventional production technology have that equipment is simple, cost is low and technology into
The advantage such as ripe, it is well received in actual industrialization.Regrettably at present there are two open defects in this production technology, when
There may be some chemical reactions for alcohol precipitation process；Second, high-temperature drying procedures can destroy some thermally labile components, two above
Subject matter can make the Chinese medicine preparation of the acquisition material base in large-scale production process change, and cause the difference on clinical efficacy
It is different.Therefore, current Chinese patent drug extraction process is continued to use classics recipe is carried out to there may be patent medicine defective in industrialization process,
Uniformity of the big production with the product of traditional handicraft acquisition in inherent quality can not be ensured.It will be apparent that traditional decocting is boiled
Decoction technology can not meet the requirement produced greatly.
Therefore, to solve problem above, it is necessary to respect traditional medication custom and decocting process, extracted with sophisticated equipment
The preparation of acquisition should keep with former technique obtained by uniformity of the decoction in chemical composition, novel formulation should also have it is easy to carry,
The advantages that stability is good and convenient to take.
The content of the invention
The purpose of the present invention is to be directed to above-mentioned the deficiencies in the prior art, there is provided a kind of preparation technology of Chinese medicine preparation, is passed through
Traditional decoction technique is groped, determines the design parameters such as water consumption, decocting time, filtering and the concentration of lab scale craft, will be small
Examination technological parameter is transformed into big production, is reconciled the decocting process (such as temperature, water consumption, decocting time) in big production, is removed
The technological parameters such as general labourer's skill (centrifugation rate, time etc.), drying condition (solution density, intake air temperature, air outlet temperature), profit
The chemical constituent uniformity in large-scale production process before and after each step is monitored with HPLC multicomponents fingerprint atlas detection method, it is ensured that
The Chinese medicine new formulation that modern extraction process obtains and the decoction material composition of traditional decoction extraction acquisition are basically identical.
The preparation technology flow and theoretical foundation of Chinese medicine preparation provided by the invention, by taking Xiao Chaihu Tang solid pharmaceutical preparation as an example,
Realized using following scheme：
(1) conversion of prescription and recipe quantity
Classics recipe modern production must solve three problems：1) flavour of a drug name problem, such as ginseng in Xiao Chaihu Tang side
Whether it is modern ginseng, or Radix Codonopsis《Chinese Pharmacopoeia》Middle Xiao Chai Hu granules have selected Radix Codonopsis to substitute ginseng.Scripture of the present invention
Access and the suggestion of clinical classical prescription doctor are offered, keeps the ginseng in former side with modern ginseng；2) problem, such as Xiao Chaihu Tang side are processed
In " tuber of pinellia (washing) ", according to the medication of modern clinic classical prescription doctor custom and actual conditions of tuber of pinellia processed product at present, the present invention
It is the flavour of a drug that feed intake to select pinellia；3) recipe quantity metering conversion, because the measurement unit of Han dynasty is different from the modern times, therefore will basis
The measurement unit of Han dynasty and the measurement unit in modern times are changed, and such as present invention is equal to the 15.6g in modern times by Han dynasty one or two and entered
Row conversion, a pipeful of of Han dynasty is decaliter, and one is upgraded to modern 200ml.
(2) water boiling and extraction process optimization
According to the relevant requirement of country, production technology and the traditional handicraft of classics recipe should be basically identical, therefore the present invention
The determination of the parameter such as middle Extraction solvent and dosage, extraction time, it is compared with traditional technique (lab scale craft)
On the basis of determine.As Xiao Chaihu Tang exists《The Treatise on Fevrile Diseases》Described in preparation method and taking dose it is as follows：
With a pipeful of two liters of water, boil and take six liters, go dregs, then take three liters, warmly take one liter, taking medicine three times daily.
The a pipeful of of Han dynasty is decaliter, and one is upgraded to modern 200ml.It is therefore the decocting of we boils dosage as 12 liters, i.e., present
2400ml.And it is 407g to put into dose, that is, the medicinal material amount of we and water consumption are about 1：6.Decocting time is according to decoction liquor
Change depending on, decoct 2400ml decoctions to 1200ml decoctions time be lab scale decocting time；Decoction after filtering is concentrated to
Half, i.e. lab scale soup.
After the dosage and decocting time of water determine, it is transferred to big production and starts to test.Because big production is closed space,
Therefore extraction time can not be judged with the reduction of extraction liquid measure, therefore big production extraction time is determined according to the lab scale time；Lab scale
The rate of charge of extract solution is consistent with big production；Extracting temperature is micro-boiling.On decocting number problem, according to《Medical institutions
Traditional Chinese medicine decocting room management regulation》Typically to decoct twice, the big PRODUCTION TRAITS situation of the invention according to different cultivars, it is determined that decocting
Number.
(3) impurity removal process is centrifuged
It is general in big production technology at present that the impurity such as polysaccharide, fiber in water extraction decoction is just removed using the method for alcohol precipitation, this
Kind of technique has changed the extraction process of traditional decoction, and the technique of alcohol precipitation also has that cost is high, operational risk is big, removal of impurities is not thorough
Bottom, there may be the problems such as chemical reaction.The present invention is low, pollution-free using the centrifuging process rapid impurity removal and cost of modernization,
More importantly go the removal of impurity relatively thoroughly and main component do not change.
The present invention, such as disk plate centrifuge or tube centrifuge, passes through ratio by being relatively applicable the supercentrifuge produced greatly
The parameters such as more different decoction density, centrifugation rate, decoction treating capacity, decoction after being centrifuged, using multi-analyte immunoassay index
Mass ratio pair is carried out to decoction before and after centrifugation with the control measure such as medicinal extract yield, it is determined that optimal decoction density, centrifugation rate and
The centrifuging process parameter such as decoction treating capacity.Ensure that centrifugal process removal of impurities is substantially thorough, and effective material base does not change.
(4) optimization of drying process
Typically medicinal extract is dried under conditions of high temperature using baking oven in big production at present, traditional Chinese medicine extraction is obtained by crushing
Thing powder.This kind of drying mode cost is relatively low, and widely used by the big production of Chinese medicine, its shortcoming is that high temperature can make in Chinese medical extract
Unstable chemical composition is decomposed, volatilization or distillation and produce loss, it is also possible to make in Chinese medical extract chemical composition mutually it
Between certain chemical reaction occurs, this changes medicinal material base to a certain extent.
The present invention uses spray drying technology, by the clarification decoction after centrifugation after vacuum and low temperature is concentrated to finite concentration,
Drying is completed by spray drying tower moment, this drying process typically completed drying in several seconds inner liquid medicines, due to heated
The material base of time shorter survivable decoction.The main temperature for including decoction of technological parameter screening and optimization of spray drying
With the parameter such as concentration, supplementary product kind and dosage, hydrojet speed, intake air temperature, air outlet temperature.Drying process in the present invention
Carry out under conditions of total quality monitoring, ensure the science and reasonability of drying process.
(5) granulating process optimizes
Traditional granulation technique, such as wet granulation or dry granulation, often with efficiency is low, complex operation, granulate quality
Poor (melting, mobility and stability are bad), the problems such as polluting easily is produced to environment.The present invention according to specific kind,
Suitable binder is selected to carry out granulation research, by (such as feeding temperature, intake air temperature, going out to boiling granulating technological parameter
Draught temperature, feed liquid treating capacity etc.) screening and optimization, obtain optimal parameter with ensure gained granule product granularity,
Moisture, melting etc. meet the requirement of national standard.Screening and optimization about grain made parameter are in the bar of total quality monitoring
Part is carried out, and ensures that pelletization does not influence the material base of product.
(6) granule is packed
In the environment of clean area, granulation products obtained therefrom is packed, according to the yield and use of each kind granule
Method dosage, it is determined that final packing specification.The index such as content uniformity, microbial limit to packing product is examined on request
Test, as a result should meet national Specification.
(7) stability study
Stability study is based on the system research and understanding to preparation and its production technology, passes through design experiment acquisition
The rule that the quality of granula changes over time under the influence of various environmental factors (such as temperature, humidity, light irradiation), and according to
This provides supportive information for the determination of granule technique, packaging, holding conditions and the term of validity.Refer to according to national stability Journal of Sex Research
Principle is led, big production sample quality is investigated, determines that process above parameter, packaging and storage condition etc. influence finished product preparation
Principal element.
Discussed based on above-mentioned scheme, the preparation technology of Chinese medicine preparation provided by the invention gives by the following technical programs
Realize：
(1) choose and qualified high-quality pharmaceutical decocting piece is examined by national standard, it is stand-by after being mixed in prescription ratio；
(2) medicine materical crude slice of step (1) is put into normal pressure extraction vessel, soaked by a certain percentage 30 minutes；
(3) after stirring, heating is boiled, and keeps micro-boiling 10~60 minutes with small fire；
(4) after micro-boiling extraction terminates, with 100~300 mesh screens, impurity and macromolecular complex is removed by centrifugation in filtrate
Matter, the extract solution clarified；
(5) extract solution of step (4) is concentrated by depressurizing low temperature, is concentrated to certain relative density, it is standby；
(6) concentrate for obtaining step (5) adds a certain proportion of auxiliary material or is not added with auxiliary material, mixes, dry by spraying
Dry rapid draing is into powder；
(7) powder for obtaining step (6), granule is prepared into by wet granulation, dry granulation or boiling granulating；
(8) global quality control is carried out to the granule of acquisition, using standard decoction as according to the finger-print for establishing feature
Control method, overall monitor is carried out to product quality.
Preferably, the medicinal material in the step (1) is required to qualified by national standard inspection, main to choose from genuine
Tcm and herbal slice in the high-quality tcm and herbal slice in producing region, including the classics recipe such as Xiao Chaihu Tang, Gegen Decoction, Xiao Chengqi Tang.
Preferably, prescription ratio derives from each taste survival dose in classics recipe in the step (1), by certain conversion factor
The modern measurement unit being converted to, as 1 liang of Han dynasty based on present standard unit 15.6g；1 liter of Han dynasty presses present standard unit
200ml meters etc..
Preferably, the water addition ratio example in the step (2) is 5~15 times of medicinal material weight.
Preferably, the micro-boiling time in the step (3) should be with the traditional decoction time consistency of classics recipe, and it decocts effect
Fruit is investigated according to the finger-print established.
Preferably, the high speed centrifugation in the step (4) is that disk centrifuges or tubular type centrifugation, wherein disk centrifugal rotational speed are
6000~12000 revs/min；Tubular type centrifugal rotational speed is 8000~30000 revs/min.
Preferably, the relative density of concentrate is 1.00~1.30 in the step (5).
Preferably, the auxiliary material in the step (6) is soluble starch, maltodextrin, the one or more of sucrose.
Preferably, the intake air temperature of spray drying is 150~200 DEG C in the step (6), air outlet temperature 60~90
DEG C, feed liquid 10~200kg/h for the treatment of capacity, wherein pneumatic spray drying throughput are 0.3~3.5m3/min；Atomizer
Dry 8000~35000 revs/min of centrifugation rate, a diameter of 50~350mm of spray disk.
Preferably, boiling granulating feeding temperature is 15~50 DEG C in the step (7), and intake air temperature is 50~150 DEG C,
30~80 DEG C of air outlet temperature, 10~100kg/h of feed liquid treating capacity.
Preferably, the standard decoction in the step (8), refer to the decocting method with traditional decoction to separate sources medicinal material
The more parts of formulas that medicine materical crude slice is made into decoct extraction, the representative decoction obtained after being compared to gained soup respectively.
Preferably, in the step (8) finger-print need testing solution preparation：Take this product appropriate, to certain volume
In volumetric flask, with water dissolving and constant volume, shake up, filter, take subsequent filtrate, produce need testing solution.
Preferably, the detection method of finger-print chromatogram is high performance liquid chromatography in the step (8).
Preferably, finger-print requires sample finger-print compared with reference fingerprint in the step (8), similar
Degree is more than 0.90.
Compared with traditional handicraft, the present invention has advantages below：
1st, decocting boils technological parameter and boils technological parameter from traditional water decoction and have equivalent extraction effect；
2nd, concentrating and impurity removing process removes impurity using physics mode under cryogenic, will not cause and be thermally decomposed, be chemical
The change of the material bases such as composition transfer；
3rd, drying process uses wink-dry technology, and material composition will not be made because of high temperature and unstable；
4th, granulation technique is quick and shaping is preferable.
5th, after the completion of standard decoction preparation, the global quality control pattern using standard decoction as reference is established, using referring to
Overall chemical compositions composition, the multicomponent Con trolling index of foundation is used in line graphical spectrum technology overall monitor standard decoction
The stability study of product is to ensure the marketization of patent medicine.
Brief description of the drawings
Fig. 1 is the gained chromatogram of system of selection one；
Fig. 2 is the gained chromatogram of system of selection two；
Fig. 3 is chromatogram obtained by system of selection two (after modification)；
Fig. 4 is the gained chromatogram of system of selection three；
Fig. 5 is chromatogram obtained by system of selection three (modification)；
Fig. 6 is the gained chromatogram of system of selection four；
Fig. 7 is Xiao Chaihu Tang reference fingerprint；
Fig. 8 is each medicinal material chromatogram in prescription；
Fig. 9 is Xiao Chaihu Tang solid pharmaceutical preparation production link quality control chart；
Figure 10 is that different manufacturers Xiao Chaihu Tang solid pharmaceutical preparation finger-print compares figure.
Embodiment
With reference to embodiment, technical scheme is further illustrated, but the embodiment is merely to illustrate this hair
The bright rather than limitation present invention.
Embodiment 1：The preparation of Xiao Chaihu Tang particle
Xiao Chaihu Tang is from Han dynasty Zhang Zhongjing《The Treatise on Fevrile Diseases》, original side is described as：
Half jin of radix bupleuri, three liang of radix scutellariae, three liang of ginseng, the tuber of pinellia half liter (washing), three liang of (processing) gingers of radix glycyrrhizae three liang (cutting), jujube
12 pieces (thumbs)；
Suggestion of the invention through Literature Consult and clinical classical prescription doctor, keeps the ginseng in former side with modern ginseng；Selection
Pinellia is the flavour of a drug that feed intake；The 15.6g that the present invention is equal to the modern times by Han dynasty one or two is converted, half liter of the tuber of pinellia i.e. 200ml dresses
The tuber of pinellia weight of amount, 12 pieces of selection common 12, jujubes in Henan of jujube, which are weighed, to be produced.Therefore the Xiao Chaihu Tang prescription of the present invention
And recipe quantity is：
Radix bupleuri 125g, radix scutellariae 47g, ginseng 47g, pinellia 47g, honey-fried licorice root 47g, ginger 47g, jujube 47g.
Scale up test recipe quantity is converted in proportion：
Bupleurum Chinese 6.6kg, radix scutellariae 2.5kg, ginseng 2.5kg, pinellia 2.5kg, honey-fried licorice root 2.5kg, ginger (section)
2.5kg, jujube 2.5kg.
Above medicinal material is put into extractor, adds 150L water, stirring, after soaking 30min, heating is boiled, and keeps boiling
After rising 40min, stop heating.
Above extract solution is filtered with the screen cloth of 150 mesh, filtrate decompression (≤0.08MPa) low temperature (≤65 DEG C) is dense
Contracting, it is 1.02g/ml to be concentrated into relative density, stops heating concentration (sampling detection 1).
After above decoction is let cool, with (8000 revs/min) centrifugations of disk plate centrifuge, extract solution (sampling detection 2) must be clarified.
Above decoction is spray-dried, by 50% containing amount of solid plus auxiliary material maltodextrin, spray drying parameters are：
170 DEG C of intake air temperature, 65 DEG C of air outlet temperature, enter medicine speed 10kg/h, 8000 revs/min of centrifugation rate, the drying of acquisition
Powder, standby (sampling detection 3).
By above powder, pelletized with fluid bed granulator, feeding temperature is 40 DEG C, and intake air temperature is 110 DEG C, air outlet temperature
60 DEG C of degree, feed liquid treating capacity 15kg/h.Granule after granulation is Xiao Chaihu Tang particle (sampling detection 4).
Embodiment 2：The foundation of Xiao Chai Hu granules finger-print
1) preparation of Chinese medicine standard decoction
The representational Xiao Chaihu Tang prescription medicine materical crude slice of more than 10 batches is commercially bought, every batch of recipe quantity is：Radix bupleuri 125g,
Radix scutellariae 47g, ginseng 47g, pinellia 47g, honey-fried licorice root 47g, ginger 47g, jujube 47g.Above medicinal material is put into marmite, added
2400ml water (1：6), stir, soak 30min after, heating is boiled, and keep seethe with excitement 40min after, stop heating.By well-done medicine
Liquid is filtered with the screen cloth of 150 mesh, and filtrate is continued heating and boiled, and is concentrated into 600ml decoctions, is stopped heating, is produced 10 batches small
Bupleurum root decoction standard decoction.
2) foundation of finger-print
Selection prepared by need testing solution
The standard decoction of this product is taken, is that (1ml contains medicinal material for the need testing solution of standard decoction with 0.45 μm of membrane filtration
0.67g)；Concentrate, intermediate, powder in production process are respectively settled to 1ml 0.67g containing medicinal material solution with water, use
0.45 μm of membrane filtration produces the need testing solution of above sample.
The selection of chromatographic condition
Method one：Phenomenon C18 250mm × 4.6mm posts, column temperature are room temperature, flow velocity 1ml/min, detect ripple
It is long：210th, 230,254,270nm, mobile phase and degree elution requirement are as shown in the table.
| Time (min) | Acetonitrile (%) | 0.1% phosphoric acid (%) |
| 0 | 10 | 90 |
| 70 | 80 | 20 |
| 80 | 80 | 20 |
| 85 | 10 | 90 |
| 100 | 10 | 90 |
Obtained chromatogram is shown in accompanying drawing 1.
As a result：Chromatographic peak is concentrated mainly on first half, and separating degree is bad, and the Chromatographic information under 210nm is relatively abundant.
Method two：Phenomenon C18 250mm × 4.6mm posts, column temperature are room temperature, flow velocity 1ml/min, detect ripple
It is long：210th, 230,254,270nm, mobile phase and degree elution requirement are as shown in the table.
| Time (min) | Acetonitrile (%) | 0.1% phosphoric acid (%) |
| 0 | 5 | 95 |
| 90 | 95 | 5 |
| 95 | 95 | 5 |
| 100 | 5 | 95 |
| 110 | 5 | 95 |
Obtained chromatogram is shown in accompanying drawing 2.
As a result：Chromatographic peak is concentrated mainly on first half, basic after 50min not have a peak, and the Chromatographic information under 210nm is richer
It is rich.
Method two (after modification)：Phenomenon C18 250mm × 4.6mm posts, column temperature are room temperature, flow velocity 1ml/
Min, Detection wavelength：210th, 230,254,270nm, mobile phase and degree elution requirement are as shown in the table.
| Time (min) | Acetonitrile (%) | 0.1% phosphoric acid (%) |
| 0 | 5 | 95 |
| 60 | 55 | 45 |
| 65 | 95 | 5 |
| 70 | 95 | 5 |
| 75 | 5 | 95 |
| 80 | 5 | 95 |
Obtained chromatogram is shown in accompanying drawing 3.
As a result：Chromatographic peak distribution is average, except a small number of peak separating degrees are not good enough, disclosure satisfy that requirement substantially.Under 210nm
Chromatographic information it is relatively abundant.
Method three：Agilent C18 150mm × 4.6mm posts, column temperature are room temperature, flow velocity 1ml/min, Detection wavelength：
210th, 280,340nm, mobile phase and degree elution requirement are as shown in the table.
| Time (min) | Acetonitrile (%) | 0.1% phosphoric acid (%) |
| 0 | 2 | 98 |
| 90 | 92 | 8 |
| 92 | 2 | 98 |
| 105 | 2 | 98 |
Obtained chromatogram is shown in accompanying drawing 4.
As a result：Chromatographic information is less, basic after 44min have a chromatographic peak, and the Chromatographic information under 210nm relatively enriches.
Method three (after modification)：Agilent C18 150mm × 4.6mm posts, column temperature are room temperature, flow velocity 1ml/min, are examined
Survey wavelength：210th, 280,340nm, mobile phase and degree elution requirement are as shown in the table.
| Time (min) | Acetonitrile (%) | 0.1% phosphoric acid (%) |
| 0 | 2 | 98 |
| 60 | 47 | 53 |
| 62 | 90 | 10 |
| 65 | 90 | 10 |
| 67 | 2 | 98 |
| 80 | 2 | 98 |
Obtained chromatogram is shown in accompanying drawing 5.
As a result：Chromatographic information is less, and peak separating degree is relatively good.
Method four：Agilent C18 150mm × 4.6mm posts, column temperature are room temperature, flow velocity 1ml/min, Detection wavelength：
210th, 280nm, mobile phase and degree elution requirement are as shown in the table.
| Time (min) | Acetonitrile (%) | 0.1% phosphoric acid (%) |
| 0 | 15 | 85 |
| 20 | 25 | 75 |
| 35 | 30 | 70 |
| 40 | 40 | 60 |
| 50 | 40 | 60 |
| 60 | 15 | 85 |
| 70 | 15 | 85 |
Obtained chromatogram is shown in accompanying drawing 6.
As a result：Chromatographic information is less, but chromatographic peak separation is fine, and peak shape is preferable.
Fingerprint spectrum method determines
By above-mentioned experiment, temporarily confirm that fingerprint spectrum method is method two (after modification), i.e.,：Phenomenon C18
250mm × 4.6mm posts, column temperature are room temperature, flow velocity 1ml/min, Detection wavelength：210nm, mobile phase and degree elution requirement are as follows
Shown in table.
| Time (min) | Acetonitrile (%) | 0.1% phosphoric acid (%) |
| 0 | 5 | 95 |
| 60 | 55 | 45 |
| 65 | 95 | 5 |
| 70 | 95 | 5 |
| 75 | 5 | 95 |
| 80 | 5 | 95 |
The foundation of finger-print
10 batch Xiao Chaihu Tang standard decoctions are taken, carry out high performance liquid chromatography detection, chromatographic condition is：C18 chromatographic columns
(250mm × 4.6mm, 5 μm), column temperature are room temperature, flow velocity 1ml/min, Detection wavelength 210nm, mobile phase and degree elution bar
Part is as shown in the table.
| Time (min) | Acetonitrile (%) | 0.1% phosphoric acid (%) |
| 0 | 5 | 95 |
| 60 | 45 | 55 |
| 65 | 95 | 5 |
| 70 | 5 | 95 |
| 80 | 5 | 95 |
Obtained collection of illustrative plates is analyzed by similarity evaluation, obtains Xiao Chaihu Tang standard
Characteristic fingerprint pattern, see accompanying drawing 7, in figure mark for：
Radix bupleuri：1、2、3、4、5、6
Radix scutellariae：1st, 6,8,9,12,13,14,17 (scutellosides), 20,21,22,23
Ginseng：1、4、5、6、15
Pinellia：1
Honey-fried licorice root：1、5、7、10、11、16、24
Ginger：1、25
Jujube：1、2、3、4
3) in prescription ingredients finger print information
Ingredients medicine materical crude slice in prescription is taken into 100g respectively, according to six times of amounts (v/w) of water are added, stirring, soaks 30min,
Heating is boiled, and keeps boiling 40min, filtering, and filtrate is continued the decocting method extraction that heating is concentrated into original liquid a quarter, carried
Take liquid to be analyzed respectively according to the fingerprint spectrum method after confirmation, find out feature of the ingredients inside patent medicine finger-print
Information.The characteristic spectrum drawn is as shown in Figure 8.
It can be seen from accompanying drawing 8 inside the finger-print of Xiao Chaihu Tang, the information ratio that radix scutellariae medicinal materials and licorice medicinal materials occupy
More, the composition that other medicinal materials can detect is less.
Embodiment 3：Xiao Chai Hu granules preparation process global quality control
According to Xiao Chaihu Tang fingerprint spectrum method, to (sampling detection 1 in embodiment 1) after being concentrated in product preparation process,
After centrifugation (sampling detection 2 in embodiment 1), after drying (sampling detection 3 in embodiment 1), (inspection is sampled in embodiment 1 after granulation
Survey the sample 4) obtained and carry out efficient liquid phase chromatographic analysis, obtained chromatogram is shown in accompanying drawing 9.With Xiao Chaihu Tang reference fingerprint
Similarity analysis is carried out, similarity is more than 0.90.Illustrate that each production link can guarantee that the inherent quality base of Xiao Chaihu Tang
This does not change, and the Xiao Chaihu Tang solid pharmaceutical preparation of preparation does not change the material base of decoction substantially.
Embodiment 4：With the comparison of in the market existing procucts
The minor decoction of Bupleurum formulation of five different manufacturers is commercially bought, according to the preparation method of finger-print sample, system
Available test product simultaneously carries out efficient liquid phase chromatographic analysis, and obtained chromatogram is as shown in Figure 10.Fingerprint image is compareed with Xiao Chaihu Tang
Spectrum carries out similarity analysis, the phase of minor decoction of Bupleurum formulation and Xiao Chaihu Tang reference fingerprint prepared by five producers and the present invention
It is respectively 0.9368,0.9281,0.9403,0.9312,0.9205,0.9636 like degree, it is seen that pass through the production technology of the present invention
The Xiao Chaihu Tang solid pharmaceutical preparation of preparation and the similarity highest of Xiao Chaihu Tang reference fingerprint, and the content of some compositions is it
Middle highest.Illustrate the material base of Xiao Chaihu Tang solid pharmaceutical preparation and Xiao Chaihu Tang traditional decoction prepared by the technique of the present invention
It is basically identical, and it is better than the existing preparation of in the market.
Present invention is mainly used in traditional classics recipe industrialization process, on tcm clinical practice using it is curative for effect, take
A kind of new ways and means is provided with convenient and convenient to take new medicine preparation.The present invention has initiated a kind of classics recipe
Patent medicine pattern, this pattern can make the quick industrialization of traditional classical recipe, the marketization.The maximum advantage of this pattern
It is the material base for not changing decoction during industrialization substantially, ensure that the maximization of decoction clinical efficacy.
Claims (10)
- A kind of 1. preparation technology of Chinese medicine preparation, it is characterised in that：Comprise the following steps：(1) choose and qualified high-quality pharmaceutical decocting piece is examined by national standard, after being mixed in prescription ratio, stand-by, medicinal material mainly selects In fetching in the high-quality tcm and herbal slice for coming from Genuine producing area, including the classics recipe such as Xiao Chaihu Tang, Gegen Decoction, Xiao Chengqi Tang Pharmaceutical decocting piece；(2) medicine materical crude slice of step (1) is put into normal pressure extraction vessel, soaked by a certain percentage 30 minutes, water addition ratio example is 5~15 times of medicinal material weight；(3) after stirring, heating is boiled, and keeps micro-boiling 10~60 minutes with small fire；(4) after micro-boiling extraction terminates, with 100~300 mesh screens, impurity and macromolecular substances is removed by centrifugation in filtrate, obtains To the extract solution of clarification；(5) extract solution of step (4) is concentrated by depressurizing low temperature, is concentrated to certain relative density, it is standby；(6) concentrate for obtaining step (5) adds a certain proportion of auxiliary material or is not added with auxiliary material, mixes, fast by being spray-dried Speed is dried to powder, and auxiliary material is the one or more in soluble starch, maltodextrin, sucrose etc.；(7) powder for obtaining step (6), granule is prepared into by wet granulation, dry granulation or boiling granulating；(8) global quality control is carried out to the granule of acquisition, controlled using standard decoction as according to the finger-print for establishing feature Method, overall monitor, wherein standard decoction are carried out to product quality, refer to the decocting method with traditional decoction to separate sources medicine The more parts of formulas that material medicine materical crude slice is made into decoct extraction, the representative decoction obtained after being compared to gained soup respectively.
- 2. the preparation technology of Chinese medicine preparation according to claim 1, it is characterised in that：Prescription ratio in the step (1) Each taste survival dose in classics recipe, the modern measurement unit being converted to by certain conversion factor, press such as 1 liang of Han dynasty 15.6g is counted；1 liter of Han dynasty is based on 200ml etc..
- 3. the preparation technology of Chinese medicine preparation according to claim 1, it is characterised in that：During micro-boiling in the step (3) Between should be with the traditional decoction time consistency of classics recipe, it decocts effect and investigated according to the finger-print established.
- 4. the preparation technology of Chinese medicine preparation according to claim 1, it is characterised in that：High speed in the step (4) from The heart is that disk centrifuges or tubular type centrifuges, and wherein disk centrifugal rotational speed is 6000~12000 revs/min；Tubular type centrifugal rotational speed is 8000~30000 revs/min.
- 5. the preparation technology of Chinese medicine preparation according to claim 1, it is characterised in that：Concentrate in the step (5) Relative density is 1.00~1.30.
- 6. the preparation technology of Chinese medicine preparation according to claim 1, it is characterised in that：It is spray-dried in the step (6) Intake air temperature be 150~200 DEG C, 60~90 DEG C of air outlet temperature, feed liquid 10~200kg/h for the treatment of capacity, wherein air-flowing type Spray drying throughput is 0.3~3.5m3/min；Atomizer dries 8000~35000 revs/min of centrifugation rate, spraying A diameter of 50~the 350mm of disk.
- 7. the preparation technology of Chinese medicine preparation according to claim 1, it is characterised in that：Boiling granulating in the step (7) Feeding temperature is 15~50 DEG C, and intake air temperature is 50~150 DEG C, 30~80 DEG C of air outlet temperature, feed liquid treating capacity 10~ 100kg/h。
- 8. the preparation technology of Chinese medicine preparation according to claim 1, it is characterised in that：Finger-print in the step (8) The preparation method of need testing solution is：Take this product in right amount into the volumetric flask of certain volume, with water dissolving and constant volume, shake up, filter Cross, take subsequent filtrate, produce need testing solution.
- 9. the preparation technology of Chinese medicine preparation according to claim 1, it is characterised in that：Finger-print in the step (8) The detection method of chromatogram is high performance liquid chromatography.
- 10. the preparation technology of Chinese medicine preparation according to claim 1, it is characterised in that：Finger-print in the step (8) It is required that sample finger-print, compared with reference fingerprint, similarity is more than 0.90.
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