CN108236626A - A kind of preparation process of prepared fleece flower root Ultramicro-powder medicine materical crude slice - Google Patents
A kind of preparation process of prepared fleece flower root Ultramicro-powder medicine materical crude slice Download PDFInfo
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- CN108236626A CN108236626A CN201711201348.7A CN201711201348A CN108236626A CN 108236626 A CN108236626 A CN 108236626A CN 201711201348 A CN201711201348 A CN 201711201348A CN 108236626 A CN108236626 A CN 108236626A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/70—Polygonaceae (Buckwheat family), e.g. spineflower or dock
- A61K36/704—Polygonum, e.g. knotweed
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- 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
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/17—Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting
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Abstract
The invention discloses a kind of preparation process of prepared fleece flower root Ultramicro-powder medicine materical crude slice, decocting its active ingredient in the form of conventional medicine materical crude slice to solve the problems, such as prepared fleece flower root cannot be fully dissolved out.Include the following steps：Feedstock processing：3h is dried to prepared fleece flower root tradition medicine materical crude slice at 60 DEG C with heated-air circulation oven；Coarse crushing：Prepared fleece flower root medicine materical crude slice is crushed with Universalpulverizer, No. two sieves is crossed, obtains coarse powder；Screening：Coarse powder with pharmacopeia is sieved and carries out rough segmentation, No. five sieves is crossed and obtains fine powder, grain size is 180 μm 20 μm；Ultramicro grinding：Fine powder is thrown in WZJ6 Baily micronizers, fine powder accounts for the 2/3 of magazine, and 5 DEG C of crushing 25min, average grain diameter is 30 μm.Ultramicro-powder particle diameter distribution prepared by the present invention is more uniform, and cell-wall breaking ratio is high, and chemical composition does not change, and the more traditional medicine materical crude slice of dissolution rate of active ingredient dissociated anthraquinone significantly improves, so as to improve the bioavilability of medicinal material.
Description
Technical field
The present invention relates to a kind of preparation processes of Ultramicro-powder, and in particular to a kind of preparation of prepared fleece flower root Ultramicro-powder medicine materical crude slice
Technique belongs to Technique for producing medicinal herbs in small pieces field.
Background technology
Prepared fleece flower root is polygonum multiflorum thunbPolygonum multiflorum The processed product of Thunb dried roots,
Have the effect of filling liver kidney, benefiting essence-blood, black beard and hair, strengthening the bones and muscles, be usually used in blood deficiency chlorosis, dizziness and tinnitus, poliosis, waist and knee acid
Under soft, extremity numbness, uterine bleeding band and hyperlipidemia etc..
Study on Supermicro-pulverization of Traditional Chinese Drugs technology is also known as Chinese medicine cell wall breaking technology.Under normal circumstances, the active ingredient of Chinese medicine is main
It is present in into the cell, active ingredient can be just utilized after only penetrating cell membrane walls.Superfine communication technique can destroy Chinese medicine
Cell membrane walls can reach more than 90% cell-wall breaking ratio.Its intracellular active ingredient is exposed after breaking-wall cell, so
Drug effect increases substantially, and action speed is fast.The particularly medicinal material of quality hard and compact, due to that can exempt from after ultramicro grinding broken wall
Except solvent penetration cell wall enters the lengthy procedure and obstacle for into the cell dissolving out effective component, therefore it is more advantageous to shortening extraction
Time reduces dosage.And the final product of ultramicro grinding is ultrafine powder, it is special with some that fine powder does not have
Physicochemical property, such as the grain size that smaller is more uniform, good dissolubility, adsorptivity, dispersibility, chemical reactivity etc. are conducive to
Develop the small novel form of dosage.
The fleece-flower root is one of rare Chinese medicine, clinically often with 6-12 g prepared fleece flower root routine medicine materical crude slice decoctions, but because it is mostly
Irregular shrinkage block piece, thickness about 1cm, matter is hard, and active ingredient contained when decocting of being used as medicine cannot be fully dissolved out, and causes medicinal material unrestrained
Take.Modern research shows that free property Anthraquinones and the main active that stibene glucoside type compound is prepared fleece flower root, wherein
Anthraquinone analog compound is fat-soluble compound, is decocted in the form of conventional medicine materical crude slice with water, is less useful for its dissolution.
Invention content
The object of the present invention is to provide a kind of preparation processes of prepared fleece flower root Ultramicro-powder medicine materical crude slice, and solving above-mentioned conventional medicine materical crude slice has
Imitate the problem of ingredient dissolution rate is not high.
To achieve the above object, the present invention uses following technical proposals：
A kind of preparation process of prepared fleece flower root Ultramicro-powder medicine materical crude slice, including step：
（1）Feedstock processing：With heated-air circulation oven to drying 3h to prepared fleece flower root routine medicine materical crude slice at 60 DEG C, this operation is to protect
It is not exceeded to demonstrate,prove prepared fleece flower root medicine materical crude slice moisture, is easy to crush；
（2）Coarse crushing：Coarse crushing is carried out to prepared fleece flower root medicine materical crude slice with Universalpulverizer, No. two sieves is crossed, obtains coarse powder；
（3）Screening：Coarse powder with pharmacopeia is sieved and carries out rough segmentation, No. five sieves is crossed and obtains fine powder, grain size is 20 μm -180 μm, it is therefore an objective to be
Crushing behind convenience；
（4）Ultramicro grinding：Fine powder is thrown in WZJ6 Baily micronizers, fine powder accounts for the 2/3 of magazine, is crushed at -5 DEG C
25min obtains prepared fleece flower root Ultramicro-powder, and average grain diameter is 30 μm.
Beneficial effects of the present invention：
By proving prepared fleece flower root routine medicine materical crude slice, fine powder and Ultramicro-powder extract and content analysis experiment, using ultramicro grinding
Prepared fleece flower root Ultramicro-powder medicine materical crude slice extract and Stibene-glucoside, rheum emodin and Physcion content prepared by technology is significantly high
In prepared fleece flower root medicine materical crude slice and fine powder.Grain size, specific surface area and single-point total pore volume are carried out to prepared fleece flower root fine powder and Ultramicro-powder to survey
It is fixed, Ultramicro-powder is found compared with fine powder grain size smaller and more uniform, and specific surface area and single-point total pore volume have very significant raising.
In addition, prepared fleece flower root Ultramicro-powder medicine materical crude slice is brewed with boiling water, active ingredient can Fast Stripping, it is convenient to take.
Description of the drawings
Fig. 1 is the infrared spectrogram of embodiment (b) and comparative example (a) in 2 infrared discriminating of test example.
Specific implementation method
With reference to example, the present invention is described in more detail, it should be noted that the description below is merely to explain this hair
It is bright, its content is not defined.
Embodiment：
A kind of preparation process of prepared fleece flower root Ultramicro-powder medicine materical crude slice, specific steps：With heated-air circulation oven to system, what is first at 60 DEG C
Black tradition medicine materical crude slice drying 3h, this operation is to ensure that prepared fleece flower root medicine materical crude slice moisture is not exceeded, be easy to crush；Use Universalpulverizer
Coarse crushing is carried out to prepared fleece flower root medicine materical crude slice, No. two sieves is crossed, obtains coarse powder；Coarse powder with pharmacopeia is sieved and carries out rough segmentation, No. five is crossed and sieves
To fine powder, grain size is 180 μm -200 μm, fine powder is thrown in WZJ6 Baily micronizers, fine powder accounts for the 2/3 of magazine, in -5
25 min are crushed at DEG C and obtain prepared fleece flower root Ultramicro-powder, average grain diameter is 30 μm.
Comparative example：
With heated-air circulation oven to drying 3h to prepared fleece flower root tradition medicine materical crude slice at 60 DEG C, this operation is to ensure that prepared fleece flower root is drunk
Piece moisture is not exceeded, is easy to crush；Coarse crushing is carried out to prepared fleece flower root medicine materical crude slice with Universalpulverizer, No. two sieves is crossed, obtains coarse powder；
Coarse powder with pharmacopeia is sieved and carries out rough segmentation, No. six sieves is crossed and obtains fine powder, average grain diameter is 48 μm.
Test example
1. grain size and dry jet mixing pile measure
Example and the Ultramicro-powder and appropriate fine powder of comparative example respectively, are placed in granularmetric analysis container, using distilled water as dispersion
Agent, 60 s of ultrasonic disperse, measures their size distribution；Example and comparative example powder are appropriate respectively, are fitted into and measure in bottle,
It is placed in pretreatment system, in degassing in 50 DEG C of nitrogen that circulate to constant weight, is placed in adsorption instrument, specific surface is measured using BET method
The relevant informations such as product and single-point total pore volume, the results are shown in Table 1.
The grain size and dry jet mixing pile of 1 two kinds of powders of table
The grain size of the Ultramicro-powder of embodiment is substantially less than comparative example as shown in Table 1, and particle diameter distribution is evenly；While embodiment
Ultramicro-powder has the specific surface area of bigger and single-point total pore volume compared with comparative example.Illustrate that the preparation method of the present invention prepares grain size
The more uniform Ultramicro-powder of smaller, while product specific surface area and porosity bigger, are conducive to active ingredient and quickly dissolve out.
2. infrared discriminating
Ultramicro-powder is weighed respectively and 1 g of fine powder is put into measuring cup, after putting 80 DEG C of 12 h of thermostatic drying chamber drying, uses bromination
Potassium (1:200) piece measures its infrared spectrogram, the result is shown in Figure 1.As can be seen from Figure 1 the infrared light of Ultramicro-powder and fine powder
It composes basically identical, shows that ultramicro grinding does not change the chemical composition of prepared fleece flower root medicine materical crude slice.
3. ethanol soluble extractives assay
Prepared fleece flower root powder each 2g that respectively prepared by Example and comparative example, it is accurately weighed, it puts in the conical flask of 100mL, essence
Close measurement 50 mL of ethyl alcohol, close plug, weighed weight after standing 1h, connect reflux condensing tube, are heated to boiling, and keep slightly boiling
1h.After letting cool, boiling flask, close plug, then weighed weight are removed, the weight of less loss is supplied with ethyl alcohol, is shaken up, filtered with dry filter
Cross, it is each it is accurate measure 25 mL of filtrate, be placed in it is dry in the evaporating dish of constant weight, after being evaporated in water-bath, in 105 DEG C of dry 3h,
It puts and 30min is cooled down in drier, rapid accurately weighed weight.It operates, measures as stated above.Obtain different prepared fleece flower root powders
The content of ethanol soluble extractives, the results are shown in Table 2.
2 ethanol soluble extractives assay of table
The Ultramicro-powder ethanol soluble extractives content higher of embodiment, comparative example ethanol soluble extractives content are significantly low as shown in Table 2
In embodiment.Illustrate that the preparation method of the present invention is more advantageous to the dissolution of alcohol-soluble substance in prepared fleece flower root medicine materical crude slice.
4. active constituent content measuring
Stibene-glucoside and dissociated anthraquinone are the principle active component of the fleece-flower root, using Stibene-glucoside and dissociated anthraquinone as system how
The index components of tuber of multiflower knotweed medicine materical crude slice.Using high performance liquid chromatography, to same a collection of prepared fleece flower root tradition medicine materical crude slice, respectively by embodiment and
Finished product is made in comparative example, carries out Stibene-glucoside and dissociated anthraquinone assay, dissociated anthraquinone content is with rheum emodin and rheum emodin
The total amount meter of methyl ether, measurement result are shown in Table 3.
Stibene-glucoside assay
Chromatographic condition:Chromatographic column is Cosmosil C18Column（250 mm × 4.6 mm）；With acetonitrile-water（25：75) it is flowing
Phase；Detection wavelength is 320 nm；Flow velocity is 1.0 mL/min；10 μ L of sample size；Column temperature：25 ℃.
The preparation of solution：Take 2,3,5,4 '-tetrahydroxystilbene -2-O-βD-Glucose glycosides reference substance is appropriate, accurate
It is weighed, add Diluted Alcohol that the solution that every lmL contains 0.2 mg is made, obtain reference substance solution.Take the system that about prepared by embodiment and comparative example
0.2 g of fleece-flower root body powder, it is accurately weighed respectively, it puts in conical flask with cover, precision adds in 25 mL of Diluted Alcohol, weighed weight, heating
Reflux 30 minutes, lets cool, then weighed weight, the weight of less loss is supplied with Diluted Alcohol, is shaken up, and stands, and supernatant filtration takes continuous filter
Liquid crosses 0.45 μm of miillpore filter, obtains test solution.
Dissociated anthraquinone assay
Chromatographic condition：Chromatographic column is；Mobile phase：With -0.1% phosphoric acid solution (80 of methanol:20) it is mobile phase；Detection wavelength：254
nm；Flow velocity：1.0 mL/min；Sample size：10 µL；Column temperature：25 ℃.
The preparation of solution:Take rheum emodin reference substance, Physcion reference substance appropriate, it is accurately weighed, methanol is added to make respectively
Into solution of every 1 μ L containing 80 μ g of rheum emodin, 40 μ g of Physcion, reference substance solution is obtained.It is prepared by Example and comparative example
Prepared fleece flower root body powder about lg, it is accurately weighed, put in conical flask with cover, precision adds in 50 mL of methanol, and weighed weight heats back
1 h is flowed, is taken out, is let cool, then weighed weight, the weight of less loss is supplied with methanol, is shaken up, is filtered, takes subsequent filtrate, crosses 0.45 μm
Miillpore filter obtains test solution.
The content of active ingredient in 3 prepared fleece flower root medicine materical crude slice of table
As shown in Table 3, the content of dissociated anthraquinone is significantly higher than comparative example, explanation in the test solution prepared by embodiment powder
The preparation method of the present invention is more advantageous to active ingredient（Especially dissociated anthraquinone）Dissolution.
Claims (4)
1. a kind of preparation process of prepared fleece flower root Ultramicro-powder medicine materical crude slice, it is characterised in that：It is the ultra micro of 25 μm -40 μm of average grain diameter
Powder.
2. the prepared fleece flower root Ultramicro-powder is required according to right 1, it is characterised in that：It is the ultra micro that average grain diameter is 30 μm
Powder.
A kind of 3. method for preparing prepared fleece flower root Ultramicro-powder described in claim 1-2 any one, it is characterised in that：Step is such as
Under：Feedstock processing：3h is dried to prepared fleece flower root tradition medicine materical crude slice at 60 DEG C with heated-air circulation oven；Coarse crushing：With omnipotent crushing
Machine crushes prepared fleece flower root medicine materical crude slice, crosses No. two sieves, obtains coarse powder；Screening：Coarse powder with pharmacopeia is sieved and carries out rough segmentation, crosses No. five
Sieve obtains fine powder, and grain size is 20 μm -180 μm,；Ultramicro grinding：Fine powder is thrown in WZJ6 Baily micronizers, fine powder accounts for
The 2/3 of magazine, -5 DEG C of crushing 25min, average grain diameter is 30 μm.
4. the prepared fleece flower root Ultramicro-powder is required according to right 3, it is characterised in that：Particle diameter distribution is more uniform, cell-wall breaking ratio
Height, surface area and single-point total pore volume all greatly increase, and the dissolution rate of dissociated anthraquinone significantly improves.
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| CN201711201348.7A CN108236626A (en) | 2017-11-27 | 2017-11-27 | A kind of preparation process of prepared fleece flower root Ultramicro-powder medicine materical crude slice |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105412278A (en) * | 2015-12-11 | 2016-03-23 | 普洱淞茂制药股份有限公司 | Medicine composition, preparation method thereof, preparation and application |
| KR20160081415A (en) * | 2014-12-31 | 2016-07-08 | 엄시용 | Manufacturing method for Rubus coreanus noodles and cooking Method thereof |
| CN106491742A (en) * | 2016-11-25 | 2017-03-15 | 成都天河中西医科技保育有限公司 | The technique that micronizing method prepares Rhizoma Coptidis micropowder |
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2017
- 2017-11-27 CN CN201711201348.7A patent/CN108236626A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20160081415A (en) * | 2014-12-31 | 2016-07-08 | 엄시용 | Manufacturing method for Rubus coreanus noodles and cooking Method thereof |
| CN105412278A (en) * | 2015-12-11 | 2016-03-23 | 普洱淞茂制药股份有限公司 | Medicine composition, preparation method thereof, preparation and application |
| CN106491742A (en) * | 2016-11-25 | 2017-03-15 | 成都天河中西医科技保育有限公司 | The technique that micronizing method prepares Rhizoma Coptidis micropowder |
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Application publication date: 20180703 |