CN107260900A - A kind of safflower ultramicro decoction piece preparation method - Google Patents
A kind of safflower ultramicro decoction piece preparation method Download PDFInfo
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- 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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- 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 present invention discloses a kind of safflower ultramicro decoction piece preparation method based on material modification, passes through：Safflower is chosen using local figure treatment technology, the removal of impurity is gone according to dislocation degree；By safflower medicinal material low-temperature treatment, cool according to chi square function, reach less than 15 DEG C；By the good pulverizing medicinal materials of precooling into coarse powder；Safflower after-treatment, first constant speed cools and freezed, then microwave heating is thawed, and by expanding with heat and contract with cold, method destroys medicinal material institutional framework, strengthens the fragility of material, the efficiency of raising air-flow crushing；Sampling, observes the surface treatment result of safflower material.After qualified, particle diameter is crushed to less than 5 microns using gas flow crushing process, then sterilization treatment, obtains safflower ultramicro decoction piece.Safflower ultramicro decoction piece preparation method of the present invention, can effectively reduce the loss of the heat-sensitive ingredients of process medicinal material, improve the dissolution rate of active ingredient, so as to strengthen safflower promoting blood circulation and cosmetology function.
Description
Technical field
The invention belongs to your detail processing of crude drugs technical field, more particularly it relates to which one kind is with safflower medicinal material
The process of ultramicro decoction piece is prepared for raw material.
Background technology
Safflower (saffron, Crocus sativus L.) is also known as west safflower, is that Iridaceae crocus napiform root class is more
Year raw herbaceous plant, medicinal part is chapiter, and original producton location is in states such as Greece, Spain and Iran, through the incoming China in Tibet.
《Compendium of Materia Medica》Described in " safron, with going out the western kind Huis and state of old name for the Arabian countries in the Middle East, i.e. that ground red blue flower.When first, used with food food.”
Because safflower yields poorly, time and effort consuming is harvested, causes it to hold at high price, rare rare traditional Chinese medicine is listed in China,
More someone's reputation is " plant gold ".Safflower have effects that strong promoting blood circulation promoting circulation of blood and it is scattered it is strongly fragrant open knot, adhere to taking for a long time
The immunity of human body can be improved comprehensively.《Compendium of Materia Medica》Record, safflower energy " promoting blood circulation, the main motive are melancholy, and palpitation with fear is controlled again ".It is modern
Research finds that the crocin class material contained in safflower also has good active anticancer, for blood cell, papillary carcinoma
There is stronger inhibitory action with soft tissue sarcoma etc., it is following probably to turn into one of preferable new anticancer drug.
Traditional prepared slices of Chinese crude drugs process mode, because the loss of its active ingredient is serious, bioavailability is low, and thus cause
Necessary enough long-term taking features, virtually add drug cost.With the development and progress of modern production process, a lot
New medicine materical crude slice type is studied exploitation, including ultramicro decoction piece, pure powder oral medicinal slice, ultramicro powder medicine materical crude slice etc., to incite somebody to action
The drawbacks of to improve traditional medicine materical crude slice, is there is provided new direction.
Because active ingredient is more sensitive to temperature in safflower, conventional ultramicro grinding technique can cause active component
Decompose and lose, influence product quality.Therefore, a kind of ultra micro that can effectively keep safflower active component and color and luster is invented to drink
Piece preparation method, has positive effect for the effect and economic value for improving the expensive thin medicinal material.
In recent years, superfine communication technique achieves significant progress in terms of Chinese medicine processing.Patent
201310387183.2 disclose a kind of preparation method of American Ginseng ultramicro pure powder oral medicinal slice.The method includes American Ginseng ultralow temperature
Liquid nitrogen is crushed, and low pressure is dried, Co 60 radiation sterilization, the step such as tabletting.It is pure that patent 201510228964.6 discloses a kind of donkey-hide gelatin
Powder ultramicro decoction piece and preparation method thereof.The invention the described method comprises the following steps：First, new fresh Donkey-hide Glue crushed after being dried is made slightly
Powder, sterilizing；2nd, coarse powder is freeze-dried；3rd, dried coarse powder is further crushed through research of super-pine crush equipment, obtains particle diameter less than 3
The ultramicro decoction piece of micron.The result of above-mentioned technological innovation shows, ultra-fine powder preparation technology is for improving the biological utilisation of Chinese medicine
Degree has significant effect.
In terms of the research of safflower medicinal material, domestic scholars and enterprise technology personnel have carried out multinomial work and obtained
Some achievements.For example, the method for the material that skimmed the cream off milk in a kind of safflower of patent 201310535173.9 invention, is extracted by water
Take, micro-pore-film filtration, reverse osmosis concentration and the step such as be dried under reduced pressure and prepare safranine flower extract.Because safflower composition has water concurrently
Dissolubility with it is fat-soluble and more sensitive to temperature, so, the defect of extraction process is part loss of effective components.Patent
201510834605.5 propose a kind of safflower super-micro wall-broken breaking method.Its core technology is that this method is in coarse powder
On the premise of addition zein and glycerin monostearate, the super-micro wall-broken for completing safflower is crushed.This method advantage is super
Micro mist preparation technology be conducive to improve safflower in bioavilability, have the disadvantage ambient ground processing technology can cause temperature-sensitive into
The loss divided.
So, for safflower character of medicinal material and the present situation of existing process technology, the present invention uses for reference Chinese medicine superfine comminution
Technology, and study the bottleneck problem of safflower character of medicinal material and process, it is proposed that one kind is based on material modification and low temperature powder
The broken ultramicro decoction piece preparation technology new method for being capable of retentive activity composition and color and luster to greatest extent being combined, to solve safflower
Grinding time length, flour extraction in traditional broken wall breaking method is low and the problems such as high loss of effective components rate.
The medicinal part of safflower is the chapiter of the plant.Relative to other Chinese medicines, safflower belong to it is soft without
Easily crush.Using conventional disintegrating process, it is desirable to provide more energy, therefore, crushing process efficiency are low, moreover, mechanical
Heat energy can be converted into, the temperature of medicinal material is substantially increased, and causes the loss of heat-sensitive ingredients.In this regard, process proposed by the present invention,
By special freezing method, control material temperature lowering curve effectively changes the physical property of safflower medicinal material, cold by low temperature heat expansion
Contracting destroys its institutional framework, mitigates mechanical crushing resistance.On the other hand, low-temperature treatment and special heat transfer type, reinforcer are passed through
The fragility of material, improves the efficiency of air-flow crushing, shortens grinding time, reduces the loss of heat-sensitive ingredients.
The content of the invention
Product bioavailability is improved it is an object of the invention to provide one kind, more easily safflower ultramicro decoction piece is taken
Preparation method.The preparation method is realized by following steps：
(1) using local figure treatment technology selection safflower, the removal of impurity is gone according to dislocation degree；
(2) by safflower medicinal material low-temperature treatment, cool according to chi square function, reach less than -15 DEG C；It is preferred that -20 DEG C~-15
℃。
(3) the good medicinal material of precooling is ground into coarse powder at 0 DEG C -5 DEG C；
(4) safflower after-treatment, first constant speed cools and freezed, then microwave heating is thawed, and by expanding with heat and contract with cold, method is broken
Bad medicinal material institutional framework, strengthens the fragility of material；
(5) sample, observe the surface texture of safflower material, material modification effect.After qualified, using gas flow crushing process
Particle diameter is crushed to less than 5 microns, then sterilization treatment, obtains safflower ultramicro decoction piece.
In above-mentioned preparation technology, step (1) is related to the selection of safflower, and its core technology is to pluck position, flower according to it
The factors such as stamen length, the integrity degree of flower, color and luster are quickly chosen, including：Video camera imaging, computer graphics analysis, safflower are special
Levy extraction, impurity and medicinal material image recognition inferior and the step such as the local medicinal material of manipulator is sorted out.
Medicinal material cryogenic treatment process described in step (2), is completed in ultra low temperature freezer or under liquid nitrogen environment, and it drops
Warm rate of acceleration needs strict control, to reach the purpose of destruction medicinal material institutional framework, the scope of cooling rate of acceleration for -0.005 DEG C/
min2~-0.05 DEG C/min2, outlet temperature is -20 DEG C -15 DEG C.
For the safflower medicinal material primary comminution described in step (3) into coarse powder, its key is low temperature and quickly handled.Powder
The broken time, temperature of charge was maintained at 0 DEG C -5 DEG C within 30min.
For the safflower after-treatment described in step (4), its core technology includes：Safflower pre-freezing temperature is -40
DEG C~-50 DEG C, the pre-freeze time is 1-3 hours；Cooling rate is between -1~-5 DEG C/h；Heated and thawed using microwave, it is quick to rise
Temperature is to 30~50 DEG C, and by expanding with heat and contract with cold, method destroys medicinal material institutional framework, strengthens the fragility of material, then, vacuum drying 12
~24 hours.
It is 0.4-0.8MPa, feed pressure to include crushing pressure for the gas flow crushing process parameter described in step (5)
For 0.3-0.7MPa, charging rate is 0.5-1.5Kg/h.Safflower ultramicro decoction piece determines its grain through dry laser particle size analyzer
Footpath is 1~5 micron.
For the Biocidal treatment method in step (5), including it is ray sterilizing, microwave sterilization or ozone sterilization method
It is any one or several.
Different from existing conventional Chinese medicine superfine comminution technique, safflower ultramicro decoction piece preparation side disclosed by the invention
Method focuses on the special nature of safflower medicinal material, including physical property and chemical property, it is proposed that the skill of new processing technology
Art requirement and quality assurance measure.In process, realize that medicinal material fragility is adjusted by specific freezing method, seek to be easy to gas
Flow the state crushed；By expanding with heat and contract with cold repeatedly, safflower institutional framework is destroyed, the mechanical energy consumption of crushing process is reduced, favorably
Lower temperature is in material, mitigates heat-sensitive ingredients degraded.
Safflower ultramicro decoction piece preparation method of the present invention based on material modification, can effectively reduce process medicine
The loss of the heat-sensitive ingredients of material, improves the dissolution rate of active ingredient, so as to strengthen safflower promoting blood circulation and cosmetology function.
Brief description of the drawings
Accompanying drawing 1 is the grain size distribution of safflower coarse powder.
Accompanying drawing 2 is the grain size distribution of safflower ultramicro decoction piece.
Embodiment
In order that the purpose of the present invention and technical scheme are more clear, below in conjunction with example, traveling one is entered to the present invention
Step is described in detail.
Embodiment 1
Safflower ultramicro decoction piece is prepared as follows method and is made：
(1) safflower raw material 1kg, is taken, it is long to pluck position, pistil using video camera imaging, computer graphics analysis
The factor such as degree, integrity degree, the color and luster of flower is sorted out as feature recognition impurity and medicinal material inferior using the local medicinal material of manipulator.Its
In qualified medicinal material 0.94kg；Defective work 0.06kg.
(2), by qualified safflower medicinal material low-temperature treatment, cool according to chi square function, with -0.05 DEG C/min2Accelerate drop
Temperature is to -15 DEG C；
(3) the good medicinal material of precooling, is ground into coarse powder in 5 DEG C of environment；
(4), safflower after-treatment, is first cooled to -40 DEG C, system is vacuumized with -2 DEG C/h constant speed, and absolute pressure is kept
In 45Pa, then lyophilization, sublimation temperature is 35 DEG C, is dried 12 hours, improves coarse powder particles surface characteristic；
(5), sample, the surface texture of micro- Microscopic observation safflower coarse powder.Ultramicro grinding is carried out after after-treatment is qualified,
Otherwise after-treatment is come again.
The technological parameter of airslide disintegrating mill is to crush pressure 0.4MPa, feed pressure 0.3MPa, charging rate 0.5kg/h,
Using microwave method sterilization treatment, safflower ultramicro decoction piece is obtained.
Obtained safflower ultramicro decoction piece, answers color and luster consistent, the phenomenon such as no moisture absorption, caking.
Also the peroral dosage forms such as tablet, capsule can be made with meeting the auxiliary material of medicament requirement in ultramicro decoction piece.
Embodiment 2
The impure medicinal materials of the 60g chosen automatically in embodiment 1 are collected, are placed in artificial selection platform, using hand
Work picking method, the safflower medicinal material of the high-quality of wherein wrong choosing is sorted out, concentrates together, returns to original qualified Chinese medicine
In, to improve the utilization rate of medicinal material, reduce medicinal material loss.Secondary recovery obtains 36g safflower medicinal materials, and the rate of recovery is 60%.
Embodiment 3
The granularmetric analysis of safflower ultramicro decoction piece powder uses Laser immunotherapy.
Before measure, laser particle size analyzer start preheating more than 30 minutes.
Sample introduction：Ultramicro decoction piece 2~4g of sample is added in sample introduction tank, click starts, start analysis.In the data of measurement
In, shading ratio should be controlled between 0.5~3, reject shading than undesirable data, work station automatic measurement goes out safflower
The grain size distribution and Cumulative logit model of ultramicro decoction piece.
Embodiment 4
The grain of coarse powder and ultramicro decoction piece finished product in safflower ultramicro decoction piece process is determined according to the method for embodiment 3
Footpath.The particle diameter distribution of coarse powder and finished product is as shown in Figures 1 and 2.The instant result of particle diameter distribution is as listed in table 1.
The particle diameter of coarse powder and finished product in the safflower ultramicro decoction piece process of table 1
| Sample | d(0.1)/μm | d(0.5)/μm | d(0.9)/μm | Peak shape |
| Coarse powder | 30.72 | 172.69 | 374.63 | It is unimodal |
| Ultramicro decoction piece | 0.88 | 2.85 | 6.29 | It is unimodal |
Note：D (0.1) represents the diameter corresponding to 10% in granularity cumulative distribution (0 to 100%).
As can be seen from Table 1, safflower ultramicro decoction piece finished product is compared with the particle diameter of semi-finished product coarse powder, and its d (0.5) have dropped
98.35%, d (0.9) have dropped 98.32%, illustrate the centralized particle diameter of safflower ultramicro decoction piece, and uniformity is good, meet thin
Degree is required.
Embodiment 5
Flour extraction compares, and takes 400g safflower medicinal materials, respectively two groups, take one group routinely ultramicro grinding method prepare safflower
Ultramicro decoction piece, takes one group of method as described in embodiment 1 to be weighed after preparing safflower ultramicro decoction piece, two groups of collection powder.
The different preparation method safflower flour extractions of table 2 compare
Drawn by that can contrast, safflower ultramicro decoction piece described herein prepares the more conventional ultramicro grinding method preparation method of yield
Yield lifting 3.6%, the active ingredient quantitative analysis in conjunction with embodiment 6 is contrasted, and preparation method described herein can be carried effectively
Rise the active constituent content and product yield of safflower ultramicro decoction piece.
Embodiment 6
With reference to standards of pharmacopoeia method, raw material and product crocin-I (C are determined44H64O24) and crocin-II
(C38H54O19) content.
Safflower, conventional Ultramicro-powder and each 10mg of this handicraft product are taken, is put in 50mL brown measuring bottles, plus appropriate Diluted Alcohol,
Put in ice bath ultrasonically treated 20 minutes, put to room temperature, plus Diluted Alcohol and be diluted to scale, shake up, filter, take subsequent filtrate, cross 0.45
Micron membrane filter, is produced.Parallel 3 parts of preparation, it is stand-by.
It is prepared by standard items：Take the reference substance of crocin-I, the reference substance of crocin-II appropriate, it is accurately weighed, plus Diluted Alcohol
The solution that every 1mL contains 30 μ g and 12 μ g is respectively prepared, produces.Parallel 3 parts of preparation, it is stand-by.
Assay：Take reference substance solution and each 10mL of need testing solution, inject liquid chromatograph, parallel determination three times,
Calculate average value and deviation.Content analysis result is as shown in table 3.
The content analysis result (n=3) of the safflower of table 3 and its converted products
| Sample | Average grain diameter (μm) | Crocin-I (%) | Crocin-II (%) |
| Crude drug | - | 13.87±0.13 | 4.55±0.04 |
| Conventional Ultramicro-powder | 8 | 14.00±1.08 | 4.74±0.60 |
| New technology product | 4.5 | 15.29±1.23 | 5.30±0.47 |
As shown in Table 3, active ingredient crocin-I contents are higher than crude drug by 10.3% in new technology product, super than conventional
Micro mist is high by 9.2%；The content of crocin-II is higher than crude drug by 16.5%, higher than conventional Ultramicro-powder by 11.6%.This shows, new work
Skill improves safflower preparation technology, improves the efficiency of air-flow crushing, shortens grinding time, effectively reduce temperature-sensitive into
The loss divided.
Embodiment 7
Safflower raw material 2kg is taken, method processing is prepared as follows：
(1), the picking method of safflower medicinal material is same as Example 1.
(2), by safflower medicinal material low-temperature treatment, cool according to chi square function, with -0.03 DEG C/min2Acceleration is cooled to -17
℃。
(3) the good medicinal material of precooling, is ground into coarse powder in 1 DEG C of environment.
(4), safflower after-treatment, is first cooled to -50 DEG C with -3 DEG C/h constant speed；Then heated, be warming up to using microwave
40 DEG C, by expanding with heat and contract with cold, method destroys medicinal material institutional framework, strengthens the fragility of coarse powder material；
(5), sample, the surface texture of micro- Microscopic observation safflower coarse powder.Air-flow crushing is carried out after qualified.Its technique is joined
Number, then using the processing of ozone sterilization method, obtains to crush pressure 0.5MPa, feed pressure 0.4MPa, charging rate 0.6kg/h
To safflower ultramicro decoction piece.
The particle diameter of safflower ultramicro decoction piece is determined according to the method for embodiment 3.
Embodiment 8
Safflower raw material 2kg is taken, method processing is prepared as follows：
(1), the picking method of safflower medicinal material is same as Example 1.
(2), by safflower medicinal material low-temperature treatment, cool according to chi square function, with -0.009 DEG C/min2Acceleration cools
To -20 DEG C；
(3) the good medicinal material of precooling, is ground into coarse powder in 3 DEG C of environment；
(4), safflower after-treatment, is first cooled to -50 DEG C, system is vacuumized with -4 DEG C/h constant speed, and absolute pressure is kept
In 50Pa, then lyophilization, sublimation temperature is 45 DEG C, is dried 16 hours；
(5), sample, observe the surface treatment result of safflower material.After qualified, grain is crushed to using gas flow crushing process
Footpath is less than 5 microns, and the technological parameter of airslide disintegrating mill is crushing pressure 0.8MPa, feed pressure 0.7MPa, charging rate 1kg/
H, is handled using ray sterilizing, obtains safflower ultramicro decoction piece.
The particle diameter of safflower ultramicro decoction piece is determined according to the method for embodiment 3.
In a word, the certain embodiments of the implementation content of the present invention are the foregoing is only, it is all according to scope of the present invention patent institute
The equivalent changes and modifications done, should all belong to the covering scope of patent of the present invention.
Claims (8)
1. a kind of safflower ultramicro decoction piece preparation method, it is characterised in that realized by following steps：
(1) safflower is chosen using graphics analysis techniques, the removal of impurity is gone according to dislocation degree；
(2) by safflower medicinal material low-temperature treatment, cool according to chi square function, reach -20 DEG C~-15 DEG C；
(3) by the good pulverizing medicinal materials of precooling into coarse powder；
(4) after-treatment, first constant speed cools and freezed, then microwave heating is thawed, and passes through method of expanding with heat and contract with cold and destroys medicinal material tissue
Structure, strengthens the fragility of material；
(5) sample, observe the surface texture of safflower material, analysis of material modified effect.Then, using gas flow crushing process powder
Particle diameter is broken to less than 5 microns, then sterilization treatment, obtain safflower ultramicro decoction piece.
2. a kind of safflower ultramicro decoction piece preparation method according to claim 1, it is characterised in that described in step (1)
Safflower medicinal material picking method be：Video camera imaging, computer graphics analysis, safflower feature extraction, impurity and medicine inferior
Material image recognition and the local medicinal material of manipulator sort out step, and local is mixed with secondary selection after impurity medicinal material can be collected.
3. a kind of safflower ultramicro decoction piece preparation method according to claim 1, it is characterised in that described in step (2)
Safflower medicinal material low-temperature treatment completed in ultra low temperature freezer or under liquid nitrogen environment, the strict rate of temperature fall of process, cooling plus
The scope of speed is -0.005 DEG C/min2~-0.05 DEG C/min2, outlet temperature is at -20 DEG C~-15 DEG C.
4. a kind of safflower ultramicro decoction piece preparation method according to claim 1, it is characterised in that described in step (3)
The requirement of safflower primary comminution be：Processing time, temperature of charge was at 0 DEG C~5 DEG C within 30min.
5. a kind of safflower ultramicro decoction piece preparation method according to claim 1, it is characterised in that described in step (4)
Safflower dual-spectrum process include：Safflower was in -40 DEG C~-50 DEG C pre-freezes 1-3 hours, and then microwave is heated to 30
~50 DEG C, by expanding with heat and contract with cold, method destroys medicinal material institutional framework, strengthens the fragility of material, then, and vacuum drying 12~24 is small
When.
6. a kind of safflower ultramicro decoction piece preparation method according to claim 1, it is characterised in that step (5) gas
Stream disintegrating process parameter includes：Crushing pressure is 0.4-0.8MPa, and feed pressure is 0.3-0.7MPa, and charging rate is 0.5-
1.5Kg/h。
7. a kind of safflower ultramicro decoction piece preparation method according to claim 1, it is characterised in that going out in step (5)
Bacterium processing method, from the one or more in ray sterilizing, microwave sterilization or ozone sterilization method.
8. a kind of safflower ultramicro decoction piece preparation method according to claim 1, it is characterised in that described in step (4)
Safflower after-treatment cooling rate between -1~-5 DEG C/h.
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| CN112076256A (en) * | 2020-09-24 | 2020-12-15 | 北京金崇光药业有限公司 | Low-temperature ultrafine grinding process |
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| CN106387584A (en) * | 2015-07-27 | 2017-02-15 | 梁伟池 | Crocus sativus solid beverage and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102772437A (en) * | 2012-05-24 | 2012-11-14 | 周明千 | Processing method of ultra-micro wall-breaking oral liquid-preparation decoction pieces by traditional Chinese medicines |
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| CN105582690A (en) * | 2014-10-21 | 2016-05-18 | 谢慧萍 | Microwave extraction method and system thereof |
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| CN112076256A (en) * | 2020-09-24 | 2020-12-15 | 北京金崇光药业有限公司 | Low-temperature ultrafine grinding process |
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Application publication date: 20171020 |