CN103536747A - Bulbus fritillariae cirrhosae ultra-fine powder preparation technology - Google Patents

Bulbus fritillariae cirrhosae ultra-fine powder preparation technology Download PDF

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CN103536747A
CN103536747A CN201310495886.7A CN201310495886A CN103536747A CN 103536747 A CN103536747 A CN 103536747A CN 201310495886 A CN201310495886 A CN 201310495886A CN 103536747 A CN103536747 A CN 103536747A
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bulbus fritillariae
fritillariae cirrhosae
freeze
micropowder
raw material
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CN103536747B (en
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陈照荣
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Zhejiang Zuo Libaicao prepared slices of Chinese crude drugs company limited
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ZHEJIANG BAICAO TRADITIONAL CHINESE MEDICINE PIECES CO Ltd
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Abstract

The invention relates a bulbus fritillariae cirrhosae processing method, and particularly relates to a bulbus fritillariae cirrhosae ultra-fine powder preparation technology. The bulbus fritillariae cirrhosae ultra-fine powder preparation technology comprises the following steps: (1) choosing a raw material; (2) pulping, namely grinding bulbus fritillariae cirrhosae serving as the raw material, adding microcrystalline cellulose powder which accounts for 10-20wt% of the raw material, and fully mixing the raw material and the microcrystalline cellulose powder through the rotation of a mixer charging bucket, thus obtaining a mixed material; then adding water which is 0.7-0.8 times of the weight of the mixed material so as to pulp; (3) prefreezing, namely, adding tween-80 which accounts for 10-15wt% of the weight of pulp before prefreezing, and fully mixing; (4) freezing and drying, and requesting for controlling the moisture content below 6wt%; (5) powdering by using a vibrating type superfine grinding mixing mill. The bulbus fritillariae cirrhosae prepared by the method can be used for retaining active ingredients in the bulbus fritillariae cirrhosae to the maximum degree.

Description

A kind of Bulbus Fritillariae Cirrhosae superfine powder preparation technology
Technical field
The present invention relates to a kind of processing method of Bulbus Fritillariae Cirrhosae, be specifically related to a kind of Bulbus Fritillariae Cirrhosae superfine powder preparation technology.
Background technology
Prior art, when concocting this herb of Bulbus Fritillariae Cirrhosae, is normally dried section.Modern study shows, traditional concocting method will the many active component of loss.
Application number is 02154200.7 Chinese invention patent; a kind of preparation method of cow-bezoar snake bile Sichuan fritillary bulb dispersive is disclosed; the method has comprised the processing method of Bulbus Fritillariae Cirrhosae, and Bulbus Fritillariae Cirrhosae powder was broken into 80~160 object fine powders, is preferably ground into 200~300 object fine powders.In the method, directly Bulbus Fritillariae Cirrhosae powder is broken into micropowder, causes active component in Bulbus Fritillariae Cirrhosae greatly to lack.
Summary of the invention
The object of the invention is to retain not high enough technical problem for solving the active component of Bulbus Fritillariae Cirrhosae superfine powder in prior art, a kind of preparation technology of Bulbus Fritillariae Cirrhosae superfine powder is provided.The method can farthest retain the active component in Bulbus Fritillariae Cirrhosae, and the Bulbus Fritillariae Cirrhosae superfine powder rehydration making is also greatly improved.
Above-mentioned technical purpose of the present invention is achieved by the following technical programs:
A superfine powder preparation technology, comprises the following steps:
(1) select materials: get Bulbus Fritillariae Cirrhosae and wash, remove impurity, drain;
(2) making beating: add the microcrystalline Cellulose powder of raw materials quality 10~20wt% after the preliminary pulverizing of raw material Bulbus Fritillariae Cirrhosae, then the rotation by mixer batch can makes described raw material fully mix with described microcrystalline Cellulose, obtains batch mixing; Then the water making beating that adds 0.7~0.8 times of batch mixing quality;
(3) pre-freeze: pre-freeze after making beating, pre-freeze be take and is frozen into solid as standard, and maintains the solid state that is frozen into 5~10 hours, pre-freeze temperature-8~-18 ℃; Described pre-freeze also will add the Tween 80 of serosity quality 10~15wt% and fully stir before pre-freeze;
(4) lyophilization: pre-freeze postlyophilization, cryodesiccated controlled condition is at-45~-50 ℃, 24~120 hours time, requires moisture control below 6wt% simultaneously;
(5) break micropowder: the powder agglomates obtaining after lyophilization is ground to mixing roll by vibration type micronizing and break into micropowder.
As technique scheme preferably, step (5) is played micropowder specific requirement and is, grain size of micropowder more than 95% is reached below 10 μ m.
As technique scheme preferably, the moisture content of described Bulbus Fritillariae Cirrhosae superfine powder is lower than 5%.
Chinese medicine is in traditional Preparation process process, and the effective ingredient such as vegetable protein, polysaccharide can be damaged.The present invention is by adding the rear pre-freeze of water making beating, and Bulbus Fritillariae Cirrhosae medical material is first through freezing before distillation dehydration, forms and stablizes " skeleton ", by low-temperature negative-pressure dehydrate, finally by vibration type micronizing, grinds mixing roll and is prepared into Bulbus Fritillariae Cirrhosae superfine powder.According to the feature of micronizing, when Chinese medicine carries out superfine grinding, affected many factors: first, and the various and complicated component of herbal species, not all medicine is all applicable to superfine grinding, neither powder more carefully better.Containing the medical material of armaticity, volatile ingredient, sporoderm-broken rate is high, is conducive to the abundant exposure emission and absorption of effective ingredient, but when pulverizing, the loss of volatile component can not be ignored, so what degree this class medical material need to be crushed to and need to study further; Secondly, for some active components, be macromolecular medical material, be crushed to what degree not saboteur's structure also need to investigate further, the index that some medical material that contains toxic component also will be using the stripping of toxic component as an investigation in addition.Except kind is different, also has moisture, former particle size distribution, pulverize the factors such as environment.Therefore, up to the present, with same equipment, same disintegrating process, realize the superfine grinding of same fineness, also acquire a certain degree of difficulty.Can only, according to concrete medicine, for specific requirement, carry out super-fine processing.Therefore, need to carry out the adjusting of a large amount of tests and disintegrating process and pulverizing parameter.
The present invention, in pulping process, has added microcrystalline Cellulose.Microcrystalline Cellulose is a kind of conventional medical auxiliary materials, its be present in reasonability in medicine with scientific through demonstration repeatedly, therefore using it as adjuvant, at medical angle, be at least out of question.In the present invention, the effect of microcrystalline Cellulose is not obviously traditional value as medical accessory, and it can help the making beating of raw material and the effective ingredient of protection raw material not to be destroyed in pulping process.
Because the extra interpolation of microcrystalline Cellulose has also proposed new problem for technique of the present invention, that is, during last micronizing, from the resistance of material, increase, make vibration type micronizing grind mixing roll usually overheated, and polishing effect is also undesirable.The inventor, after having used Tween 80, has solved this problem.Tween 80 is also a kind of conventional medical auxiliary agent, the same with microcrystalline Cellulose, is safe and reliable equally.The detailed directions of Tween 80 is: before pre-freeze, add the Tween 80 of serosity quality 10~15wt% and fully stir, then pre-freeze.
The Bulbus Fritillariae Cirrhosae superfine powder steady quality of preparing by the present invention, long preservation at normal temperatures, its rehydration is fabulous, the recovery that can absorb water rapidly, its color and luster, quality and fresh goods are basic identical.In addition, by In Vitro Dissolution, test, the medical material under known unit mass, Bulbus Fritillariae Cirrhosae superfine powder prepared by the inventive method is than dry Bulbus Fritillariae Cirrhosae after concocting, containing more effective ingredient.In experimentation, also find, Bulbus Fritillariae Cirrhosae superfine powder prepared by the inventive method, after inhaling a small amount of water recovery, is thick, and the Bulbus Fritillariae Cirrhosae superfine powder that employing traditional method is concocted, the water gagings such as use restore obviously deficiency of rear sliminess.Known by method of the present invention, can retain to a greater degree the active component of Bulbus Fritillariae Cirrhosae medical material.By pharmacodynamic study, find, Bulbus Fritillariae Cirrhosae superfine powder prepared by the inventive method, the drug effect of its smaller dose can be equal to the drug effect of dry Bulbus Fritillariae Cirrhosae extractum clinical medicine dose.
The present invention has following technique effect:
(1) the Bulbus Fritillariae Cirrhosae superfine powder that adopts the inventive method to prepare, can farthest retain the active component in Bulbus Fritillariae Cirrhosae;
(2) the Bulbus Fritillariae Cirrhosae superfine powder that adopts the inventive method to prepare, the drug effect of its smaller dose can be equal to the drug effect of dry Bulbus Fritillariae Cirrhosae extractum clinical medicine dose;
(3) the Bulbus Fritillariae Cirrhosae superfine powder that adopts the inventive method to prepare, steady quality, at normal temperatures long preservation;
(4) the bright Bulbus Fritillariae Cirrhosae superfine powder that adopts the inventive method to prepare, its rehydration is fabulous, the recovery that can absorb water rapidly, its color and luster, quality and fresh goods are basic identical.
Accompanying drawing explanation
Fig. 1 is imperialine reference substance canonical plotting;
Fig. 2 is the imperialine canonical plotting of making beating micropowder;
Fig. 3 is Bulbus Fritillariae Cirrhosae micropowder, coarse powder and the comparison of extractum In Vitro Dissolution.
The specific embodiment
This specific embodiment is only explanation of the invention; it is not limitation of the present invention; any change that those skilled in the art can do after having read description of the present invention, as long as within claim limited range of the present invention, all will be subject to the protection of Patent Law.
embodiment 1
A superfine powder preparation technology, comprises the following steps:
(1) select materials: get Bulbus Fritillariae Cirrhosae and wash, remove impurity, drain;
(2) making beating: add the microcrystalline Cellulose powder of raw materials quality 10wt% after the preliminary pulverizing of raw material Bulbus Fritillariae Cirrhosae, then the rotation by mixer batch can makes described raw material fully mix with described microcrystalline Cellulose, obtains batch mixing; Then the water making beating that adds 0.70 times of batch mixing quality;
(3) pre-freeze: pre-freeze after making beating, pre-freeze be take and is frozen into solid as standard, and maintains the solid state that is frozen into 5~10 hours, pre-freeze temperature-8~-18 ℃; Described pre-freeze also will add the Tween 80 of serosity quality 10wt% and fully stir before pre-freeze;
(4) lyophilization: pre-freeze postlyophilization, cryodesiccated controlled condition is at-45~-50 ℃, 24~120 hours time, requires moisture control below 6wt% simultaneously;
(5) break micropowder: the powder agglomates obtaining after lyophilization is ground to mixing roll by vibration type micronizing and break into micropowder, grain size of micropowder more than 95% is reached below 10 μ m, moisture content is lower than 5%.
embodiment 2
A superfine powder preparation technology, comprises the following steps:
(1) select materials: get Bulbus Fritillariae Cirrhosae and wash, remove impurity, drain;
(2) making beating: add the microcrystalline Cellulose powder of raw materials quality 12wt% after the preliminary pulverizing of raw material Bulbus Fritillariae Cirrhosae, then the rotation by mixer batch can makes described raw material fully mix with described microcrystalline Cellulose, obtains batch mixing; Then the water making beating that adds 0.72 times of batch mixing quality;
(3) pre-freeze: pre-freeze after making beating, pre-freeze be take and is frozen into solid as standard, and maintains the solid state that is frozen into 5~10 hours, pre-freeze temperature-8~-18 ℃; Described pre-freeze also will add the Tween 80 of serosity quality 11wt% and fully stir before pre-freeze;
(4) lyophilization: pre-freeze postlyophilization, cryodesiccated controlled condition is at-45~-50 ℃, 24~120 hours time, requires moisture control below 6wt% simultaneously;
(5) break micropowder: the powder agglomates obtaining after lyophilization is ground to mixing roll by vibration type micronizing and break into micropowder, grain size of micropowder more than 95% is reached below 10 μ m, moisture content is lower than 5%.
embodiment 3
A superfine powder preparation technology, comprises the following steps:
(1) select materials: get Bulbus Fritillariae Cirrhosae and wash, remove impurity, drain;
(2) making beating: add the microcrystalline Cellulose powder of raw materials quality 14wt% after the preliminary pulverizing of raw material Bulbus Fritillariae Cirrhosae, then the rotation by mixer batch can makes described raw material fully mix with described microcrystalline Cellulose, obtains batch mixing; Then the water making beating that adds 0.74 times of batch mixing quality;
(3) pre-freeze: pre-freeze after making beating, pre-freeze be take and is frozen into solid as standard, and maintains the solid state that is frozen into 5~10 hours, pre-freeze temperature-8~-18 ℃; Described pre-freeze also will add the Tween 80 of serosity quality 12wt% and fully stir before pre-freeze;
(4) lyophilization: pre-freeze postlyophilization, cryodesiccated controlled condition is at-45~-50 ℃, 24~120 hours time, requires moisture control below 6wt% simultaneously;
(5) break micropowder: the powder agglomates obtaining after lyophilization is ground to mixing roll by vibration type micronizing and break into micropowder, grain size of micropowder more than 95% is reached below 10 μ m, moisture content is lower than 5%.
embodiment 4
A superfine powder preparation technology, comprises the following steps:
(1) select materials: get Bulbus Fritillariae Cirrhosae and wash, remove impurity, drain;
(2) making beating: add the microcrystalline Cellulose powder of raw materials quality 16wt% after the preliminary pulverizing of raw material Bulbus Fritillariae Cirrhosae, then the rotation by mixer batch can makes described raw material fully mix with described microcrystalline Cellulose, obtains batch mixing; Then the water making beating that adds 0.76 times of batch mixing quality;
(3) pre-freeze: pre-freeze after making beating, pre-freeze be take and is frozen into solid as standard, and maintains the solid state that is frozen into 5~10 hours, pre-freeze temperature-8~-18 ℃; Described pre-freeze also will add the Tween 80 of serosity quality 13wt% and fully stir before pre-freeze;
(4) lyophilization: pre-freeze postlyophilization, cryodesiccated controlled condition is at-45~-50 ℃, 24~120 hours time, requires moisture control below 6wt% simultaneously;
(5) break micropowder: the powder agglomates obtaining after lyophilization is ground to mixing roll by vibration type micronizing and break into micropowder, grain size of micropowder more than 95% is reached below 10 μ m, moisture content is lower than 5%.
embodiment 5
A superfine powder preparation technology, comprises the following steps:
(1) select materials: get Bulbus Fritillariae Cirrhosae and wash, remove impurity, drain;
(2) making beating: add the microcrystalline Cellulose powder of raw materials quality 18wt% after the preliminary pulverizing of raw material Bulbus Fritillariae Cirrhosae, then the rotation by mixer batch can makes described raw material fully mix with described microcrystalline Cellulose, obtains batch mixing; Then the water making beating that adds 0.78 times of batch mixing quality;
(3) pre-freeze: pre-freeze after making beating, pre-freeze be take and is frozen into solid as standard, and maintains the solid state that is frozen into 5~10 hours, pre-freeze temperature-8~-18 ℃; Described pre-freeze also will add the Tween 80 of serosity quality 14wt% and fully stir before pre-freeze;
(4) lyophilization: pre-freeze postlyophilization, cryodesiccated controlled condition is at-45~-50 ℃, 24~120 hours time, requires moisture control below 6wt% simultaneously;
(5) break micropowder: the powder agglomates obtaining after lyophilization is ground to mixing roll by vibration type micronizing and break into micropowder, grain size of micropowder more than 95% is reached below 10 μ m, moisture content is lower than 5%.
embodiment 6
A superfine powder preparation technology, comprises the following steps:
(1) select materials: get Bulbus Fritillariae Cirrhosae and wash, remove impurity, drain;
(2) making beating: add the microcrystalline Cellulose powder of raw materials quality 20wt% after the preliminary pulverizing of raw material Bulbus Fritillariae Cirrhosae, then the rotation by mixer batch can makes described raw material fully mix with described microcrystalline Cellulose, obtains batch mixing; Then the water making beating that adds 0.80 times of batch mixing quality;
(3) pre-freeze: pre-freeze after making beating, pre-freeze be take and is frozen into solid as standard, and maintains the solid state that is frozen into 5~10 hours, pre-freeze temperature-8~-18 ℃; Described pre-freeze also will add the Tween 80 of serosity quality 15wt% and fully stir before pre-freeze;
(4) lyophilization: pre-freeze postlyophilization, cryodesiccated controlled condition is at-45~-50 ℃, 24~120 hours time, requires moisture control below 6wt% simultaneously;
(5) break micropowder: the powder agglomates obtaining after lyophilization is ground to mixing roll by vibration type micronizing and break into micropowder, grain size of micropowder more than 95% is reached below 10 μ m, moisture content is lower than 5%.
ultraviolet content method and interpretation of result
The preparation of reference substance solution
Get imperialine reference substance 0.00301g, accurately weighed, add chloroform 15ml and make every 1ml containing the solution of 0.2mg, both.
The preparation of standard curve
Precision measures reference substance solution 0.1ml, 0.2ml, 0.4ml, 0.6ml, 1.0ml, put in 25ml tool plug test tube, add respectively chloroform to 10.0ml, precision adds water 5ml, precision adds 0.05% bromocresol green buffer and (gets bromocresol green 0.05g again, with 0.2mol/ L sodium hydroxide solution 6ml, make to dissolve, add potassium dihydrogen phosphate 1g, add water and make to dissolve and be diluted to 100ml, obtain) 2ml, close plug, violent jolting, is transferred in separatory funnel, places 30 minutes.Get chloroform liquid, with dry filter paper, filter, get subsequent filtrate, take corresponding reagent as blank, according to ultraviolet visible spectrophotometry (appendix V A), at the wavelength place of 415nm, measure absorbance, take absorbance as vertical coordinate, concentration is abscissa, drawing standard curve.
Figure 2013104958867100002DEST_PATH_IMAGE001
Algoscopy
The about 2g of sample thief, accurately weighed, put in tool plug conical flask, add strong ammonia solution 3ml, infiltrate 1 hour, add chloroform-methanol (4:1) mixed solution 40m1, putting 80 ℃ of heating in water bath refluxes 2 hours, let cool, filter, filtrate is put in 50ml volumetric flask, with appropriate chloroform-methanol (4:1) mixed solution, wash medicinal residues 2-3 time, washing liquid is incorporated in same volumetric flask, add chloroform-methanol (4:1) mixed solution and be settled to scale, shake up precision and measure 2-5ml, put in 25ml tool plug test tube, evaporate to dryness in water-bath, precision adds chloroform 10ml to make to dissolve, method under the preparation of sighting target directrix curve, from " precision adds water 5ml ", measure absorbance in accordance with the law, the weight (mg) of reading imperialine in need testing solution from standard curve, calculate, both.
methodological study
Precision test
Precision measures reference substance solution 0.6ml, puts in 25ml tool plug test tube, and the method under the preparation of sighting target directrix curve from " adding chloroform to 10ml ", is measured absorbance in accordance with the law, calculates relative standard deviation (RSD), to investigate the precision of instrument.
Figure 95115DEST_PATH_IMAGE002
Result shows that imperialine reference substance is 0.45% in the relative standard deviation (RSD) of 415nm place absorbance, shows that the method precision is good.
stability test
The about 2g of Bulbus Fritillariae Cirrhosae making beating micropowder, accurately weighed, according to the preparation method of test sample under 2.2.1.3 algoscopy, in accordance with the law at 0min, 5min, 10min, 15min, 20min, 25min measures absorbance, calculates relative standard deviation.
Figure 874852DEST_PATH_IMAGE003
Result show sample stability relative standard deviation (RSD) is 1.53%, shows that this sample is good at 25min internal stability.
repeatability experiment
Get 6 batches of samples according to the preparation method of test sample under algoscopy, measure absorbance in accordance with the law, and calculate its relative standard deviation.
Figure 270062DEST_PATH_IMAGE004
Result shows that 6 batches of sample repeatability relative standard deviations (RSD) are 2.58%, and between each batch, diversity is less.
average recovery
Get the portion in repeatability sample, absorbance is surveyed, and content is known.Then from this part of test sample processing procedure standardize solution above to that step in 50ml measuring bottle, precision pipettes six parts, every part of 5ml respectively to six test tube, add appropriate imperialine reference substance, preparation method under 2.2.1.3 algoscopy item, from " evaporate to dryness in water-bath ", measure absorbance, calculate recovery rate in accordance with the law.
Figure 22117DEST_PATH_IMAGE005
Result show sample average recovery is all between 95%-105%, and meansigma methods is 102.0%, and relative standard deviation is 2.37%, process stabilizing.
the assay of imperialine
The preparation method drawing standard curve of secundum legem curve.Get respectively the sample micropowder under different disposal method, by preparation method under algoscopy, measure absorbance in accordance with the law, the dry product of pressing Bulbus Fritillariae Cirrhosae micropowder calculates the content of imperialine.
  
Figure 2013104958867100002DEST_PATH_IMAGE003
Result demonstration, Bulbus Fritillariae Cirrhosae micropowder imperialine content is higher than coarse powder, and making beating powder content is again higher than drying and cold dry micropowder.
bulbus Fritillariae Cirrhosae micro powder granule, common flour, the test of extractum dissolution in vitro
Get respectively Bulbus Fritillariae Cirrhosae making beating micropowder 10g, drop in 500ml dissolution medium; Bulbus Fritillariae Cirrhosae coarse powder 10g drops in 500ml dissolution medium; Bulbus Fritillariae Cirrhosae decoction pieces 10g, adding distil water 400ml, at 150 ℃, reflux is two hours, centrifugal filtration, filtrate decoction is settled to 100ml, drops in 400ml dissolution medium.According to Chinese Pharmacopoeia (version appendix in 2010) dissolution method slurry method, rotating speed 100r/min, temperature is (37 scholar 0.5) ℃, respectively at 5,15,30,45,60,90min samples 5mL, simultaneously to the water that supplements uniform temp and volume in stripping rotor.The centrifugal rear film of crossing of sample taking out, the filtrate precision of each sample pipettes 1ml, add chloroform 10ml, distilled water 5ml, 0.05% bromocresol green solution 2ml, violent jolting, be transferred in paging funnel standing 15 minutes, get chloroform layer, then cross leaching subsequent filtrate, at 415nm wavelength place, measure absorbance.Sample size, in the average content of Bulbus Fritillariae Cirrhosae micropowder quality standard, is 0.0541%, calculates this In Vitro Dissolution of various kinds percentage rate.
Figure 746731DEST_PATH_IMAGE008
Dissolution in vitro experimental result shows, in 5min, Bulbus Fritillariae Cirrhosae micropowder dissolution rate in vitro, faster than common flour and extractum, is accumulated stripping quantity also higher in 90min, meets the rapid dissolution characteristic of effective ingredient after micro mist cell breaking cellular wall.

Claims (3)

1. a Bulbus Fritillariae Cirrhosae superfine powder preparation technology, comprises the following steps:
(1) select materials: get Bulbus Fritillariae Cirrhosae and wash, remove impurity, drain;
(2) making beating: add the microcrystalline Cellulose powder of raw materials quality 10~20wt% after the preliminary pulverizing of raw material Bulbus Fritillariae Cirrhosae, then the rotation by mixer batch can makes described raw material fully mix with described microcrystalline Cellulose, obtains batch mixing; Then the water making beating that adds 0.7~0.8 times of batch mixing quality;
(3) pre-freeze: pre-freeze after making beating, pre-freeze be take and is frozen into solid as standard, and maintains the solid state that is frozen into 5~10 hours, pre-freeze temperature-8~-18 ℃; Described pre-freeze also will add the Tween 80 of serosity quality 10~15wt% and fully stir before pre-freeze;
(4) lyophilization: pre-freeze postlyophilization, cryodesiccated controlled condition is at-45~-50 ℃, 24~120 hours time, requires moisture control below 6wt% simultaneously;
(5) break micropowder: the powder agglomates obtaining after lyophilization is ground to mixing roll by vibration type micronizing and break into micropowder.
2. a kind of Bulbus Fritillariae Cirrhosae superfine powder preparation technology according to claim 1, is characterized in that: step (5) is played micropowder specific requirement and is, grain size of micropowder more than 95% is reached below 10 μ m.
3. a kind of Bulbus Fritillariae Cirrhosae superfine powder preparation technology according to claim 1 and 2, is characterized in that: the moisture content of described Bulbus Fritillariae Cirrhosae superfine powder is lower than 5%.
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CN104226442A (en) * 2014-09-03 2014-12-24 肖平安 As-cast chilling split-crushing method of rare earth ferrosiliconmagnesium alloy nodulizing agent
CN105412533A (en) * 2015-11-25 2016-03-23 苏州普罗达生物科技有限公司 Fritillaria-praewalskii-maxim-ex-Batal ultramicro wall-breaking smashing method
CN108014258A (en) * 2016-10-31 2018-05-11 四川德仁堂中药科技股份有限公司 A kind of concocting method for improving tendril-leaved fritillary bulb powder drug effect and products thereof and purposes
CN110123938A (en) * 2019-05-30 2019-08-16 胡爱娣 A kind of activity bulbus fritillariae cirrhosae pure powder tablet preparation method

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104226442A (en) * 2014-09-03 2014-12-24 肖平安 As-cast chilling split-crushing method of rare earth ferrosiliconmagnesium alloy nodulizing agent
CN105412533A (en) * 2015-11-25 2016-03-23 苏州普罗达生物科技有限公司 Fritillaria-praewalskii-maxim-ex-Batal ultramicro wall-breaking smashing method
CN108014258A (en) * 2016-10-31 2018-05-11 四川德仁堂中药科技股份有限公司 A kind of concocting method for improving tendril-leaved fritillary bulb powder drug effect and products thereof and purposes
CN110123938A (en) * 2019-05-30 2019-08-16 胡爱娣 A kind of activity bulbus fritillariae cirrhosae pure powder tablet preparation method

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