CN111307673A - Method for testing particle size of fluticasone bulk drug - Google Patents
Method for testing particle size of fluticasone bulk drug Download PDFInfo
- Publication number
- CN111307673A CN111307673A CN202010240869.9A CN202010240869A CN111307673A CN 111307673 A CN111307673 A CN 111307673A CN 202010240869 A CN202010240869 A CN 202010240869A CN 111307673 A CN111307673 A CN 111307673A
- Authority
- CN
- China
- Prior art keywords
- fluticasone
- particle size
- particles
- test method
- bulk drug
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000002245 particle Substances 0.000 title claims abstract description 113
- 238000000034 method Methods 0.000 title claims abstract description 36
- MGNNYOODZCAHBA-GQKYHHCASA-N fluticasone Chemical compound C1([C@@H](F)C2)=CC(=O)C=C[C@]1(C)[C@]1(F)[C@@H]2[C@@H]2C[C@@H](C)[C@@](C(=O)SCF)(O)[C@@]2(C)C[C@@H]1O MGNNYOODZCAHBA-GQKYHHCASA-N 0.000 title claims abstract description 34
- 229960002714 fluticasone Drugs 0.000 title claims abstract description 33
- 239000003814 drug Substances 0.000 title claims abstract description 28
- 229940079593 drug Drugs 0.000 title claims abstract description 21
- 238000012360 testing method Methods 0.000 title claims abstract description 8
- 230000008014 freezing Effects 0.000 claims description 21
- 238000007710 freezing Methods 0.000 claims description 21
- 229960000289 fluticasone propionate Drugs 0.000 claims description 14
- WMWTYOKRWGGJOA-CENSZEJFSA-N fluticasone propionate Chemical compound C1([C@@H](F)C2)=CC(=O)C=C[C@]1(C)[C@]1(F)[C@@H]2[C@@H]2C[C@@H](C)[C@@](C(=O)SCF)(OC(=O)CC)[C@@]2(C)C[C@@H]1O WMWTYOKRWGGJOA-CENSZEJFSA-N 0.000 claims description 14
- 238000005469 granulation Methods 0.000 claims description 7
- 230000003179 granulation Effects 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 5
- 238000001125 extrusion Methods 0.000 claims description 3
- 229960001469 fluticasone furoate Drugs 0.000 claims description 2
- XTULMSXFIHGYFS-VLSRWLAYSA-N fluticasone furoate Chemical compound O([C@]1([C@@]2(C)C[C@H](O)[C@]3(F)[C@@]4(C)C=CC(=O)C=C4[C@@H](F)C[C@H]3[C@@H]2C[C@H]1C)C(=O)SCF)C(=O)C1=CC=CO1 XTULMSXFIHGYFS-VLSRWLAYSA-N 0.000 claims description 2
- 238000005563 spheronization Methods 0.000 claims description 2
- 238000010998 test method Methods 0.000 claims 9
- 239000008186 active pharmaceutical agent Substances 0.000 claims 3
- 229940088679 drug related substance Drugs 0.000 claims 3
- 238000005259 measurement Methods 0.000 abstract description 34
- 239000002994 raw material Substances 0.000 abstract description 5
- 239000000463 material Substances 0.000 description 17
- 238000009826 distribution Methods 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 7
- 238000001033 granulometry Methods 0.000 description 4
- 238000007561 laser diffraction method Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 210000004072 lung Anatomy 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000001186 cumulative effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000011361 granulated particle Substances 0.000 description 2
- 238000000691 measurement method Methods 0.000 description 2
- 238000003908 quality control method Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 230000005653 Brownian motion process Effects 0.000 description 1
- 208000006545 Chronic Obstructive Pulmonary Disease Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 208000006673 asthma Diseases 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000005537 brownian motion Methods 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007012 clinical effect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003862 glucocorticoid Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 210000003300 oropharynx Anatomy 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 229940098458 powder spray Drugs 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/02—Investigating particle size or size distribution
- G01N15/0205—Investigating particle size or size distribution by optical means
- G01N15/0211—Investigating a scatter or diffraction pattern
Landscapes
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Steroid Compounds (AREA)
Abstract
The invention provides a method for testing the particle size of a fluticasone bulk drug, which comprises the following steps: (a) granulating the fluticasone bulk drug to form uniform spherical small particles; (b) the particle size of the uniform spherical small particles obtained in step (a) was measured using a laser particle sizer. The invention solves the problem that the traditional dry method has larger fluctuation caused by larger viscosity of the raw material medicine in the process of determining the particle size of the fluticasone, and provides the method for determining the particle size of the fluticasone with accurate measurement result and high reproducibility.
Description
Technical Field
The invention belongs to the technical field of pharmaceutical preparations, and particularly relates to a method for testing particle size of a fluticasone bulk drug.
Background
It is well known to those skilled in the art that the lung has a particular physiological configuration and that particles can enter the lung through the respiratory tract, which acts as a particle screening system. When the aerodynamic diameter of the particles is larger than 5 μm, the particles have large inertia and high deposition rate at the oropharynx; when the aerodynamic diameter of the particles is in the range of 1-5 mu m, the particles can reach the peripheral air passage of the most effective absorption part; when the aerodynamic diameter of the particles is less than 0.5 μm, the particles will not deposit and will continue to travel with the brownian motion and finally be exhaled out.
The inhalation powder spray refers to a preparation which is prepared by actively inhaling atomized medicine into the lung by a patient by adopting a special dry powder inhalation device in a capsule, vesicle or multi-dose storage form of micronized medicine or carriers. In the process of preparing the preparation, a skilled person usually micronizes the material to obtain a material with a smaller particle size, but the finer the particle size of the material, the stronger the adhesion and the higher the requirement for detection.
The laser diffraction particle analyzer is an on-line measurement and analysis tool integrating laser, electron, photoelectric conversion and other technologies. The laser diffraction method can measure the particle size of solid particles and the particle size of liquid drops. The laser diffraction method has the advantages of simple operation, rapid process, good repeatability and the like, and is an indispensable measurement method for researching and developing prescription of inhalation preparations gradually at present.
Fluticasone is a very important glucocorticoid drug in an inhalation preparation, and is mainly suitable for asthma and chronic obstructive pulmonary disease. The crude drug of fluticasone propionate is relatively viscous and not easy to disperse, so that the particle size measurement is one of the key limiting factors for the development of the fluticasone propionate. The furoic acid fluticasone is a new-generation fluticasone derivative, has stronger anti-inflammatory effect and more obvious clinical effect, but still has larger viscosity, and still has the defect of difficult dispersion when the particle size is measured, so the particle size measurement is also a technical barrier for the research and development of the furoic acid fluticasone.
Because the solid powder of the fluticasone micro-powder bulk drug has higher adhesiveness and is easy to agglomerate, if the particle size is measured by using a dry laser diffraction method, the situation that the fluticasone is difficult to uniformly disperse in the air can occur. In actual operation, the fluctuation of the measurement results of the particle size and the particle size distribution of the fluticasone is large, and the situation that the nozzle of a laser diffraction particle size analyzer is easily blocked by the powder of the raw material medicine is found, so that accurate and stable data cannot be obtained when the particle size of the fluticasone medicine is directly measured by using a dry laser diffraction method. In actual research, the particle size of the raw material drug cannot be effectively evaluated, which is not beneficial to the research of prescription particle size screening. In industrial production, the quality control of the medicine is not facilitated.
The prior art does not report a method for effectively measuring the particle size or the particle size distribution of fluticasone bulk drug. Therefore, it is urgently needed to develop a method for determining the particle size or the particle size distribution of the fluticasone bulk drug with accuracy and high reproducibility, which is very important for particle size screening and quality control of the fluticasone bulk drug, and simultaneously can ensure the stability of the related inhalation preparation raw materials and accelerate the research and development process.
Disclosure of Invention
In order to overcome the defects of the prior art and meet the requirements of the field, the invention provides a method for testing the particle size of a fluticasone bulk drug.
The purpose of the invention is realized by the following technical scheme:
the invention provides a method for testing the particle size of a fluticasone bulk drug, which comprises the following steps:
(a) granulating the fluticasone bulk drug to form uniform spherical small particles;
(b) and (b) measuring the particle size of the uniform spherical small particles obtained in the step (a) by using a laser particle size analyzer (also called a laser scattering diffraction particle size analyzer, wherein the laser is scattered by particles, the scattered light is interfered with each other to form a diffraction spectrogram, and then the particle size distribution is calculated according to a theoretical model).
Preferably, the fluticasone bulk drug is fluticasone propionate or fluticasone furoate.
Preferably, the fluticasone bulk drug is solid powder.
Preferably, the fluticasone bulk drug is subjected to a pre-freezing treatment prior to granulation in step (a).
Preferably, in the pre-freezing treatment, the freezing time is at least 0.5 hour, preferably 0.5 to 100 hours, and more preferably 20 to 100 hours.
Preferably, in the pre-freezing treatment, the freezing temperature is 0 ℃ to-50 ℃, preferably 0 ℃ to-30 ℃, and more preferably 0 ℃ to-20 ℃.
Preferably, the fluticasone bulk drug is used within 1h, preferably within 0.5h after pre-freeze treatment (i.e. for granulation).
Preferably, in step (a), the diameter of the spherical small particles is 60-1200 μm, preferably 100-300 μm.
Preferably, in step (a), the granulation method is an extrusion spheronization method, i.e. the material is passed through a hole or a sieve with a certain diameter by extrusion and then rolled on a container to form small granules with the diameter meeting the requirement. For example, the material is extruded through a screen and rounded in a vibrating screen machine to produce small particles of desired particle diameter.
Preferably, in step (b), the shade is from 0.5% to 8.0%, preferably from 2.0% to 3.0%.
Preferably, in step (b) the pressure is measured in the range of from 2bar to 5bar, preferably from 4bar to 5 bar.
In the present invention, the detected particle diameter may be represented as D10、D50、D90Etc. D10、D50、D90The equivalent diameters of the largest particles in the cumulative distribution of 10%, 50%, 90% of the distribution curve, respectively.
Compared with the prior art, the application has the following beneficial technical effects:
the invention solves the problem that the traditional dry method has larger fluctuation caused by larger viscosity of the raw material medicine in the process of determining the particle size of the fluticasone, and provides the method for determining the particle size of the fluticasone with accurate measurement result and high reproducibility.
Drawings
FIG. 1 the samples of example 1.1 were tested for the results of the 6 sets of data.
FIG. 2 the samples of example 1.2 were tested for the results of the 6 sets of data.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The experimental procedures, in which specific conditions are not noted in the following examples, are generally carried out under conventional conditions or under conditions recommended by the manufacturers.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In addition, any methods and materials similar or equivalent to those described herein can be used in the methods of the present invention. The preferred embodiments and materials described herein are intended to be exemplary only.
In the present invention, D10Particle diameter, D50Particle diameter, D90The particle diameters are equivalent diameters of the largest particles in the cumulative distributions of 10%, 50%, and 90% in the distribution curves, respectively.
Reference to the chinese pharmacopoeia of the 2015 edition specifies in the 0982 particle size and particle size distribution assay: the "standard particles" having a particle diameter of less than 10 μm were measured for D50RSD of the parallel measurement is less than 6%; d10And D90The RSD of the parallel determination of (1) is not more than 10% as a reference standard.
Example 1
1.1 the fluticasone propionate solid powder is put into a freezer, the temperature is set to-20 ℃ and the time is 20 h. After the freezing, the operation is carried out for 0.5h, the materials are extruded to pass through a 100-mesh screen and are rounded in a rounding machine, and the diameter of the particles is 150-200 mu m; the particles were subjected to dry laser granulometry (RODOS) at a measurement pressure of 4bar and a light shade of 2.0-3.0%, and samples were tested to obtain 6 sets of data, as shown in fig. 1.
1.2 the fluticasone propionate is not granulated, and is directly measured by a dry laser particle size method (RODOS), the measurement pressure is 4bar, the light shading degree is 2.0-3.0 percent, and 6 groups of data of sample test are shown in figure 2.
1.3 the fluticasone propionate is put into a refrigerator, the temperature is set to-20 ℃ and the time is 10 min. After the freezing, the operation is carried out for 0.5h, the materials are extruded to pass through a 100-mesh screen and are rounded in a rounding machine, and the diameter of the particles is 80-600 mu m; the particles were subjected to dry laser granulometry (RODOS) at a pressure of 4bar with a opacity of 2.0-3.0%, and 6 sets of data were tested on the samples.
1.4 the fluticasone propionate is put into a refrigerator, the temperature is set to-20 ℃ and the time is 20 h. After the freezing, the operation is carried out for 2h, the material is extruded to pass through a 100-mesh screen and is rounded in a rounding machine, and the diameter of the particles is 40-500 mu m; the particles were subjected to dry laser granulometry (RODOS) at a pressure of 4bar with a opacity of 2.0-3.0%, and 6 sets of data were tested on the samples.
1.5 the fluticasone propionate is put into a refrigerator, the temperature is set to-40 ℃ and the time is 20 h. After the freezing, the operation is carried out for 0.5h, the materials are extruded to pass through a 100-mesh screen and are rounded in a rounding machine, and the diameter of the particles is 100-400 mu m; the particles were subjected to dry laser granulometry (RODOS) at a pressure of 4bar with a opacity of 2.0-3.0%, and 6 sets of data were tested on the samples.
The results of the sample measurements for examples 1.1-1.5 are detailed in Table 1.
TABLE 1 results of measurements on samples of examples 1.1 to 1.5
D measured by the method of the invention by comparing the results of the experiments in example 1.1 with those in example 1.210，D50And D90The RSD of (A) is less than 1.5%, and stable data can be obtained. Using conventional measurement methods, D10，D50And D90The RSD of the particles is more than 10 percent, the particle size measurement fluctuation is large, and stable and reliable data cannot be obtained. In comparison with example 1.1 and 1.3, the refrigeration time is insufficient, so that the particle size range of the granulated particles is large, and therefore, the RSD result of laser particle size measurement is improved to a certain extent. In comparison between example 1.1 and example 1.4, the results of RSD measurement were higher because the granulation was not satisfactory and the range of particle size was large because the treatment was not performed immediately after the completion of freezing. Example 1.1 compares with 1.5, the low freezing temperature makes the range of the particle size of the granulated particles larger, and the result of measuring RSD is higher.
Example 2
2.1 the furoic acid fluticasone is put into a freezer, the temperature is set to-5 ℃ and the time is 48 h. And after the freezing time is finished, operating for 0.5h, extruding the material through a 40-mesh screen, and rounding in a vibrating screen machine, wherein the diameter of the particles is 400-800 mu m. The particles are measured by a dry laser particle size method, the measurement pressure is 2bar, the light shading degree is 2.0-3.0%, and 6 groups of data are tested by a sample.
2.2 the particles obtained in 2.1 are measured by a dry laser particle size method, the measurement pressure is 3bar, the light shading degree is 2.0-3.0%, and 6 groups of data are tested by a sample.
2.3 the particles obtained from 2.1 are measured by a dry laser particle size method, the measurement pressure is 4bar, the light shading degree is 2.0-3.0%, and 6 groups of data are tested by a sample.
2.4 the particles obtained from 2.1 are measured by a dry laser particle size method, the measurement pressure is 5bar, the light shading degree is 2.0-3.0%, and 6 groups of data are tested by a sample.
2.5 the particles obtained by the preparation of the 2.1 are measured by a dry laser particle size method, the measurement pressure is 4bar, the light shading degree is 0.5-2.0%, and 6 groups of data are tested by a sample.
2.6 the particles obtained by the preparation of the 2.1 are subjected to dry laser particle size measurement, the measurement pressure is 4bar, the light shading degree is 4.0-6.0%, and 6 groups of data are tested by a sample.
The results of the sample measurements for examples 2.1-2.6 are detailed in Table 2.
TABLE 2 results of sample measurements for examples 2.1-2.6
From the experimental data of examples 2.1 to 2.6, it can be found that among the measurement parameters, when the measurement pressure is 4bar to 5bar and the light shielding degree is 2.0% to 3.0%, the RSD of the measurement result is the smallest and the reproducibility of the measurement result is the highest.
Example 3
3.1 the fluticasone propionate is placed in a freezer, the temperature is set to-10 ℃ and the time is 0.5 h. After the freezing is finished for 10min, extruding the material through a 250-mesh screen, and rounding in a vibrating screen machine, wherein the diameter of the particles is 70-100 mu m; the particles are measured by a dry laser particle size method, the measurement pressure is 4bar, the light shading degree is 2.0-3.0%, and 6 groups of data are tested by a sample.
3.2 the fluticasone propionate is put into a freezer, the temperature is set to-10 ℃ and the time is 0.5 h. After the freezing is finished for 10min, extruding the material through a 110-mesh screen, and rounding in a vibrating screen machine, wherein the diameter of the particles is 120-180 mu m; the particles are measured by a dry laser particle size method, the measurement pressure is 4bar, the light shading degree is 2.0-3.0%, and 6 groups of data are tested by a sample.
3.3 the fluticasone propionate is put into a freezer, the temperature is set to-10 ℃ and the time is 0.5 h. After the freezing is finished for 10min, extruding the material through a 80-mesh screen, and rounding in a vibrating screen machine, wherein the diameter of the particles is 190-270 mu m; the particles are measured by a dry laser particle size method, the measurement pressure is 4bar, the light shading degree is 2.0-3.0%, and 6 groups of data are tested by a sample.
3.4 the fluticasone propionate is placed in a freezer, the temperature is set to-10 ℃ and the time is 0.5 h. After the freezing is finished for 10min, extruding the material through a 40-mesh screen, and rounding in a vibrating screen machine, wherein the diameter of the particles is 350-680 mu m; the particles are measured by a dry laser particle size method, the measurement pressure is 4bar, the light shading degree is 2-3%, and 6 groups of data are tested by a sample.
3.5 the fluticasone propionate is placed in a freezer, the temperature is set to-10 ℃ and the time is 0.5 h. After the freezing is finished for 10min, extruding the material through a 30-mesh screen, and rounding in a vibrating screen machine, wherein the diameter of the particles is 850-1200 mu m; the particles are measured by a dry laser particle size method, the measurement pressure is 4bar, the light shading degree is 2.0-3.0%, and 6 groups of data are tested by a sample.
The results of the sample measurements for examples 3.1-3.5 are detailed in Table 3.
TABLE 3 results of measurements on samples of examples 3.1 to 3.5
By using the experimental data of examples 3.1-3.5, it can be found that in step (b), the RSD of the measured result is the minimum, and the measured result is accurate and has high reproducibility when the diameter of the granulation particle is 100-300 μm.
Claims (10)
1. A method for testing the particle size of a fluticasone bulk drug comprises the following steps:
(a) granulating the fluticasone bulk drug to form uniform spherical small particles;
(b) the particle size of the uniform spherical small particles obtained in step (a) was measured using a laser particle sizer.
2. The test method according to claim 1, wherein the fluticasone bulk drug is fluticasone propionate or fluticasone furoate.
3. The test method according to claim 1 or 2, wherein the fluticasone drug substance is a solid powder.
4. The test method according to any one of claims 1 to 3, wherein the fluticasone drug substance is pre-frozen prior to granulation in step (a).
5. The test method according to claim 4, wherein the pre-freezing treatment is performed for a freezing time of at least 0.5 hours, preferably 0.5 to 100 hours, more preferably 20 to 100 hours.
6. The test method according to claim 4, wherein the freezing temperature in the pre-freezing treatment is 0 ℃ to-50 ℃, preferably 0 ℃ to-30 ℃, and more preferably 0 ℃ to-20 ℃.
7. The test method according to claim 4, wherein the fluticasone drug substance is used within 1h, preferably within 0.5h, of pre-freeze treatment.
8. The test method according to any one of claims 1 to 7, wherein in step (a), the diameter of the spherical small particles is 60-1500 μm, preferably 100-300 μm.
9. The test method according to any one of claims 1 to 8, wherein in step (a), the granulation process is an extrusion spheronization process.
10. The test method according to any one of claims 1 to 9, wherein in step (b) the opacity is 0.5% -8.0%, preferably 2.0% -3.0%;
preferably, in step (b) the pressure is measured in the range of from 2bar to 5bar, preferably from 4bar to 5 bar.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010240869.9A CN111307673B (en) | 2020-03-31 | 2020-03-31 | Method for testing particle size of fluticasone crude drug |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010240869.9A CN111307673B (en) | 2020-03-31 | 2020-03-31 | Method for testing particle size of fluticasone crude drug |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111307673A true CN111307673A (en) | 2020-06-19 |
| CN111307673B CN111307673B (en) | 2023-06-27 |
Family
ID=71151682
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010240869.9A Active CN111307673B (en) | 2020-03-31 | 2020-03-31 | Method for testing particle size of fluticasone crude drug |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111307673B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114112814A (en) * | 2021-11-24 | 2022-03-01 | 上海方予健康医药科技有限公司 | Method for testing cascade impactor level cut-off diameter and application |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102949379A (en) * | 2012-11-14 | 2013-03-06 | 中山大学 | Netilmicin sulfate inhalation powder and preparation method thereof |
| CN104435743A (en) * | 2014-06-10 | 2015-03-25 | 武义寿仙谷中药饮片有限公司 | Method for preparing dendrobium officinale super micropowder |
| CN104812377A (en) * | 2012-11-20 | 2015-07-29 | 耶萨利斯制药有限公司 | Method for increasing the particle size of crystalline active micro-particles |
| CN108066329A (en) * | 2016-11-11 | 2018-05-25 | 江苏恒瑞医药股份有限公司 | A kind of preparation method of the particle of sucking fluticasone or derivatives thereof |
| CN109115661A (en) * | 2018-09-27 | 2019-01-01 | 湖北省宏源药业科技股份有限公司 | A method of for measuring azithromycin drug partial size and size distribution |
| WO2019067708A1 (en) * | 2017-09-27 | 2019-04-04 | Teva Branded Pharmaceutical Products R&D, Inc. | Method for particle size reduction |
| CN110369052A (en) * | 2019-08-06 | 2019-10-25 | 陕西工业职业技术学院 | A kind of Chinese medicine System of Ultra Thin Power Rubbing and its operating method |
-
2020
- 2020-03-31 CN CN202010240869.9A patent/CN111307673B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102949379A (en) * | 2012-11-14 | 2013-03-06 | 中山大学 | Netilmicin sulfate inhalation powder and preparation method thereof |
| CN104812377A (en) * | 2012-11-20 | 2015-07-29 | 耶萨利斯制药有限公司 | Method for increasing the particle size of crystalline active micro-particles |
| CN104435743A (en) * | 2014-06-10 | 2015-03-25 | 武义寿仙谷中药饮片有限公司 | Method for preparing dendrobium officinale super micropowder |
| CN108066329A (en) * | 2016-11-11 | 2018-05-25 | 江苏恒瑞医药股份有限公司 | A kind of preparation method of the particle of sucking fluticasone or derivatives thereof |
| WO2019067708A1 (en) * | 2017-09-27 | 2019-04-04 | Teva Branded Pharmaceutical Products R&D, Inc. | Method for particle size reduction |
| CN109115661A (en) * | 2018-09-27 | 2019-01-01 | 湖北省宏源药业科技股份有限公司 | A method of for measuring azithromycin drug partial size and size distribution |
| CN110369052A (en) * | 2019-08-06 | 2019-10-25 | 陕西工业职业技术学院 | A kind of Chinese medicine System of Ultra Thin Power Rubbing and its operating method |
Non-Patent Citations (2)
| Title |
|---|
| 袁华: "丙酸氟替卡松鼻喷剂处方工艺研究", 《中国优秀博硕士学位论文全文数据库(硕士) 工程科技Ⅰ辑》 * |
| 陆彬: "《药物新剂型与新技术》", 31 May 2005, 人民卫生出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114112814A (en) * | 2021-11-24 | 2022-03-01 | 上海方予健康医药科技有限公司 | Method for testing cascade impactor level cut-off diameter and application |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111307673B (en) | 2023-06-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Telko et al. | Dry powder inhaler formulation | |
| DE60030721T2 (en) | SMOOTH POWDER PARTICLE FOR USE IN INHALATION THERAPY | |
| CN105338960B (en) | For sucking the dry powder formulations comprising anticholinergic drug, corticosteroid and beta-adrenergic medicine of application | |
| TWI530301B (en) | Process for providing particles with reduced electrostatic charges | |
| Adi et al. | The influence of drug morphology on aerosolisation efficiency of dry powder inhaler formulations | |
| Pilcer et al. | Correlations between cascade impactor analysis and laser diffraction techniques for the determination of the particle size of aerosolised powder formulations | |
| CN108289962B (en) | Method for preparing dry powder formulations comprising anticholinergics, corticosteroids and beta-adrenergic agents | |
| Kaialy et al. | Improved aerosolization performance of salbutamol sulfate formulated with lactose crystallized from binary mixtures of ethanol—acetone | |
| CN111307673B (en) | Method for testing particle size of fluticasone crude drug | |
| EP3151812B1 (en) | Inhalation particles comprising a combination of an anticholinergic, a corticosteroid and a beta-adrenergic | |
| Kaialy et al. | Treating mannitol in a saturated solution of mannitol: a novel approach to modify mannitol crystals for improved drug delivery to the lungs | |
| CN113654956A (en) | Method for determining particle size and particle size distribution of amoxicillin bulk drug | |
| US20110097409A1 (en) | Particles comprising a salt of 8-hydroxy-2-[[(1r)-2-(4-methoxyphenyl)-1-methylethyl]amino]ethyl]-2(1h)-quinolinone having improved adhesion properties for powder formulations for inhalation | |
| Djokić et al. | A study of jet-milling and spray-drying process for the physicochemical and aerodynamic dispersion properties of amiloride HCl | |
| CN111610261B (en) | Method for screening an aerosolization device suitable for use with beta 2 receptor agonists | |
| Babenko et al. | 1H NMR quantification of spray dried and spray freeze-dried saccharide carriers in dry powder inhaler formulations | |
| Borowski et al. | Selecting lactose for a capsule-based dry powder inhaler | |
| Alaboud | In-vitro inhalation performance for formoterol dry powder and metred dose inhalers. In-vitro characteristics of the emitted dose from the formoterol dry powder and metred dose inhalers to identify the influence of inhalation flow, inhalation volume and the number of inhalation per dose. | |
| CN109953965A (en) | A kind of pharmaceutical composition containing tartaric acid Mo Fanselin | |
| CN106551919B (en) | Novel inhalation formulations | |
| Kwok et al. | Solid state testing of inhaled formulations | |
| Parisini | Improved Aerosol Deposition Profiles from Dry Powder Inhalers | |
| Boekestein et al. | Uniform and reproducible delivery of albuterol from a variety of lactose powder blends using the Oriel active dispersion platform | |
| Mönckedieck | Particle-particle interactions between tailored mannitol carrier particles and drug particles for inhalation | |
| Åslund | Investigation of mixing time and relative concentration effects in adhesive mixtures for drug inhalation |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |