CN115343198A - Particle size determination method for dapagliflozin bulk drug - Google Patents
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- 239000002245 particle Substances 0.000 title claims abstract description 93
- 239000003814 drug Substances 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 47
- JVHXJTBJCFBINQ-ADAARDCZSA-N Dapagliflozin Chemical compound C1=CC(OCC)=CC=C1CC1=CC([C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)=CC=C1Cl JVHXJTBJCFBINQ-ADAARDCZSA-N 0.000 title claims abstract description 40
- 229960003834 dapagliflozin Drugs 0.000 title claims abstract description 40
- 229940079593 drug Drugs 0.000 title claims abstract description 35
- 239000002994 raw material Substances 0.000 claims abstract description 24
- 239000006185 dispersion Substances 0.000 claims abstract description 19
- 238000002347 injection Methods 0.000 claims abstract description 19
- 239000007924 injection Substances 0.000 claims abstract description 19
- 238000005259 measurement Methods 0.000 claims description 24
- GOADIQFWSVMMRJ-UPGAGZFNSA-N dapagliflozin propanediol monohydrate Chemical compound O.C[C@H](O)CO.C1=CC(OCC)=CC=C1CC1=CC([C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)=CC=C1Cl GOADIQFWSVMMRJ-UPGAGZFNSA-N 0.000 claims description 8
- 230000000052 comparative effect Effects 0.000 description 13
- 238000005303 weighing Methods 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000009826 distribution Methods 0.000 description 4
- 238000000691 measurement method Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000008186 active pharmaceutical agent Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229940088679 drug related substance Drugs 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 206010019280 Heart failures Diseases 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 102000000070 Sodium-Glucose Transport Proteins Human genes 0.000 description 1
- 108010080361 Sodium-Glucose Transport Proteins Proteins 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003472 antidiabetic agent Substances 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 229940126904 hypoglycaemic agent Drugs 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 208000001072 type 2 diabetes mellitus Diseases 0.000 description 1
- 238000010200 validation analysis Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
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
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- 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)
- Nitrogen Condensed Heterocyclic Rings (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention relates to a particle size determination method of dapagliflozin bulk drug, which comprises the following steps: taking a dapagliflozin raw material medicine to be detected, and feeding the sample into a particle size analyzer for particle size determination; wherein the particle analyzer is a laser particle analyzer, the gap of a hopper is 1.2 mm-1.8 mm, and the dispersion air pressure is 2 bar-3.5 bar; the sample injector is a dry-method sample injector, the sample injection amount is 220-350 mg, and the sample injection speed is 25-35%. The particle size determination method of the dapagliflozin bulk drug obtains a determination method with good repeatability and high intermediate precision by comprehensively optimizing parameters in various aspects such as sample injection amount, hopper clearance, sample injection speed, pressure and the like on the basis of combining a laser particle sizer and dry sample injection, and meets the control requirements of pharmacopoeia on the particle size determination of the bulk drug. In addition, the method is simple and easy to operate.
Description
Technical Field
The invention relates to the technical field of drug analysis, in particular to a particle size determination method for dapagliflozin bulk drug.
Background
Dapagliflozin (Dapagliflozin) is the first sodium glucose co-transporter2 (SGLT 2) inhibitor marketed worldwide and was jointly developed by Bristol-Myers Squibb, usa and AstraZeneca, sweden. Dapagliflozin tablets in 11 months in 2012 are approved by EMA to be marketed as a novel hypoglycemic agent for treating type 2 diabetes (T2 DM), are approved by FDA in usa in 1 month in 2014, are approved by FDA in china in 3 months in 2017, and are added with indications for treating heart failure in 3 months in 2021.
The dapagliflozin bulk drug is dapagliflozin propylene glycol monohydrate, the chemical name of which is (1S) -1, 5-anhydride-1-C- [ 4-chloro-3- [ (4-ethoxyphenyl) methyl ] phenyl ] -D-glucitol, and the molecular structure of the hydrate (1:
dapagliflozin propylene glycol monohydrate is white to off-white powder, has no hygroscopicity, and is easily soluble in methanol. The agglomeration phenomenon of the raw material medicine is obvious, so the raw material medicine needs to be crushed before production, and the particle size of the crushed raw material medicine needs to be measured in order to ensure the consistency of the particle sizes of the raw material medicine contained in preparation batches.
There is a method of measuring the particle size distribution of dapagliflozin by a wet measurement method in a light scattering method, which is performed after suspending dapagliflozin in water to prepare a suspension. However, dapagliflozin propylene glycol monohydrate is not suitable for dispersion in water because dapagliflozin propylene glycol monohydrate is sparingly soluble in water and tends to lose crystal water in water. In other organic solvents, however, there is a risk of uneven dispersion. Meanwhile, when other dispersion media are explored, the problems of poor repeatability and low intermediate precision of the particle size measuring method are found.
Disclosure of Invention
Based on the particle size determination method, the particle size determination method of the dapagliflozin bulk drug is good in repeatability and high in intermediate precision.
The application provides a particle size determination method for dapagliflozin bulk drug, which comprises the following steps:
taking a dapagliflozin raw material medicine to be detected, and feeding the sample into a particle size analyzer for particle size determination;
wherein the particle analyzer is a laser particle analyzer, the gap of the hopper is 1.2 mm-1.8 mm, and the dispersion air pressure is 2 bar-3.5 bar;
the sample injector is a dry-method sample injector, the sample injection amount is 220-350 mg, and the sample injection speed is 25-35%.
In one embodiment, the particle sizer has a measurement time of 8s to 14s.
In one embodiment, the measurement time is 10s.
In one embodiment, the sample size is 300mg.
In one embodiment, the injection rate is 30%.
In one embodiment, the dispersion pressure is 3.5bar.
In one embodiment, the dispersion pressure is 2.5bar.
In one embodiment, the hopper gap is 1.5mm.
In one embodiment, the dry injector is an Areo S dry injector.
In one embodiment, the laser particle sizer is a malvern Mastersizer3000 laser particle sizer.
In one embodiment, the dapagliflozin drug substance is dapagliflozin propylene glycol monohydrate.
The particle size determination method of the dapagliflozin bulk drug is based on the combination of a laser particle analyzer and dry sampling, comprehensively optimizes parameters in various aspects such as sampling amount, hopper clearance, sampling speed, pressure and the like, obtains a determination method with good repeatability and high intermediate precision, and meets the control requirements of pharmacopoeia on the particle size determination of the bulk drug.
In addition, the method is simple and easy to operate, avoids complex operations such as solution preparation and the like in a wet method particle size determination method, can effectively improve the research and development efficiency and the production efficiency, ensures the uniformity of the dapagliflozin preparation, and provides a reliable quality control technical means for the research of the dapagliflozin preparation.
Detailed Description
The method for measuring the particle size of dapagliflozin bulk drug according to the present invention is described in further detail below with reference to specific examples. This application may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
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 to which this application belongs. The terminology used herein in the description of the present application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application.
In the technical features described in the open-ended form, the closed technical scheme comprising the listed features also comprises the open technical scheme comprising the listed features.
In the present application, reference is made to a range of values which, unless otherwise indicated, are considered to be continuous within the range and include both the minimum and maximum values of the range and each and every value between such minimum and maximum values. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range describing features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to encompass any and all subranges subsumed therein.
The percentage contents referred to in the present application mean, unless otherwise specified, mass percentages for solid-liquid mixing and solid-solid phase mixing, and volume percentages for liquid-liquid phase mixing.
The percentage concentrations referred to in this application, unless otherwise indicated, refer to the final concentrations. The final concentration refers to the ratio of the added component in the system after the component is added.
The temperature parameter in the present application is not particularly limited, and may be a constant temperature treatment or a treatment within a certain temperature range. The constant temperature process allows the temperature to fluctuate within the accuracy of the instrument control.
The particle size in this application refers to the size of the particles, also known as "particle size" or "diameter". When a certain physical property or physical behavior of the measured particle is most similar to a homogeneous sphere (or combination) with a certain diameter, the diameter (or combination) of the sphere is taken as the equivalent particle size (or particle size distribution) of the measured particle. The D90 particle size is the equivalent diameter of the largest particle in the distribution curve with a cumulative distribution of 90%, and its physical meaning is that the particle size is less than 90% of its particle size.
The application provides a particle size determination method for dapagliflozin bulk drug, which comprises the following steps:
taking a dapagliflozin raw material medicine to be detected, and feeding the sample into a particle size analyzer for particle size determination;
wherein the particle analyzer is a laser particle analyzer, the gap of the hopper is 1.2 mm-1.8 mm, and the dispersion air pressure is 2 bar-3.5 bar;
the sample injector is a dry-method sample injector, the sample injection amount is 220-350 mg, and the sample injection speed is 25-35%. Specifically, the sample size includes, but is not limited to: 220mg, 230mg, 240mg, 250mg, 260mg, 270mg, 280mg, 290mg, 300mg, 310mg, 320mg, 330mg, 340mg, 350mg.
In some examples, the sample size is 260mg to 340mg. Further, the sample injection amount is 280-320 mg. Still further, the sample size was 300mg.
Specifically, the sample injection speed includes but is not limited to: 25%, 26%, 27%, 28%, 29%, 30%, 31%, 32%, 33%, 34%, 35%.
In some examples, the sample injection rate is 26% to 34%. Further, the sample injection speed is 28% -32%. Further, the sample injection speed is 30%.
In some of these examples, the particle sizer has a measurement time of 8s to 14s.
Specifically, the measurement time includes, but is not limited to: 8s, 9s, 10s, 11s, 12s, 13s, 14s.
In some of these examples, the measurement time is between 9s and 13s. Further, the measurement time is 10s.
Specifically, the dispersed gas pressure includes, but is not limited to: 2.0bar, 2.1bar, 2.2bar, 2.3bar, 2.4bar, 2.5bar, 2.6bar, 2.7bar, 2.8bar, 2.9bar, 3.0bar, 3.1bar, 3.2bar, 3.3bar, 3.4bar, 3.5bar.
In some of these examples, the dispersion pressure is 2.5bar to 3.5bar. Further, the dispersion pressure was 3.5bar. Further, the dispersion pressure was 2.5bar.
Specifically, the hopper gap includes, but is not limited to: 1.2mm, 1.3mm, 1.4mm, 1.5mm, 1.6mm, 1.7mm, 1.8mm.
In some of these examples, the hopper gap is 1.3mm to 1.7mm. Further, the hopper gap is 1.5mm.
Additionally, in some of these examples, the drysampler is an Areo S drysampler.
In some of these examples, the laser particle sizer is a malvern Mastersizer3000 laser particle sizer.
In some of these examples, the dapagliflozin drug substance is dapagliflozin propylene glycol monohydrate, which has the following structural features:
the following examples and comparative examples are further described in the following, and the raw materials used in the following examples and comparative examples can be obtained from commercial sources if not specifically mentioned, the equipment used can be obtained from commercial sources if not specifically mentioned, and the processes involved are those conventionally selected by those skilled in the art or according to the conditions suggested by manufacturers if not specifically mentioned.
Particle size measurement instrument: malvern Mastersizer3000 laser particle sizer.
Sample injector: areo S dry sampler.
In determining the particle size determination method of the crude drug, the standard (USP 429 particle size determination method) is accepted: more than 10 μm, RSD of D50 is less than or equal to 10%, RSD of D10 and D90 is less than or equal to 15%; less than 10 μm, RSD of D50 less than or equal to 20%, RSD of D10 and D90 less than or equal to 30%.
Example 1
The embodiment is a method for measuring the particle size of a dapagliflozin bulk drug, comprising the following steps:
opening a Malvern Mastersizer3000 laser particle analyzer, setting parameters of an injector which is an Areo S dry-process injector: the mode is a general mode, the hopper gap is 1.5mm, the sample measuring time is 10s, the sample introduction speed is 30%, and the dispersion air pressure is 3.5bar.
And (3) sample measurement: 300mg of crushed dapagliflozin propylene glycol monohydrate raw material drug (hereinafter referred to as a raw material drug sample) is added into a sample hopper, and after background measurement is finished, the particle size of the sample is measured. The same batch was run in parallel for 3 groups of drug samples.
The results are shown in table 1 below.
TABLE 1
As can be seen from Table 1, the RSD of the particle size measured by this measurement method meets the acceptance criterion.
Example 2
The present example is a method for determining the particle size of dapagliflozin bulk drug, the steps are the same as example 1, and the parameters are set as follows:
weighing 300mg of a raw material medicine sample, setting a hopper gap of 1.5mm, setting a sample introduction speed of 30%, setting a dispersion air pressure of 2.5bar, measuring for 10s, and determining the particle size of the sample. The same batch was run in parallel for 3 groups of drug samples.
The results are shown in table 2 below.
TABLE 2
As can be seen from Table 2, the RSD of the particle size measured at a pressure of 2.5bar, with the other parameters being unchanged, meets the acceptance criteria.
Example 3 repeatability verification
Referring to the determination method in example 1, about 300mg of the raw material drug sample, 6 parts in total, is weighed, the gap of a hopper is set to be 1.5mm, the sample introduction speed is 30%, the dispersion air pressure is 3.5bar, the measurement time is 10s, and the particle size of the sample is determined.
The results are shown in table 3 below.
TABLE 3
Experimental results show that RSD of the determination method meets the acceptable standard, namely the repeatability is good.
Example 4 intermediate precision validation
Weighing about 300mg of the raw material medicine sample by another person, 6 parts in total, setting a hopper gap of 1.5mm, a sample introduction speed of 30%, a dispersion air pressure of 3.5bar, a measurement time of 10s, and measuring the particle size of the sample.
The measurement results are shown in tables 4 to 5 below:
TABLE 4
TABLE 5 Combined assay results
The experimental results show that another person can determine 6 samples by the same method at different times, and the RSD meets the acceptable standard; the results of the combined measurements show that RSD still meets the acceptable standard, so the intermediate precision of the determined method is good.
Comparative example
The sample introduction amount, the hopper clearance, the sample introduction speed, the dispersion air pressure and the measurement time in the particle size measurement method of the dapagliflozin bulk drug of example 1 were variously adjusted, and the following comparative example experiment was performed:
comparative example 1: weighing about 100mg of raw material medicine sample, 3 parts in total, setting hopper gap of 1.5mm, sample introduction speed of 30%, pressure of 3.5bar, measuring time of 10s, and determining sample particle size.
Comparative example 2: weighing about 200mg of raw material medicine sample, 3 parts in total, setting a hopper gap of 1.5mm, a sample introduction speed of 30%, a pressure of 3.5bar, a measurement time of 10s, and measuring the particle size of the sample.
Comparative example 3: weighing about 300mg of raw material medicine sample, 3 parts in total, setting hopper gap of 1.0mm, sample introduction speed of 30%, pressure of 3.5bar, measuring time of 10s, and determining sample particle size.
Comparative example 4: weighing about 300mg of raw material medicine sample, 3 parts in total, setting a hopper gap of 2.0mm, a sample introduction speed of 30%, a pressure of 3.5bar, a measurement time of 10s, and measuring the particle size of the sample.
Comparative example 5: weighing about 300mg of raw material medicine sample, 3 parts in total, setting hopper gap of 1.5mm, sample introduction speed of 20%, pressure of 3.5bar, measuring time of 10s, and determining sample particle size.
Comparative example 6: weighing about 300mg of raw material medicine sample, 3 parts in total, setting hopper gap of 1.5mm, sample introduction speed of 40%, pressure of 3.5bar, measuring time of 10s, and determining sample particle size.
Comparative example 7: weighing about 300mg of raw material medicine sample, 3 parts in total, setting hopper gap of 1.5mm, sample introduction speed of 30%, pressure of 4.0bar, measuring time of 10s, and determining sample particle size.
Comparative example 8: weighing about 300mg of raw material medicine sample, 3 parts in total, setting a hopper gap of 1.5mm, a sample introduction speed of 30%, a pressure of 3.5bar, a measurement time of 5s, and measuring the particle size of the sample.
Comparative example 9: weighing about 300mg of raw material medicine sample, 3 parts in total, setting hopper gap of 1.5mm, sample introduction speed of 30%, pressure of 3.5bar, measuring time of 15s, and determining sample particle size.
The test results are shown in table 6 below:
TABLE 6
The above experimental results show that:
(1) For the sample addition amount: when the sample addition amount is 100mg, the RSD of D90 exceeds the acceptable standard; when the sample addition amount is 200mg, the RSD of D90 reaches the upper limit.
(2) For the hopper gap: when the hopper gap is 1.0mm and 2.0mm, the RSD of D90 is above the acceptable standard and too large a hopper gap results in too high a sample concentration and smaller measured particle size due to multiple scattering.
(3) For the sample introduction rate: the RSD of D90 exceeded the acceptance criteria at injection rates of 20% and 40%.
(4) For the pressure: the RSD of D90 exceeds the acceptance criterion at a pressure of 4.0 bar.
(5) For the measurement time: the RSD of D90 exceeds the acceptance criterion when the measurement times are 5s and 15 s.
From the above, when the dry method is used for determining the dapagliflozin particle size, the measurement of the particle size of the raw material medicine can be obviously influenced by the sample adding amount, the hopper gap, the sample introduction speed, the dispersion pressure and the measurement time. The method comprehensively optimizes parameters in various aspects such as sample introduction amount, hopper clearance, sample introduction speed, pressure, measurement time and the like, and obtains the measurement method with good repeatability and high intermediate precision.
All possible combinations of the technical features of the above embodiments may not be described for the sake of brevity, but should be considered as within the scope of the present disclosure as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, so as to understand the technical solutions of the present invention specifically and in detail, but not to be understood as the limitation of the protection scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. It should be understood that the technical solutions provided by the present invention, which are obtained by logical analysis, reasoning or limited experiments, are within the scope of the appended claims. Therefore, the protection scope of the patent of the invention is subject to the content of the appended claims, and the description can be used for explaining the content of the claims.
Claims (11)
1. A particle size determination method for dapagliflozin bulk drug is characterized by comprising the following steps:
taking a dapagliflozin raw material medicine to be detected, and feeding the sample into a particle size analyzer for particle size determination;
wherein the particle analyzer is a laser particle analyzer, the gap of a hopper is 1.2 mm-1.8 mm, and the dispersion air pressure is 2 bar-3.5 bar;
the sample injector is a dry-method sample injector, the sample injection amount is 220-350 mg, and the sample injection speed is 25-35%.
2. The method for measuring the particle size of dapagliflozin bulk drug according to claim 1, characterized in that the measurement time of a particle size analyzer is 8 s-14 s.
3. The method for determining the particle size of dapagliflozin bulk drug according to claim 2, characterized in that the measurement time is 10s.
4. The method for determining the particle size of dapagliflozin bulk drug according to claim 1, characterized in that the sample size is 300mg.
5. The method for determining the particle size of dapagliflozin bulk drug according to claim 1, characterized in that the sample injection speed is 30%.
6. The method for determining the particle size of a dapagliflozin bulk drug according to claim 1, characterized in that the dispersion gas pressure is 3.5bar.
7. The method for determining the particle size of a dapagliflozin bulk drug according to claim 1, characterized in that the dispersion gas pressure is 2.5bar.
8. The method for determining the particle size of a dapagliflozin bulk drug according to claim 1, wherein the hopper gap is 1.5mm.
9. The method for measuring the particle diameter of a dapagliflozin bulk drug according to any one of claims 1 to 8, characterized in that the dry injector is an AreO S dry injector.
10. The method for determining the particle size of dapagliflozin bulk drug according to any one of claims 1-8, characterized in that the laser particle sizer is a malvern Mastersizer3000 laser particle sizer.
11. The method for determining the particle size of a dapagliflozin bulk drug according to any one of claims 1 to 8, characterized in that the dapagliflozin bulk drug is dapagliflozin propylene glycol monohydrate.
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| CN202210988089.1A CN115343198A (en) | 2022-08-17 | 2022-08-17 | Particle size determination method for dapagliflozin bulk drug |
| PCT/CN2023/104365 WO2024037221A1 (en) | 2022-08-17 | 2023-06-30 | Method for measuring particle size of dapagliflozin active pharmaceutical ingredient |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2024037221A1 (en) * | 2022-08-17 | 2024-02-22 | 扬子江药业集团上海海尼药业有限公司 | Method for measuring particle size of dapagliflozin active pharmaceutical ingredient |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20180058510A (en) * | 2016-11-24 | 2018-06-01 | 한미약품 주식회사 | Pharmaceutical formulation comprising dapagliflozin l-proline |
| KR20180078762A (en) * | 2016-12-30 | 2018-07-10 | 한미약품 주식회사 | Pharmaceutical composition comprising DAPAGLIFLOZIN L-PROLINE for the prevention or treatment of diabetes |
| 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 |
| CN113654956A (en) * | 2021-07-27 | 2021-11-16 | 广州白云山医药集团股份有限公司白云山制药总厂 | Method for determining particle size and particle size distribution of amoxicillin bulk drug |
| CN114062208A (en) * | 2021-11-18 | 2022-02-18 | 上海新亚药业闵行有限公司 | Method for analyzing particle size of cefalexin |
| CN115343198A (en) * | 2022-08-17 | 2022-11-15 | 扬子江药业集团上海海尼药业有限公司 | Particle size determination method for dapagliflozin bulk drug |
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2023
- 2023-06-30 WO PCT/CN2023/104365 patent/WO2024037221A1/en unknown
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2024037221A1 (en) * | 2022-08-17 | 2024-02-22 | 扬子江药业集团上海海尼药业有限公司 | Method for measuring particle size of dapagliflozin active pharmaceutical ingredient |
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| Publication number | Publication date |
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| WO2024037221A1 (en) | 2024-02-22 |
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