Halobetasol Propionate
C25H31ClF2O5 484.96
Pregna-1,4-diene-3,20-dione, 21-chloro-6,9-difluoro-11-hydroxy-16-methyl-17-(1-oxopropoxy)-, (6
,11
,16)-;
21-Chloro-6,9-difluoro-11,17-dihydroxy-16-methylpregna-1,4-diene-3,20-dione 17-propionate
[66852-54-8].
(hal'' oh bay' ta sol proe' pee oh nate).
+'&img=../../images/v35300/cas-66852-54-8.gif&casNumber=66852-54-8&usp=35&nf=30&chemicalStructureImage=true&ID='+parent.myID,600,500);)
C25H31ClF2O5 484.96
Pregna-1,4-diene-3,20-dione, 21-chloro-6,9-difluoro-11-hydroxy-16-methyl-17-(1-oxopropoxy)-, (6
,11,16)-;
21-Chloro-6
,9-difluoro-11,17-dihydroxy-16-methylpregna-1,4-diene-3,20-dione 17-propionate
[66852-54-8].DEFINITION
Halobetasol Propionate contains NLT 98.0% and NMT 102.0% of C25H31ClF2O5, calculated on the dried basis.
IDENTIFICATION
• B.
The retention time of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.
ASSAY
• Procedure
Solution A:
Acetonitrile and water (9:11)
Solution B:
Acetonitrile
Mobile phase:
See the gradient table below.
| Time (min) |
Solution A (%) |
Solution B (%) |
|---|---|---|
| 0 | 100 | 0 |
| 2 | 64.5 | 35.5 |
| 22 | 64.5 | 35.5 |
| 23 | 100 | 0 |
| 30 | 100 | 0 |
Standard solution:
0.2 mg/mL of USP Halobetasol Propionate RS in acetonitrile
Sample solution:
0.2 mg/mL of Halobetasol Propionate in acetonitrile
Chromatographic system
Mode:
LC
Detector:
UV 240 nm
Column:
4.6-mm × 25-cm; 5-µm packing L1
Column temperature
40
Flow rate:
0.8 mL/min
Injection size:
20 µL
System suitability
Sample:
Standard solution
Suitability requirements
Relative standard deviation:
NMT 2.0%
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of C25H31ClF2O5 in the portion of Halobetasol Propionate taken:
Result = (rU/rS) × (CS/CU) × 100
| rU | = | = peak response from the Sample solution |
| rS | = | = peak response from the Standard solution |
| CS | = | = concentration of the Standard solution (mg/mL) |
| CU | = | = concentration of the Sample solution (mg/mL) |
Acceptance criteria:
98.0%–102.0% on the dried basis
IMPURITIES
Organic Impurities
• Procedure
Mobile phase, Standard solution, and Sample solution:
Proceed as directed in the Assay.
Chromatographic system
Mode:
LC
Detector:
UV 240 nm
Column:
4.6-mm × 25-cm; 5-µm packing L1
Column temperature:
40
Flow rate:
0.8 mL/min
Injection size:
20 µL
System suitability
Sample:
Standard solution
Suitability requirements
Column efficiency:
NLT 22,000 theoretical plates
Tailing factor:
NLT 0.9 and NMT 1.1 for halobetasol propionate
Relative standard deviation:
NMT 2.0%
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of any impurity in the portion of Halobetasol Propionate taken:
Result = (rU/rT) × 100
| rU | = | = peak response of any individual impurity from the Sample solution |
| rT | = | = sum of responses for all the peaks from the Sample solution |
Acceptance criteria
Individual impurities:
See Impurity Table 1.
Total impurities:
NMT 1.0%
Impurity Table 1
| Name | Relative Retention Time |
Acceptance Criteria, NMT (%) |
|
|---|---|---|---|
| 21-Chloro diflorasonea | 0.75 | 0.15 | |
| 21-Acetate 17-propionate diflorasoneb | 0.88 | 0.15 | |
| 11-Propionate 21- chloro diflorasonec | 0.95 | 0.15 | |
| Halobetasol propionate | 1.0 | — | |
| 9-Chloro halobetasol propionated | 1.12 | 0.15 | |
| 6-Chloro halobetasol propionatee | 1.24 | 0.15 | |
| Any individual, unspecified degradation product | — | 0.10 | |
|
a
21-Chloro-6
,9-difluoro-11,17-dihydroxy-16-methylpregna-1,4-diene-3,20-dione.
b
6
,9-Difluoro-11,17,21-trihydroxy-16-methylpregna-1,4-diene-3,20-dione 21-acetate 17-propionate.
c
21-Chloro-6
,9-difluoro-11,17-dihydroxy-16-methylpregna-1,4-diene-3,20-dione 11-propionate.
d
9,21-Dichloro-6
,-fluoro-11,17-dihydroxy-16-methylpregna-1,4-diene-3,20-dione 17-propionate.
e
6
,21-Dichloro-9-fluoro-11,17-dihydroxy-16-methylpregna-1,4-diene-3,20-dione 17-propionate.
|
|||
SPECIFIC TESTS
• Loss on Drying 
731
:
Dry a sample in a vacuum at 70 for 3 h: it loses NMT 1.0% of its weight.
731:
Dry a sample in a vacuum at 70 for 3 h: it loses NMT 1.0% of its weight.
• Optical Rotation, Specific Rotation 781S
781S
Sample solution:
10 mg/mL in dioxane
Acceptance criteria
Between +87 and +99
and +99
ADDITIONAL REQUIREMENTS
• Packaging and Storage:
Preserve in well-closed, light resistant containers. Store between 2 and 8.
and 8.
• USP Reference Standards 11
11
USP Halobetasol Propionate RS 
Pregna-1,4-diene-3,20-dione, 21-chloro-6,9-difluoro-11-hydroxy-16-methyl-17-(1-oxopropoxy)-, (6,11,16)-.
21-Chloro-6,9-difluoro-11,17-dihydroxy-16-methylpregna-1,4-diene-3,20-dione 17-propionate.
C25H31ClF2O5 484.96
') + '&img=../../images/v35300/cas-66852-54-8.gif',600,500);)
Pregna-1,4-diene-3,20-dione, 21-chloro-6,9-difluoro-11-hydroxy-16-methyl-17-(1-oxopropoxy)-, (6
,11,16)-.
21-Chloro-6
,9-difluoro-11,17-dihydroxy-16-methylpregna-1,4-diene-3,20-dione 17-propionate.
C25H31ClF2O5 484.96
Auxiliary Information—
Please check for your question in the FAQs before contacting USP.
| Topic/Question | Contact | Expert Committee |
|---|---|---|
| Monograph | Clydewyn M. Anthony, Ph.D.
Senior Scientific Liaison 1-301-816-8139 |
(SM22010) Monographs - Small Molecules 2 |
| Reference Standards | RS Technical Services 1-301-816-8129 rstech@usp.org |
USP35–NF30 Page 3396
Pharmacopeial Forum: Volume No. 35(6) Page 1458