Mometasone Furoate Topical Solution
DEFINITION
Mometasone Furoate Topical Solution is Mometasone Furoate in a suitable aqueous vehicle. It contains NLT 90.0% and NMT 110.0% of the labeled amount of mometasone furoate (C27H30Cl2O6).
IDENTIFICATION
• A.
The retention time of the major peak of the Sample solution corresponds to that of the Standard solution, both relative to the internal standard, as obtained in the Assay.
• B. Thin-Layer Chromatographic Identification Test 
201
201
Standard solution:
1 mg/mL of USP Mometasone Furoate RS in a mixture of chloroform and methanol (4:1)
Sample solution:
Transfer the equivalent of 2 mg of mometasone furoate from Topical Solution to a 50-mL centrifuge tube. Add 10 mL of water. Extract the aqueous solution with 20 mL of chloroform. Remove the chloroform layer, dry over anhydrous sodium sulfate, and filter through a cotton pledget. Repeat the chloroform extraction, and combine the dried extracts. Evaporate the chloroform solution to dryness on a steam bath under a stream of nitrogen. Allow the sample specimen to cool to room temperature. Dissolve the residue in a mixture of chloroform and methanol (4:1) to obtain 1 mg/mL of Sample solution.
Application volume:
20 µL
Developing solvent system:
Chloroform and ethyl acetate (3:1)
Acceptance criteria:
The RF value of the principal spot of the Sample solution corresponds to the that of the Standard solution.
ASSAY
• Procedure
[Note—Protect from light. ]
Diluent:
Acetonitrile, water, and glacial acetic acid (50:50:1)
Solution A:
Water
Solution B:
Acetonitrile
Mobile phase:
See Table 1.
Table 1
| Time (min) |
Solution A (%) |
Solution B (%) |
|---|---|---|
| 0 | 70 | 30 |
| 2 | 70 | 30 |
| 45 | 45 | 55 |
| 46 | 70 | 30 |
| 50 | 70 | 30 |
Standard solution:
0.1 mg/mL of USP Mometasone Furoate RS in Solution B
Sample solution:
Transfer a portion of Topical Solution, equivalent to about 2.5 mg of mometasone furoate, to a 25-mL flask. Dilute with Diluent to volume, and mix. Pass a portion of the solution through a polypropylene filter of 0.2-µm pore size, discarding the first 1–2 mL of filtrate.
Chromatographic system
Mode:
LC
Detector:
UV 254 nm
Column:
4.6-mm × 25-cm; 5-µm packing L60
Flow rate:
2 mL/min
Injection size:
50 µL
System suitability
Sample:
Standard solution
Suitability requirements:
Tailing factor:
NMT 1.5 for the mometasone furoate peak
Relative standard deviation:
NMT 2.0%
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of mometasone furoate (C27H30Cl2O6) in the portion of Topical Solution taken:
Result = (rU/rS) × (CS/CU) × 100
| rU | = | = peak response from the Sample solution |
| rS | = | = peak response from the Standard solution |
| CS | = | = concentration of USP Mometasone Furoate RS in the Standard solution (mg/mL) |
| CU | = | = nominal concentration of mometasone furoate in the Sample solution (mg/mL) |
Acceptance criteria:
90.0%–110.0%
IMPURITIES
• Organic Impurities
[Note—Protect from light. ]
Diluent, Solution A, Solution B, Mobile phase, Standard solution, and Sample solution:
Prepare as directed in the Assay.
System suitability solution:
0.1 µg/mL of USP Mometasone Furoate RS from Standard solution in Diluent
Chromatographic system
Mode:
LC
Detector:
UV 254 nm
Column:
4.6-mm × 25-cm; 5-µm packing L60
Column temperature:
25 ± 5
Flow rate:
2 mL/min
Injection size:
50 µL
System suitability
Sample:
System suitability solution
Suitability requirements
Relative standard deviation:
NMT 10%
Analysis
Samples:
Diluent, System suitability solution, and Sample solution
[Note—Exclude any peak areas less than that of the System suitability solution. Also, exclude any peaks with the same retention times as those observed in the Diluent. Any peaks having a relative retention time of 1.04 or 1.13 are controlled in the Mometasone Furoate monograph, and therefore are not included in the total specified and unspecified impurities limit. ]
Calculate the percentage of each impurity in the portion of Topical Solution taken:
Result = (rU/rT) × 100
| rU | = | = peak response of each impurity from the Sample solution |
| rT | = | = sum of all the peak responses from the Sample solution |
Acceptance criteria:
See Table 2.
Table 2
| Name | Relative Retention Time |
Acceptance Criteria, NMT (%) |
|
|---|---|---|---|
9 -Chloro-11 ,17,21-trihydroxy-16-methylpregna-1,4-diene-3,20-dione 17-(2-furoate) |
0.56 | 0.3 | |
| 9,21-Dichloro-11,17-dihydroxy-16-methylpregna-1,4-diene-3,20-dione |
0.73 | 0.1 | |
| 21-Chloro-17-hydroxy-16- methylpregna-1,4-diene-3,11,20-trione 17-(2-furoate) |
0.88 | 0.1 | |
| 21-Chloro-9,11-epoxy-17-hydroxy-16-methylpregna-1,4-diene-3,20-dione 17-(2-furoate) |
0.94 | 1.0 | |
| Mometasone furoate | 1.0 | — | |
| Unspecified individual impurity | — | 0.5 | |
| Total specified and unspecified impurities | — | 2.0 | |
SPECIFIC TESTS
• Microbial Enumeration Tests 61 and Tests for Specified Microorganisms 62:
It meets the requirements of the tests for absence of Staphylococcus aureus, Pseudomonas aeruginosa, Escherichia coli, and Salmonella species.
61 and Tests for Specified Microorganisms 62:
It meets the requirements of the tests for absence of Staphylococcus aureus, Pseudomonas aeruginosa, Escherichia coli, and Salmonella species.
• pH 791:
4.0–5.0
791:
4.0–5.0
ADDITIONAL REQUIREMENTS
• Packaging and Storage:
Preserve in well-closed containers, and store at controlled room temperature.
• USP Reference Standards 11
11
USP Mometasone Furoate RS 
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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 |
| 61 |
Radhakrishna S Tirumalai, Ph.D.
Principal Scientific Liaison 1-301-816-8339 |
(GCM2010) General Chapters - Microbiology |
| 62 |
Radhakrishna S Tirumalai, Ph.D.
Principal Scientific Liaison 1-301-816-8339 |
(GCM2010) General Chapters - Microbiology |
| Reference Standards | RS Technical Services 1-301-816-8129 rstech@usp.org |
USP35–NF30 Page 3947
Pharmacopeial Forum: Volume No. 35(1) Page 87