Mometasone Furoate Ointment
DEFINITION
Mometasone Furoate Ointment is Mometasone Furoate in a suitable ointment base. 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 Chromatography
Standard solution:
0.6 mg/mL of USP Mometasone Furoate RS in methanol
Sample solution:
Transfer the equivalent to 3 mg of mometasone furoate from Ointment to a 50-mL screw-capped centrifuge tube. Pipet 5.0 mL of methanol into the tube, and attach the cap. Heat in a steam bath until the Ointment completely melts, and shake vigorously until the Ointment resolidifies. Place in an ice-water bath for 10 min. Centrifuge, and filter a portion of the supernatant. Extract 1 mL of the filtrate with 1 mL of hexane, and use the lower phase.
Adsorbent:
0.25-mm layer of chromatographic silica gel mixture
Application volume:
10 µL
Developing solvent system A:
Methanol
Developing solvent system B:
Chloroform and ethyl acetate (3:1)
Analysis
Samples:
Standard solution and Sample solution
Allow the spots to dry, and develop the chromatogram in Developing solvent system A until the solvent front has moved 2 cm from the origin. Remove the plate from the developing chamber, and air-dry. Develop the chromatogram in Developing solvent system B until the solvent front has moved three-fourths of the length of the plate. Remove the plate from the developing chamber, mark the solvent front, and allow the spots to air-dry. Examine the plate under short-wavelength UV light.
Acceptance criteria:
The RF value of the principal spot of the Sample solution corresponds to that of the Standard solution.
ASSAY
• Procedure
[Note—Protect from light. ]
Diluent A:
Tetrahydrofuran and glacial acetic acid (100:1)
Diluent B:
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 |
Internal standard solution:
1.4 mg/mL of diethyl phthalate in acetonitrile
Standard stock solution:
0.2 mg/mL of USP Mometasone Furoate RS in Diluent A
Standard solution:
0.05 mg/mL of mometasone furoate and 0.35 mg/mL of diethyl phthalate from equal quantities of the Standard stock solution and the Internal standard solution, in Diluent B
Sample solution:
Transfer a portion of Ointment, equivalent to 1.0 mg of mometasone furoate, to a 50-mL screw-capped centrifuge tube. Add 5.0 mL of Diluent A and a few glass beads, and mix on a vortex mixer. Add 5.0 mL of Internal standard solution, and mix. Add 10.0 mL of Diluent B, mix on a vortex mixer for 1 min, and centrifuge for 10 min. Pass the aqueous phase 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:
20 µL
System suitability
Sample:
Standard solution
[Note—The relative retention times for diethyl phthalate and mometasone furoate are 0.4 and 1.0, respectively. ]
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 fuorate (C27H30Cl2O6) in the portion of Ointment taken:
Result = (RU/RS) × (CS/CU) × 100
| RU | = | = ratio of the mometasone furoate peak response to the diethyl phthalate peak response from the Sample solution |
| RS | = | = ratio of the mometasone furoate peak response to the diethyl phthalate 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 A, Solution A, Solution B, Mobile phase, and Standard stock solution:
Prepare as directed in the Assay.
Diluent C:
Acetonitrile, water, and glacial acetic acid (30:70:1)
System suitability solution:
0.1 µg/mL of USP Mometasone Furoate RS from Standard stock solution in Diluent C
Sample solution:
Transfer a portion of Ointment, equivalent to 2.0 mg of mometasone furoate, to a 50-mL screw-capped centrifuge tube. Add 5.0 mL of Diluent A and a few glass beads, and mix on a vortex mixer. Add 15.0 mL of Diluent C, and mix. Centrifuge for 10 min. Pass the aqueous phase through a polypropylene filter of 0.2-µm pore size, discarding the first 1–2 mL of filtrate.
Blank solution:
Diluent C and Diluent A (3:1)
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:
System suitability solution, Sample solution, and Blank solution
[Note—Exclude any peak areas less than those from the chromatogram of the System suitability solution. Also exclude any peaks with the same retention time as that observed in the chromatogram of the Blank solution. Any peaks having a relative retention time of about 1.04 or 1.13 are controlled in the monograph for Mometasone Furoate, and therefore are not included in the total specified and unspecified impurities limit. ]
Calculate the percentage of each impurity in the portion of Ointment 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 | 0.2 |
| 9,21-Dichloro-11,17-dihydroxy-16-methylpregna-1,4-diene-3,20-dione |
0.73 | 0.2 |
| 21-Chloro-17-hydroxy-16-methylpregna-1,4-diene-3,11,20-trione 17-(2-furoate) |
0.88 | 0.2 |
| 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 |
— | 0.2 |
| Total specified and unspecified impurities |
— | 1.0 |
PERFORMANCE TESTS
• Minimum Fill 
755
:
Meets the requirements
755:
Meets the requirements
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.
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 3945
Pharmacopeial Forum: Volume No. 35(1) Page 84