Ofloxacin Tablets
DEFINITION
Ofloxacin Tablets contain NLT 90.0% and NMT 110.0% of the labeled amount of ofloxacin (C18H20FN3O4).
IDENTIFICATION
• 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:
Dissolve 2.72 mg/mL of monobasic potassium phosphate in water. Adjust with diluted phosphoric acid to a pH of 3.3 ± 0.1.
Mobile phase:
Acetonitrile and Solution A (3:22)
Diluent 1:
Methanol and glacial acetic acid (3:1)
Diluent 2:
Acetonitrile and water (1:9)
Standard stock solution:
1 mg/mL of USP Ofloxacin RS in Diluent 1
Standard solution:
20 µg/mL of USP Ofloxacin RS from the Standard stock solution in Diluent 2
Sample solution:
Transfer an equivalent of 100 mg of ofloxacin from powdered Tablets to a 100-mL volumetric flask. Add 70 mL of Diluent 1, and sonicate for 20 min. Dilute with Diluent 1 to volume. Pass a portion of this solution through a filter having a 0.45-µm or finer porosity, and collect the filtrate. Dilute 2.0 mL of the filtrate with Diluent 2 to 100 mL.
Chromatographic system
Mode:
LC
Detector:
UV 294 nm
Column:
4.6-mm × 10-cm; packing L1
Flow rate:
1 mL/min
Injection size:
20 µL
System suitability
Sample:
Standard solution
Suitability requirements
Tailing factor:
NMT 2.0
Relative standard deviation:
NMT 2.0%
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of C18H20FN3O4 in the portion of Tablets 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 Ofloxacin RS in the Standard solution (mg/mL) |
| CU | = | = nominal concentration of the Sample solution (mg/mL) |
Acceptance criteria:
90.0%–110.0%
PERFORMANCE TESTS
• Dissolution 
711
711
Medium:
0.1 N hydrochloric acid; 900 mL
Apparatus 1:
100 rpm
Time:
30 min
Standard stock solution:
0.44 mg/mL of USP Ofloxacin RS in methanol
Standard solution:
8.8 µg/mL of USP Ofloxacin RS from the Standard stock solution diluted with Medium
Sample solution:
Pass a portion of the solution under test through a suitable 0.45-µm filter. Dilute a portion of the filtrate with Medium to obtain a final theoretical concentration of 8.8 µg/mL, assuming complete dissolution of the label claim.
Spectrometric conditions
Mode:
UV-Vis
Analytical wavelength:
294 nm
Cell:
1 cm
Blank:
Medium
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of C18H20FN3O4 dissolved:
Result = (AU/AS) × CS × D × V × (100/L)
| AU | = | = absorbance from the Sample solution |
| AS | = | = absorbance from the Standard solution |
| CS | = | = concentration of ofloxacin in the Standard solution (mg/mL) |
| D | = | = dilution factor of the Sample solution |
| V | = | = volume of Medium, 900 mL |
| L | = | = label claim of a Tablet (mg) |
Tolerances:
NLT 80% (Q) of the labeled amount of C18H20FN3O4 is dissolved.
• Uniformity of Dosage Units 905:
Meet the requirements
905:
Meet the requirements
IMPURITIES
Organic Impurities
• Procedure 1
Phosphate buffer:
2.72 mg/mL of monobasic potassium phosphate in water. Adjust with diluted phosphoric acid to a pH of 3.3 ± 0.1.
Solution A:
Acetonitrile and Phosphate buffer (3:22)
Solution B:
Acetonitrile and Phosphate buffer (3:2)
Mobile phase:
See the gradient table below.
| Time (min) |
Solution A (%) |
Solution B (%) |
|---|---|---|
| 0 | 100 | 0 |
| 8 | 100 | 0 |
| 25 | 40 | 60 |
| 26 | 100 | 0 |
| 40 | 100 | 0 |
Standard solution:
4 µg/mL of USP Ofloxacin RS in methanol
Sample solution:
Transfer an equivalent of 100 mg of ofloxacin from powdered Tablets to a 100-mL volumetric flask. Add 70 mL of methanol, and sonicate for 20 min. Dilute with methanol to volume. Pass a portion of this solution through a filter having a 0.45-µm or finer porosity, discarding the first 5 mL. Use the filtrate.
Chromatographic system
Mode:
LC
Detector:
UV 294 nm
Column:
4.6-mm × 10-cm; packing L1
Flow rate:
1 mL/min
Injection size:
10 µL
System suitability
Sample:
Standard solution
Suitability requirements
Tailing factor:
NMT 2.0
Relative standard deviation:
NMT 5.0%
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of each impurity in the portion of Tablets taken:
Result = (rU/rS) × (CS/CU) × (1/F) × 100
| rU | = | = peak response of the impurity from the Sample solution |
| rS | = | = peak response of ofloxacin from the Standard solution |
| CS | = | = concentration of USP Ofloxacin RS in the Standard solution (mg/mL) |
| CU | = | = nominal concentration of ofloxacin in the Sample solution (mg/mL) |
| F | = | = relative response factor for each impurity (see Impurity Table 1) |
Acceptance criteria:
See Impurity Table 1.
Impurity Table 1
| Name | Relative Retention Time |
Relative Response Factor |
Acceptance Criteria, NMT (%) |
|---|---|---|---|
| Impurity Aa | 0.5 | 1 | 0.3 |
| Impurity Bb | 3.6 | 0.22 | 0.3 |
| Any other impurity | — | 1 | 0.2 |
| All impurities | — | — | 1.0 |
|
a
(2,3-Dihydro-3-methyl-10-(4-methyl-1-piperazinyl)-7-oxo-7H-pyrido[1,2,3-de]-1,4-benzoxazine-6-carboxylic acid).
b
(9,10-Difluoro-3-methyl-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de]-1,4-benzoxazine-6-carboxylic acid).
|
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ADDITIONAL REQUIREMENTS
• Packaging and Storage:
Preserve in well-closed containers, and store at controlled room temperature.
• USP Reference Standards 11
11
USP Ofloxacin RS 
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Auxiliary Information—
Please check for your question in the FAQs before contacting USP.
| Topic/Question | Contact | Expert Committee |
|---|---|---|
| Monograph | Leonel M. Santos, Ph.D.
Senior Scientific Liaison 1-301-816-8168 |
(SM12010) Monographs - Small Molecules 1 |
| 711 |
Margareth R.C. Marques, Ph.D.
Senior Scientific Liaison 1-301-816-8106 |
(GCDF2010) General Chapters - Dosage Forms |
| Reference Standards | RS Technical Services 1-301-816-8129 rstech@usp.org |
USP35–NF30 Page 4100
Pharmacopeial Forum: Volume No. 34(6) Page 1467