Fluconazole Tablets
DEFINITION
Fluconazole Tablets contain NLT 90.0% and NMT 110.0% of the labeled amount of fluconazole (C13H12F2N6O).
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
Buffer:
0.01 M anhydrous sodium acetate solution. Adjust with glacial acetic acid to a pH of 5.0.
Mobile phase:
Methanol, acetonitrile, and Buffer (20:10:70)
Standard stock solution:
1.0 mg/mL of USP Fluconazole RS dissolved in water, and diluted with Mobile phase to volume. Sonicate the solution, if necessary. [NoteThe target ratio is about 5% water to 95% Mobile phase. ]
Standard solution:
0.2 mg/mL of USP Fluconazole RS in Mobile phase prepared from the Standard stock solution
Sample solution:
Weigh NLT 5 Tablets, and disperse in a suitable quantity of water. Sonicate the solution, if necessary. Add a sufficient quantity of Mobile phase, sonicate for 5 min, and shake for 30 min. Dilute with Mobile phase to volume to obtain a concentration between about 1 and 4 mg/mL, and mix. [NoteThe target ratio is about 5% water to 95% Mobile phase. ] Centrifuge a suitable portion of the mixture. Filter and quantitatively dilute a portion of the supernatant with Mobile phase to obtain a solution of about 0.2 mg/mL of fluconazole.
Chromatographic system
Mode:
LC
Detector:
UV 261 nm
Column:
3.9-mm × 150-mm; 4-µm packing L1
Flow rate:
1 mL/min
Injection size:
20 µL
System suitability
Sample:
Standard solution
Suitability requirements
Column efficiency:
NLT 1100 theoretical plates
Tailing factor:
NMT 3.0
Relative standard deviation:
NMT 2.0%
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of the labeled amount of fluconazole (C13H12F2N6O) in the portion of Tablets taken:
Result = (rU/rS) × (CS/CU) × 100
Acceptance criteria:
90.0%110.0%
PERFORMANCE TESTS
• Dissolution 711
Test 1
Medium:
Water; 500 mL (900 mL for Tablets labeled to contain more than 100 mg)
Apparatus 2:
50 rpm
Time:
45 min
Buffer, Mobile phase, and System suitability:
Proceed as directed in the Assay.
Standard solution:
2 mg/mL of USP Fluconazole RS in Medium. Sonicate the solution to facilitate dissolution, if necessary. Quantitatively dilute a portion of this solution with Medium to obtain a final concentration similar to the one expected in the Sample solution.
Sample solution:
Pass a portion of the solution under test through a suitable filter of 0.45-µm pore size.
Chromatographic system and System suitability:
Proceed as directed in the Assay, making any necessary modifications.
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of the labeled amount of fluconazole (C13H12F2N6O) dissolved:
Result = (rU/rS) × (CS/L) × V × 100
Tolerances:
NLT 75% (Q) of the labeled amount of C13H12F2N6O is dissolved.
Test 2:
If the product complies with this test, the labeling indicates that it meets Dissolution Test 2.
Medium:
Water; 900 mL (for all Tablet strengths)
Apparatus 2:
50 rpm
Time:
45 min
Mobile phase:
Water and acetonitrile (4:1)
Standard stock solution:
1.1 mg/mL of USP Fluconazole RS in methanol
Standard solution:
Dilute the Standard stock solution with Medium to obtain a final concentration of (L/900) mg/mL, where L is the Tablet label claim in mg.
Sample solution:
Pass a portion of the solution under test through a suitable filter.
Chromatographic system
Mode:
LC
Detector:
UV 260 nm
Column:
4.6-mm × 15-cm; 5-µm packing L1
Column temperature:
40
Flow rate:
1.5 mL/min
Injection size:
50 µL
System suitability
Sample:
Standard solution
Suitability requirements
Column efficiency:
NLT 1000 theoretical plates
Tailing factor:
NMT 1.5
Relative standard deviation:
NMT 2.0%
Calculate the percentage of the labeled amount of fluconazole (C13H12F2N6O) dissolved:
Result = (rU/rS) × (CS/L) × V × 100
Tolerances:
NLT 75% (Q) of the labeled amount of fluconazole is dissolved.
• Uniformity of Dosage Units 905:
Meet the requirements
ADDITIONAL REQUIREMENTS
• Packaging and Storage:
Preserve in well-closed containers. Store at controlled room temperature.
• Labeling:
When more than one Dissolution test is given, the labeling states the Dissolution test used only if Test 1 is not used.
Auxiliary Information
Please check for your question in the FAQs before contacting USP.
USP35NF30 Page 3208
Pharmacopeial Forum: Volume No. 34(4) Page 932
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