Gemifloxacin Tablets

This article is compiled based on the United States Pharmacopeia (USP) – 2025 Edition

Issued and maintained by the United States Pharmacopeial Convention (USP)

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1 DEFINITION

Gemifloxacin Tablets contain an amount of gemifloxacin mesylate equivalent to NLT 90.0% and NMT 110.0% of the labeled amount of gemifloxacin (C₁₈H₂₀FN₅O₄).

2 IDENTIFICATION

A. SPECTROSCOPIC IDENTIFICATION TESTS (197), Infrared Spectroscopy: 197A or 197M

B. The retention time of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.

3 ASSAY

3.1 PROCEDURE

Store the solutions in amber vials and protect from light.

Buffer: 138 g/L of monobasic sodium phosphate in water

Mobile phase: Acetonitrile, water, and trifluoroacetic acid (20:80:0.1)

Diluent: Acetonitrile, water, and Buffer (20:72:8)

Standard solution: 0.17 mg/mL of USP Gemifloxacin Mesylate RS in Diluent

Sample stock solution: Nominally 0.64 mg/mL of gemifloxacin from a portion of finely powdered Tablets in Diluent prepared as follows. Finely powder NLT 20 Tablets. Transfer a suitable portion of the powder to a suitable volumetric flask. Add Diluent using 70% of the final volume, shake it for 15 min, and then sonicate for about 30 min. Allow the solution to cool, if necessary, and dilute with Diluent to volume.

Sample solution: Nominally 0.13 mg/mL of gemifloxacin from the Sample stock solution in Diluent

3.2 Chromatographic system

(See Chromatography (621), System Suitability.)

Mode: LC

Detector: UV 272 nm

Column: 4.6-mm × 25-cm; 5-µm packing L1

Column temperature: 30°

Flow rate: 1 mL/min

Injection volume: 20 µL

Run time: NLT 1.3 times the retention time of the gemifloxacin peak

System suitability

Sample: Standard solution

Suitability requirements

Tailing factor: NMT 2.0

Relative standard deviation: NMT 1.0%

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of gemifloxacin (C₁₈H₂₀FN₅O₄) in the portion of Tablets taken:

Result = (r_U/r_S) x (C_S/C_U) x (M_r1/M_r2) x 100

r_U = peak response of gemifloxacin from the Sample solution

r_S = peak response of gemifloxacin from the Standard solution

C_S = concentration of USP Gemifloxacin Mesylate RS in the Standard solution (mg/mL)

C_U = nominal concentration of gemifloxacin in the Sample solution (mg/mL)

M_r1 = molecular weight of gemifloxacin, 389.38

M_r2 = molecular weight of gemifloxacin mesylate, 485.49

Acceptance criteria: 90.0%-110.0%

4 PERFORMANCE TESTS

4.1 DISSOLUTION (711)

Medium: 0.01 N hydrochloric acid; 900 mL

Apparatus 2: 50 rpm

Time: 30 min

Standard solution: 0.01 mg/mL of USP Gemifloxacin Mesylate RS in Medium

Sample solution: Pass a portion of the solution under test through a suitable filter of 0.45-µm pore size, and dilute with Medium to a concentration that is similar to the Standard solution.

Instrumental conditions

Mode: UV

Detector: 343 nm

Blank: Medium

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of gemifloxacin (C₁₈H₂₀FN₅O₄) dissolved:

Result = (A_U/A_S) x (C_S/L) x (M_r1/M_r2) x D x V x 100

A_U = absorbance of the Sample solution

A_S = absorbance of the Standard solution

C_S = concentration of USP Gemifloxacin Mesylate RS in the Standard solution (mg/mL)

L = label claim (mg/Tablet)

M_r1 = molecular weight of gemifloxacin, 389.38

M_r2 = molecular weight of gemifloxacin mesylate, 485.49

D = dilution factor of the Sample solution, as needed

V = volume of Medium, 900 mL

Tolerances: NLT 70% (Q) of the labeled amount of gemifloxacin (C₁₈H₂₀FN₅O₄) is dissolved.

4.2 UNIFORMITY OF DOSAGE UNITS (905)

Meet the requirements

5 IMPURITIES

Store the solutions in amber vials and protect from light.

ORGANIC IMPURITIES

Buffer, Mobile phase, Diluent, Standard solution, Sample stock solution, Sample solution, and Chromatographic system: Proceed as directed in the Assay.

System suitability solution: 0.5 mg/mL of USP Gemifloxacin Mesylate RS in Diluent

Sensitivity solution: 0.06 µg/mL of USP Gemifloxacin Mesylate RS in Diluent

System suitability

Samples: Standard solution, System suitability solution, and Sensitivity solution

Suitability requirements

Resolution: NLT 5.0 between E-gemifloxacin and gemifloxacin, System suitability solution

Tailing factor: NMT 2.0, Standard solution

Relative standard deviation: NMT 1.0%, Standard solution

Signal-to-noise ratio: NLT 10, Sensitivity solution

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of any individual impurity in the portion of Tablets taken:

Result = (r_U/r_S) x (C_S/C_U) x (M_r1/M_r2) x 100

r_U = peak response of any individual impurity from the Sample solution

r_S = peak response of gemifloxacin from the Standard solution

C_S = concentration of USP Gemifloxacin Mesylate RS in the Standard solution (mg/mL)

C_U = nominal concentration of gemifloxacin in the Sample solution (mg/mL)

M_r1 = molecular weight of gemifloxacin, 389.38

M_r2 = molecular weight of gemifloxacin mesylate, 485.49

Acceptance criteria: See Table 1. The reporting threshold is 0.1%.

Table 1

^a (E)-7-[3-(Aminomethyl)-4-(methoxyimino)pyrrolidin-1-yl]-1-cyclopropyl-6-fluoro-4-oxo-1,4-dihydro-1,8-naphthyridine-3-carboxylic acid monomethanesulfonate.

6 ADDITIONAL REQUIREMENTS

6.1 PACKAGING AND STORAGE

Preserve in tightly closed containers, protected from light. Store at controlled room temperature.

6.2 USP REFERENCE STANDARDS (11)

USP Gemifloxacin Mesylate RSA (USP 1-May-2022)