Gefitinib Tablets

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

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

DOWNLOAD PDF HERE

1 DEFINITION

Gefitinib Tablets contain NLT 90.0% and NMT 110.0% of the labeled amount of gefitinib (C₂₂H₂₄CIFN₄O₃).

2 IDENTIFICATION

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

B. The UV spectrum 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

Solution A: 9.7 g/L of ammonium acetate in water

Solution B: 0.2% trifluoroacetic acid in water

Mobile phase: Acetonitrile and Solution A (38:62)

Diluent: Acetonitrile and Solution B (40:60)

System suitability solution: 0.35 mg/mL of USP Gefitinib RS and 0.25 mg/mL of USP Dichloroaniline RS in Diluent. Sonicate to dissolve.

Standard solution: 0.35 mg/mL of USP Gefitinib RS in Diluent. Sonicate to dissolve.

Sample solution: Nominally 0.35 mg/mL of gefitinib prepared as follows. Transfer a suitable amount of the fine powder, equivalent to about 35 mg of gefitinib, from NLT 10 Tablets to a 100-mL volumetric flask. Add about 70 mL of Diluent and sonicate to dissolve. Dilute with Diluent to volume. Pass a portion of the solution through a suitable filter of 0.45-µm pore size. Discard the first few milliliters of filtrate.

3.2 Chromatographic system

(See Chromatography (621), System Suitability.)

Mode: LC

Detector: UV 247 nm. For Identification B, use a diode array detector in the range of 200-400 nm.

Column: 3.0-mm × 10-cm; 3-µm packing L1

Column temperature: 60°

Flow rate: 0.9 mL/min

Injection volume: 5 µL

Run time: NLT 5 times the retention time of gefitinib

3.3 System suitability

Samples: System suitability solution and Standard solution

Suitability requirements

Resolution: NLT 5.0 between dichloroaniline and gefitinib, System suitability solution

Tailing factor: NMT 1.5, Standard solution

Relative standard deviation: NMT 1.0%, Standard solution

3.4 Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of gefitinib (C₂₂H₂₄CIFN₄O₃) in the portion of Tablets taken:

Result = (r_U/r_S) x (C_S/C_U) x 100

r_U = peak response of gefitinib from the Sample solution

r_S = peak response of gefitinib from the Standard solution

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

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

Acceptance criteria: 90.0%-110.0%

4 PERFORMANCE TESTS

4.1 DISSOLUTION (711)

Medium: 5% Polysorbate 80 in water; 1000 mL

Apparatus 2: 50 rpm

Time: 45 min

Standard solution: 0.25 mg/mL of USP Gefitinib RS in Medium

Sample solution: Pass a portion of the solution under test through a suitable filter of 0.45-µm pore size, discarding the first few milliliters.

Blank: Medium

Instrumental conditions

(See Ultraviolet-Visible Spectroscopy. (857)..)

Mode: UV

Analytical wavelength: 334 nm

Cell: 1 mm

Analysis:

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of gefitinib (C₂₂H₂₄CIFN₄O₃) dissolved:

Result = (A_U/A_S) x C_S x V x (1/L) x 100

A_U = absorbance of the Sample solution

A_S = absorbance of the Standard solution

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

V = volume of Medium, 1000 mL

L = label claim (mg/Tablet)

Tolerances: NLT 80% (Q) of the labeled amount of gefitinib (C₂₂H₂₄CIFN₄O₃) is dissolved.

4.2 UNIFORMITY OF DOSAGE UNITS (905)

Meet the requirements

5 IMPURITIES

5.1 ORGANIC IMPURITIES

Solution A, Solution B, Mobile phase, Diluent, System suitability solution, Sample solution, and Chromatographic system: Proceed as directed in the Assay.

Standard stock solution: Use the Standard solution as prepared in the Assay.

Standard solution: 0.7 µg/mL of USP Gefitinib RS from the Standard stock solution in Diluent

Sensitivity solution: 0.18 µg/mL of USP Gefitinib RS from the Standard solution in Diluent

5.2 System suitability

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

[NOTE-The relative retention times for dichloroaniline and gefitinib are 0.7 and 1.0, respectively. These relative retention times are provided as information that could aid in peak assignment.]

Suitability requirements

Resolution: NLT 5.0 between dichloroaniline and gefitinib, System suitability solution

Relative standard deviation: NMT 5.0%, Standard solution

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

5.3 Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of any unspecified degradation product in the portion of Tablets taken:

Result = (r_U/r_S) x (C_S/C_U) x 100

r_U = peak response of any unspecified degradation product from the Sample solution

r_S = peak response of gefitinib from the Standard solution

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

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

Acceptance criteria: See Table 1. The reporting threshold is 0.05%.

Table 1

6 ADDITIONAL REQUIREMENTS

6.1 PACKAGING AND STORAGE

Preserve in tight containers. Store at controlled room temperature.

6.2 USP REFERENCE STANDARDS (11)

USP Dichloroaniline RS

3,4-Dichloroaniline.

C₆H₅CI₂N 162.01

USP Gefitinib RSA (USP 1-Aug-2024)