Etravirine 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

Etravirine Tablets contain NLT 90.0% and NMT 110.0% of the labeled amount of etravirine(C₂₀H₁₅BrN₆O).

2 IDENTIFICATION

A. SPECTROSCOPIC IDENTIFICATION TESTS (192), Infrared Spectroscopy: 197K or 1974

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

PROCEDURE

Protect solutions containing etravirine from light.

Buffer: 10 mM ammonium formate in water

Diluent: Acetonitrile and Buffer (50:50, v/v)

Solution A: 50 mM formic acid in Buffer

Solution B: Acetonitrile

Solution C: Methanol

Mobile phase: See Table 1.

Standard solution: 0.10 mg/mL of USP Etravirine RS prepared as follows. Transfer a suitable amount of USP Etravirine BS to a suitable volumetric flask and dissolve in 5% of the total volume of 1-methyl-2-pyrrolidone. Dilute with Diluent to volume.

Sample solution: Nominally 0.10 mg/ml, of etravirine in Diluent prepared as follows. Transfer a portion equivalent to NLT 50 mg of etravirine from finely powdered Tablets (NLT 20) to a suitable volumetric flask. Add 5% of the flask volume of Diluent and shake for 5 min. Add 5% of the flask volume of 1-methyl-2-pyrrolidong and shake for 30 min. Dilute with Diluent to volume. Allow the solution to stand for 4 h at room temperature. Pass a portion of the solution through a suitable filter of 0.45-um pore size, and use the clear filtrate.

Chromatographic system

(See Chromatography (621), System Suitability)

Mode: LC

Detector: UV 310 nm

Column: 3.0-mm × 15-cm; 5-μm packing L1

Column temperature: 35°

Flow rate: 0.6 mL/min

Injection volume: 10 μL

System suitability

Sample: Standard solution

Suitability requirements

Tailing factor: NMT 1.5

Relative standard deviation: NMT 1.0%

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of etravirine (C₂₀H₁₅BrN₆O) in the portion of Tablets taken

Result = (r_U/(r_S) × (C_S /C_U) x 100

r_U = peak response of etravirine from the Sample solution

r_S = peak response of etravirine from the Standard solution

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

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

Acceptance criteria: 90.0%-110.0%

4 PERFORMANCE TESTS

DISSOLUTION (711)

Protect solutions containing etravirine from light.

Solution A: 0.01 M bydrochloric acid

Solution B: 2.25% sodium lauryl sulfate in Solution A

Medium

For Tablets labeled to contain 25 and 100 mg: 500 ml of Solution A and 400 ml of Solution B

For Tablets labeled to contain 200 mg: 1000 ml of Solution A and 800 mL of Solution B

Apparatus 2

For Tablets labeled to contain 25 and 100 mg: 50 rpm

For Tablets labeled to contain 200 mg: 70 rpm

Time

For Tablets labeled to contain 25 and 100 mg: 45 min

For Tablets labeled to contain 200 mg: 30 min

Mobile phase: Acetonitrile and 0.5% phosphoric acid (65:35)

Standard solution: 0.111 mg/ml. of USP Etravirine RS in Medium for Tablets labeled to contain 100 and 200 mg; 0.0278 mg/ml. of USP Etravirine RS in Medium for Tablets labeled to contain 25 mg, prepared as follows. Transfer a suitable amount of USP Etravirine RS to a suitable volumetric flask and dissolve in 5% of the total volume of 1-methyl-2-pyrrolidone. Add acetonitrile to 50% of the total volume, equilibrate to room temperature, and dilute with Solution B to volume.

Sample solution: Place 1 Tablet in each vessel filled with a volume of Solution A as specified in Mediurn. After 10 min, add a volume of preheated Solution B as specified in Medium and reset the time to zero. Pass a portion of the solution under test through a suitable filter of 0.45-µm pore size.

Chromatographic system

(See Chromatography (621) System Suitability)

Mode: LC

Detector: UV 260 mm

Column: 3.0-mm × 5.0-cm; 5-μm packing L1

Column temperature: 35°

Flow rate: 0.5 mL/min

Injection volume

For Tablets labeled to contain 25 mg: 40 μL

For Tablets labeled to contain 100 and 200 mg: 10 μL

Run time: NLT 2 times the retention time of etravirine

System suitability

Sample: Standard solution

Suitability requirements

Tailing factor: NMT 2.0

Relative standard deviation NMT 2.0%

Analysis

Samples: Samdant acution and Sample solution

Calculate the percentage of the labeled amount of etravirine (C₂₀H₁₅BrN₆O) dissolved:

Result = (r_U/(r_S) × (C_S /L) x 100

r_U = peak response of etravirine from the Sample solution

r_S = peak response of etravirine from the Standard solution

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

L = label claim (mg/Tablet)

V = volume of Medium; 900 mL for Tablets labeled to contain 25 and 100 mg; 1800 mL for Tablets labeled to contain 200 mg

Tolerances: NLT 80% (0) of the labeled amount of etravirine (CH BND) is drescived

Uurostar Donar Uwers (905): Meet the requinements

5 IMPURITIES

Protect solutions ntaining elraviime from light

Buffer, Diluent, Solution A, Solution B, Solution C, Mobile phase, Standard solution, Sample solution, and Chromatographic

system: Proceed as directed in the Assay

System suitability solution: 0.10 mg/mL of ISP Evinine Sistem Suitability Misture RS prepared as follows. Transfer a suitable amount of LSP Ettastrine Salum Saltability Mixture 85 to a sutable volumetric flask and duschie in 10% of the total volume of 12-xmalidong Dilute with Dilvent to volume

Sensitivity solution: 0.05 g/ml. of LSP Etrasinne RS from the Standard solution in Dent

System suitability

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

Sultability requirements

Resolution: NLT 4.3 between the etraccine amino analog (4-4-Amino-5-bromo-6-chloropyrimidin-2-yl)aminobenzonitrile) and distrometrasirine (4-116-amino-2-4-cyanophenyl)amesseymidin-4-yly-3,5 dimethylbenzonitrile), with pakos at relative retention times of 0.56 and 0.73, respectively. System subalty solution

Relative standard deviation: NMT 1.0, Standard solution

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

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) × (C_S /C_U) x 100

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

r_S = peak response of etravirine from the Standard solution

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

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

Acceptance criteria: The reporting threshold is 0.1%.

Any unspecified degradation product: NMT 0.20%.

Total degradation products: NMT 0.50%.

6 ADDITIONAL REQUIREMENTS

PNS AND Sass Presserve in tight containers, protect from mastare, and share at controlled room temperature.