Sulconazole Nitrate

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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C₁₈H₁₅Cl₃N₂OS · HNO₃ 460.76

1H-Imidazole, 1-[2-[[(4-chlorophenyl)methyl]thio]-2-(2,4-dichlorophenyl)ethyl]-, mononitrate, (±)-;

(±)-1-[2,4-Dichloro-β-[(p-chlorobenzyl)thio] phenethyl]imidazole mononitrate CAS RN®: 61318-91-0; UNII: 1T89100D5U.

1 DEFINITION

Sulconazole Nitrate contains NLT 98.0% and NMT 102.0% of sulconazole nitrate (C₁₈H₁₅Cl₃N₂OS · HNO₃), calculated on the dried basis.

2 IDENTIFICATION

Change to read:

A. Spectroscopic Identification Tests 〈197〉, Infrared Spectroscopy: 197K (CN 1-May-2020)

B. Identification Tests—General 〈191〉, Nitrate: Meets the requirements of test A

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

3 ASSAY

Procedure

Buffer: Dissolve 7.7 g of ammonium acetate in 992 mL of water and add 3.3 mL of glacial acetic acid. Pass through a suitable fIlter of 0.45- μm pore size under vacuum and degas with helium purging.

Solution A: Methanol, water, and Buffer (200:640:160)

Solution B: Methanol and acetonitrile (40:60)

Mobile phase: See Table 1.

Table 1

Diluent: Methanol and water (60:40)

Standard solution: 0.15 mg/mL of USP Sulconazole Nitrate RS in Diluent, prepared as follows. Transfer an appropriate quantity of USP

Sulconazole Nitrate RS to a suitable volumetric flask, dissolve in 80% of the flask volume of Diluent, sonicate until dissolved, and dilute with

Diluent to volume.

Sample solution: 0.15 mg/mL of Sulconazole Nitrate in Diluent, prepared as follows. Transfer an appropriate quantity of Sulconazole Nitrate to a suitable volumetric flask, dissolve in 80% of the flask volume of Diluent, sonicate until dissolved, and dilute with Diluent to volume.

Chromatographic system

(See Chromatography 〈621〉, System Suitability.)

Mode: LC

Detector: UV 230 nm

Column: 2.1-mm × 10-cm; 1.7-μm packing L1

Flow rate: 0.5 mL/min

Injection volume: 5 μL

System suitability

Sample: Standard solution

Suitability requirements

Tailing factor: NMT 2.0

Relative standard deviation: NMT 0.73%

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of sulconazole nitrate (C₁₈H₁₅Cl₃N₂OS · HNO₃) in the portion of Sulconazole Nitrate taken:

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

r_U = peak response from the Sample solution

r_S = peak response from the Standard solution

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

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

Acceptance criteria: 98.0%–102.0% on the dried basis

4 IMPURITIES

Residue on Ignition 〈281〉: NMT 0.1%

Organic Impurities

Buffer, Solution A, Solution B, Mobile phase, Diluent, and Chromatographic system: Proceed as directed in the Assay.

Standard solution: 1.5 μg/mL each of USP Sulconazole Nitrate RS and USP Sulconazole Related Compound A RS in Diluent, prepared as follows. Transfer appropriate quantities of USP Sulconazole Nitrate RS and USP Sulconazole Related Compound A RS to a suitable volumetric flask, dissolve in 80% of the flask volume of Diluent, sonicate until dissolved, and dilute with Diluent to volume.

Sample solution: 1.5 mg/mL of Sulconazole Nitrate in Diluent, prepared as follows. Transfer an appropriate quantity of Sulconazole Nitrate to a suitable volumetric flask, dissolve in 80% of the flask volume of Diluent, sonicate until dissolved, and dilute with Diluent to volume.

System suitability

Sample: Standard solution

[Note—See Table 2 for relative retention times.]

Suitability requirements

Relative standard deviation: NMT 2.0% for sulconazole nitrate and sulconazole related compound A

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of sulconazole related compound A in the portion of Sulconazole Nitrate taken:

Result = (r_U/r_S) × (C_S/C_U) × 100

r_U = peak response of sulconazole related compound A from the Sample solution

r_S = peak response of sulconazole related compound A from the Standard solution

C_S = concentration of USP Sulconazole Related Compound A RS in the Standard solution (mg/mL)

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

Calculate the percentage of any individual unspecified impurity in the portion of Sulconazole Nitrate taken:

Result = (r_U/r_S) × (C_S/C_U) × 100

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

r_S = peak response of sulconazole nitrate from the Standard solution

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

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

Acceptance criteria: See Table 2.

Table 2

5 SPECIFIC TESTS

Loss on Drying 〈731〉

Analysis: Dry under vacuum at 80° for 3 h.

Acceptance criteria: NMT 1.0%

6 ADDITIONAL REQUIREMENTS

Packaging and Storage: Preserve in well-closed containers, protected from light.

USP Reference Standards 〈11〉

USP Sulconazole Nitrate RS

USP Sulconazole Related Compound A RS

1-[2-(4-Chlorobenzyl)sulfinyl-2-(2,4-dichlorophenyl)ethyl]-1H-imidazole.

C₁₈H₁₅Cl₃N₂OS 413.74