Halcinonide

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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C₂₄H₃₂CIFO₅ 454.96

Pregn-4-ene-3,20-dione, 21-chloro-9-fluoro-11-hydroxy-16,17-[(1-methylethylidene)bis(oxy)]-, (11β,16α)-;

21-Chloro-9-fluoro-11β,16α,17-trihydroxypregn-4-ene-3,20-dione cyclic 16,17-acetal with acetone CAS RN^®: 3093-35-4; UNII: SI86V6QNEG.

1 DEFINITION

Halcinonide contains NLT 97.0% and NMT 102.0% of halcinonide (C₂₄H₃₂CIFO₅).

2 IDENTIFICATION

Change to read:

A. SPECTROSCOPIC IDENTIFICATION TESTS (197), Infrared Spectroscopy: 197K (CN 1-MAY-2020)

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

Mobile phase: Acetonitrile and water (50:50)

Diluent: Acetonitrile and water (2:1)

Standard solution: 0.3 mg/mL of USP Halcinonide RS in Diluent

Sample solution: 0.3 mg/mL of Halcinonide in Diluent. [NOTE-Sonication may be needed to aid in the dissolution of the Standard solution and Sample solution.]

3.2 Chromatographic system

(See Chromatography (621), System Suitability.)

Mode: LC

Detector: UV 240 nm

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

Flow rate: 2 mL/min

Injection volume: 20 µL

3.3 System suitability

Sample: Standard solution

Suitability requirements

Tailing factor: NMT 1.5

Relative standard deviation: NMT 0.85% for six replicate injections

3.4 Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of halcinonide (C₂₄H₃₂CIFO₅) in the portion of Halcinonide taken:

Result = (r_U/r_S) x (C_S/C_U) x 100

r_U = peak response from the Sample solution

r_S = peak response from the Standard solution

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

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

Acceptance criteria: 97.0%-102.0%

4 IMPURITIES

4.1 RESIDUE ON IGNITION (281)

NMT 0.2%

4.2 ORGANIC IMPURITIES

Solution A: 10 mM of ammonium acetate in water

Solution B: Acetonitrile

Mobile phase: See Table 1.

Table 1

Diluent 1: Acetonitrile and water (60:30)

Diluent 2: Acetonitrile and water (10:90)

Standard stock solution: 0.2 mg/mL of USP Halcinonide RS in Diluent 1

Standard solution: 0.1 µg/mL of USP Halcinonide RS from Standard stock solution in Diluent 2

Sample stock solution: 0.2 mg/mL of Halcinonide in Diluent 1

Sample solution: 0.1 mg/mL of Halcinonide from Sample stock solution in Diluent 2

Chromatographic system

(See Chromatography (621), System Suitability.)

Mode: LC

Detector: UV 240 nm

Column: 2.1-mm × 15-cm; 1.7-µm packing L1

Flow rate: 0.3 mL/min

Injection volume: 10 µL

System suitability

Sample: Standard solution

[NOTE-See Table 2 for the relative retention times.]

Suitability requirements

Relative standard deviation: NMT 2.8%

Signal-to-noise ratio: NLT 50

Analysis

Samples: Standard solution and Sample solution

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

Result = (r_U/r_S) x (C_S/C_U) x 100

r_U = peak response of each individual unspecified impurity from the Sample solution

r_S = peak response of halcinonide from the Standard solution

C_S = concentration of USP Halcinonide RS in the Standard solution (µg/mL)

C_U = concentration of Halcinonide in the Sample solution (µg/mL)

Acceptance criteria: See Table 2.

Table 2

^a 9-Fluoro-11β,16α,17,21-tetrahydroxypregna-4-ene-3,20-dione.

5 SPECIFIC TESTS

5.1 OPTICAL ROTATION, Specific Rotation(781S)

Sample solution: 20 mg/mL in chloroform

Acceptance criteria: +150° to +160°

5.2 LOSS ON DRYING (731)

Analysis: Dry under vacuum at 100° for 3 h.

Acceptance criteria: NMT 1.0%

6 ADDITIONAL REQUIREMENTS

6.1 PACKAGING AND STORAGE

Preserve in well-closed containers.

6.2 USP REFERENCE STANDARDS (11)

USP Halcinonide RS