Hydrocortisone Valerate

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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C₂₆H₃₈O₆ 446.58 

Pregn-4-ene-3,20-dione, 11,21-dihydroxy-17-[(1-oxopentyl)oxy]-, (11β)-; 

Cortisol 17-valerate; 

11β,17,21-Trihydroxypregn-4-ene-3,20-dione 17-valerate CAS RN®: 57524-89-7; UNII: 68717P8FUZ. 

1 DEFINITION 

Hydrocortisone Valerate contains NLT 97.0% and NMT 102.0% of hydrocortisone valerate (C₂₆H₃₈O₆), calculated on the dried basis

2 IDENTIFICATION 

Change to read: 

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

3 ASSAY 

Procedure 

Mobile phase: Acetonitrile and water (45:55) 

Internal standard solution: 2.0 mg/mL of ethyl benzoate in methanol 

Standard stock solution: 0.5 mg/mL of USP Hydrocortisone Valerate RS in methanol. Prepare immediately before use. Standard solution: 0.1 mg/mL of USP Hydrocortisone Valerate RS in methanol, prepared as follows. Pipet 2 mL of the Standard stock solution and 2 mL of the Internal standard solution into a 10-mL volumetric flask, and dilute with methanol to volume. Sample stock solution: 1 mg/mL of Hydrocortisone Valerate in methanol 

Sample solution: 0.1 mg/mL of Hydrocortisone Valerate in methanol, prepared as follows. Pipet 1 mL of the Sample stock solution and 2 mL of the Internal standard solution into a 10-mL volumetric flask, and dilute with methanol to volume. 

Chromatographic system 

(See Chromatography 〈621〉, System Suitability.) 

Mode: LC 

Detector: UV 254 nm 

Column: 3.9-mm × 30-cm; packing L1 

Flow rate: 1 mL/min 

Injection volume: 10 µL 

System suitability 

Sample: Standard solution 

[Note—The relative retention times for ethyl benzoate and hydrocortisone valerate are about 0.8 and 1.0, respectively.] Suitability requirements 

Resolution: NLT 3.0 between ethyl benzoate and hydrocortisone valerate 

Relative standard deviation: NMT 2.0% 

Analysis 

Samples: Standard solution and Sample solution 

Calculate the percentage of hydrocortisone valerate (C₂₆H₃₈O₆) in the portion of Hydrocortisone Valerate taken: 

Result = (R_U/R_S ) × (C_S /C_U) × 100 

R_U = peak area ratio of the free hydrocortisone valerate to the internal standard from the Sample solution 

R_S = peak area ratio of the free hydrocortisone valerate to the internal standard from the Standard solution 

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

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

Acceptance criteria: 97.0%–102.0% on the dried basis 

4 SPECIFIC TESTS 

Loss on Drying 〈731〉 

Sample: Dry at 105° for 3 h. 

Acceptance criteria: NMT 1.0% 

Optical Rotation, Specific Rotation〈781S〉 

Sample: 10 mg/mL in dioxane 

Acceptance criteria: +37° to +43° 

5 ADDITIONAL REQUIREMENTS 

Packaging and Storage: Preserve in well-closed containers. 

USP Reference Standards 〈11〉 

USP Hydrocortisone Valerate RS