Prednisolone Tebutate

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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C₂₇H₃₈O₆ (USP 1-Aug-2022) 458.59

Pregna-1,4-diene-3,20-dione, 11,17-dihydroxy-21-(3,3-dimethyl-1-oxobutyl)oxy-, (11β)-;

11β,17,21-Trihydroxypregna-1,4-diene-3,20-dione 21-(3,3-dimethylbutyrate)  CAS RN^®: 7681-14-3; UNII: 1V7A1U282K.

1 DEFINITION

Prednisolone Tebutate contains NLT 97.0% and NMT 103.0% of prednisolone tebutate (C₂₇H₃₈O₆), calculated on the dried basis.

2 IDENTIFICATION

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2.1 A. Spectroscopic Identification Tests 〈197〉, Infrared Spectroscopy: 197M (USP 1-Aug-2022)

Sample: Dissolve a portion of Prednisolone Tebutate in acetone and evaporate to dryness, then dry at a pressure not exceeding 5 mm of mercury at 105° for 4 h.

Acceptance criteria: Meets the requirements (USP 1-Aug-2022)

2.2 B. Spectroscopic Identification Tests 〈197〉, Ultraviolet-Visible Spectroscopy: 197U

Analytical wavelength: 242 nm

Sample solution: 20 µg/mL in methanol

Acceptance criteria: Absorptivities, calculated on the dried basis, differ by NMT 3.0%

3 ASSAY

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3.1 Procedure

Mobile phase: Isooctane, tetrahydrofuran, and alcohol (89:10:1)

Diluent: Isooctane and tetrahydrofuran (50:50)

Standard solution: 1 mg/mL of USP Prednisolone Tebutate RS in Diluent

Sample solution: 1 mg/mL of Prednisolone Tebutate in Diluent

Chromatographic system

(See Chromatography 〈621〉, System Suitability.) (USP 1-Aug-2022)

Mode: LC

Detector: UV 254 nm

Column: 3.9-mm × 30-cm; packing L3

Column temperature: 25°

Flow rate: 1.0 mL/min

Injection volume: 25 µL

Run time: NLT 1.5 times the retention time of prednisolone tebutate

System suitability

Sample: Standard solution

[Note—The retention time for prednisolone tebutate is about 30 min.]

Suitability requirements

Relative standard deviation: NMT 1.5%

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of prednisolone tebutate (C₂₇H₃₈O₆) in the portion of Prednisolone Tebutate taken:

Result = (r_U/r_S) × (C_S/C_U) × 100

r_U = peak area of prednisolone tebutate from the Sample solution

r_S = peak area of prednisolone tebutate from the Standard solution

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

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

Acceptance criteria: 97.0%–103.0% on the dried basis

4 IMPURITIES

Residue on Ignition 〈281〉: NMT 0.1%

Delete the following:

Selenium 〈291〉

Sample: 200 mg of Prednisolone Tebutate

Acceptance criteria: 0.003% (USP 1-Aug-2022)

5 SPECIFIC TESTS

Optical Rotation 〈781S〉, Procedures, Specific Rotation

Sample solution: 10 mg/mL in chloroform

Acceptance criteria: +100° to +115°

Loss on Drying 〈731〉

Analysis: Dry at a pressure not exceeding 5 mm of mercury at 105° for 4 h.

Acceptance criteria: NMT 5.0%

6 ADDITIONAL REQUIREMENTS

Packaging and Storage: Preserve in tight containers sealed under sterile nitrogen, in a cold place.

USP Reference Standards 〈11〉

USP Prednisolone Tebutate RS