Desonide

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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C₂₄H₃₂O₆              416.51

Pregna-1,4-diene-3,20-dione, 11,21-dihydroxy-16,17-[(1-methylethylidene)bis(oxy))-, (118,16α)-;

118,16,17,21-Tetrahydroxypregna-1,4-diene-3,20-dione cyclic 16,17-acetal with acetone CAS RN^®: 638-94-8; UNII: J280872010.

1 DEFINITION

Desonide contains NLT 98.0% and NMT 102.0% of the labeled amount of desonide (C₂₄H₃₂O₆), calculated on the dried basis.

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

Use low-actinic glassware for all solutions containing desonide.

Solution A: 0.1% Phosphoric acid in water

Solution B: Acetonitrile

Mobile phase: See Table 1.

Table 1

Diluent: Solution A and acetonitrile (60:40)

System suitability solution: 0.7 mg/mL of USP Desonide Impurities Mixture RS in Diluent

Standard solution: 0.7 mg/mL of USP Desonide RS in Diluent

Sample solution: 0.7 mg/mL of Desonide in Diluent

3.1.1 Chromatographic system

(See Chromatography (621), System Suitability.)

Mode: LC

Detector: UV 254 nm

Column: 4.6-mm x 15-cm; 2.6-µm packing L7

3.1.2 Temperatures

Column: 20° (15°-22° was shown to be acceptable)

Autosampler: 20°

Flow rate: 1 mL/min

Injection volume: 5 µL

3.1.3 System suitability

Samples: System suitability solution and Standard solution

3.1.4 Suitability requirements

Resolution: NLT 2.0 between desonide glyoxal and deoxyprednisolone-16-ene; NLT 2.0 between desonide and dihydrodesonide, System suitability solution

Relative standard deviation: NMT 0.73%, Standard solution

3.1.5 Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of desonide (C₂₄H₃₂O₆) in the portion of Desonide taken:

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

r_U = peak response from the Sample solution

r_S = peak response from the Standard solution s

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

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

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

4 IMPURITIES

4.1 RESIDUE ON IGNITION (281): NMT 0.10%

4.2 ORGANIC IMPURITIES

Solution A, Solution B, Mobile phase, Diluent, System suitability solution, Standard solution, Sample solution, and Chromatographic system: Proceed as directed in the Assay.

Sensitivity solution: 0.28 µg/mL of USP Desonide RS in Diluent from the Standard solution

4.2.1 System suitability

Samples: System suitability solution and Sensitivity solution

4.2.2 Suitability requirements

Resolution: NLT 2.0 between desonide glyoxal and deoxyprednisolone-16-ene; NLT 2.0 between desonide and dihydrodesonide, System suitability solution

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

4.2.3 Analysis

Sample: Sample solution

Calculate the percentage of each impurity in the portion of Desonide taken:

                Result = (r_U/r_T) x (1/F) x 100

r_U = peak area of each impurity from the Sample solution

r_T = total peak area from the Sample solution

F = relative response factor (see Table 2)

Acceptance criteria: See Table 2.

[NOTE-Disregard peaks that are less than 0.04% of the desonide peak from the Standard solution.]

Table 2 
 

^a 11ẞ,16α,17,21-Tetrahydroxy-3,20-dioxopregna-1,4-diene.

^b 11ẞ,17,21-Trihydroxy-3,20-dioxopregna-1,4-diene.

^c 11ẞ-Hydroxy-16α,17-[(1-methylethylidene)bis(oxy)]-3,20-dioxopregna-1,4-dien-21-al.

^d 11ẞ,21-Dihydroxypregna-1,4,16-triene-3,20-dione.

^e 11ẞ,21-Dihydroxy-16α, 17-[(1-methylethylidene)bis(oxy)]pregn-4-ene-3,20-dione.

^f 11ẞ-Epoxy-21-hydroxy-16α, 17-(1-methylethylidenedioxy)pregna-1,4-diene-3,20-dione.

^g 9α-Bromo-113,21-dihydroxy-16α, 17-[(1-methylethylidene)bis(oxy)]pregna-1,4-diene-3,20-dione.

^h 11ẞ-Hydroxy-16α,17-[(1-methylethylidene)bis(oxy)]-3,20-dioxopregna-1,4-dien-21-yl acetate.

5 SPECIFIC TESTS

5.1 LOSS ON DRYING (731)

Sample: 1.0 g

Analysis: Dry at 105° for 3 h.

Acceptance criteria: NMT 0.5%

5.2 OPTICAL ROTATION, Specific Rotation (781S)

Sample: 10 mg/mL in dioxane

Acceptance criteria: +104.0° to +110.0°, calculated on the dried basis

6 ADDITIONAL REQUIREMENTS

PACKAGING AND STORAGE: Preserve in tight containers, and store at controlled room temperature. Protect from light.

USP REFERENCE STANDARDS (11)

USP Desonide RS

USP Desonide Impurities Mixture RS

This is a mixture that contains desonide and may contain about 1% each of 16a-hydroxyprednisolone, Prednisolone, desonide glyoxal, deoxyprednisolone-16-ene, dihydrodesonide, epoxydesonide, bromodesonide, and acetyldesonide.