Desoxycorticosterone Pivalate Injectable Suspension

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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1 DEFINITION

Desoxycorticosterone Pivalate Injectable Suspension is a sterile suspension of Desoxycorticosterone Pivalate in an aqueous medium. It contains NLT 90.0% and NMT 110.0% of the labeled amount of desoxycorticosterone pivalate (C₂₆H₃₈O₄)

2 IDENTIFICATION

A.

Sample: Centrifuge a portion of Injectable Suspension, decant the supernatant, wash the residue by stirring with several successive portions of water, centrifuging and decanting each time, and finally dry the residue at 105°. The residue so obtained meets the following requirements.

Analysis 1: Melting point

Acceptance criteria 1: Melts at 198°-206°

Analysis 2: Dissolve 5 mg in 2 mL of sulfuric acid.

Acceptance criteria 2: The solution is yellowish, with a greenish fluorescence.

Analysis 3: Dilute the solution obtained from Analysis 2 with 2 mL of water.

Acceptance criteria 3: The color changes to a dark red-blue, and on further dilution with 2 ml of water, the color is discharged.

3 ASSAY

3.1 PROCEDURE

Mobile phase: Methanol and water (4:1)

Internal standard solution: 2 mg/ml of desoxycorticosterone acetate in methanol

Standard solution: 0.5 mg/mL of USP Desoxycorticosterone Pivalate RS in methanol, prepared as follows. Transfer 12.5 mg of USP Desoxycorticosterone Pivalate RS to a 25-mL volumetric flask, and add 20 mL of methanol. Add 2.5 mL of the Internal standard solution, and dilute with methanol to volume.

Sample solution: Nominally 0.5 mg/mL of desoxycorticosterone pivalate in methanol, prepared as follows. Transfer a nominal equivalent of 125 mg of desoxycorticosterone pivalate from Injectable Suspension to a 250-mL volumetric flask. Add 200 mL of methanol, and sonicate to dissolve. Add 25.0 mL of Internal standard solution, and dilute with methanol to volume. Centrifuge a 20-mL portion at high speed for 5 min. Filter the supernatant through a 5-µm disk, discarding the first 5 mL of the filtrate.

3.1.1 Chromatographic system

(See Chromatography (621), System Suitability.)

Mode: LC

Detector: UV 254 nm

Column: 4.6-mm x 25-cm; packing L7

Flow rate: 1.5 mL/min

Injection volume: 25 µL

3.1.2 System suitability

Sample: Standard solution

[NOTE-The relative retention times for desoxycorticosterone acetate and for desoxycorticosterone pivalate are about 0.5 and 1.0, respectively.]

3.1.3 Suitability requirements

Resolution: NLT 2.0 between desoxycorticosterone acetate and desoxycorticosterone pivalate

Relative standard deviation: NMT 1.5% for the peak response ratio of desoxycorticosterone pivalate to the internal standard

3.1.4 Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of desoxycorticosterone pivalate (C₂₆H₃₈O₄) in the portion of Injectable Suspension taken:

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

R_U = peak response ratio of desoxycorticosterone pivalate to the internal standard from the Sample solution

R_S = peak response ratio of desoxycorticosterone pivalate to the internal standard from the Standard solution

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

C_U = nominal concentration of desoxycorticosterone pivalate in the Sample solution (mg/mL)

Acceptance criteria: 90.0%-110.0%

4 SPECIFIC TESTS

PH (791): 5.0-7.0

OTHER REQUIREMENTS: It meets the requirements in Injections and Implanted Drug Products (1).

BACTERIAL ENDOTOXINS TEST (85): It contains NMT 2.78 USP Endotoxin Units/mg of desoxycorticosterone pivalate.

5 ADDITIONAL REQUIREMENTS

PACKAGING AND STORAGE: Preserve in single-dose or multiple-dose containers, preferably of Type I glass, protected from light.

LABELING: Label Suspension to indicate that it is for veterinary use only.

USP REFERENCE STANDARDS (11)

USP Desoxxcorticosterone Pivalate RS