Dihydroergotamine Mesylate Injection

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 

Dihydroergotamine mesylate Injection is a sterile solution of Dihydroergotamine Mesylate in Water for Injection. It contains NLT 90.0% and NMT 110.0% of the labeled amount of dihydroergotamine mesylate (C₃₃H₃₇N₅O₅ . CH₄O₃S). 

2 IDENTIFICATION 

A. 

Sample solution: 2 mL of Injection in 25 mL water 

Acceptance criteria: The UV absorption spectrum of the Sample solution exhibits maxima and minima at the same wavelengths as those of a similar solution of USP Dihydroergotamine Mesylate RS. 

3 ASSAY 

3.1 Procedure 

Diluent: 10 mg/mL of tartaric acid in water 

Solution A: Dissolve 250 mg of p-dimethylaminobenzaldehyde in a cooled mixture of 130 mL of sulfuric acid and 70 mL of water, and add 0.40 mL of ferric chloride solution (1 in 20). 

Standard solution: 50 µg/mL of USP Dihydroergotamine Mesylate RS in Diluent 

Sample solution: Nominally 50 µg/mL of dihydroergotamine mesylate from a suitable volume of Injection containing NLT 5 mg of dihydroergotamine mesylate in Diluent 

Blank: Diluent 

Instrumental conditions 

Mode: Vis 

Analytical wavelength: 585 nm 

Cell: 1 cm 

Analysis 

Samples: Standard solution, Sample solution, and Blank 

Transfer 5.0 mL each of the Standard solution, the Sample solution, and the Blank to separate 50-mL conical asks. Add 10.0 mL of Solution A to each ask, shake, and allow to stand for 30 min. Measure the absorbance of the resulting Standard solution and Sample solution against the Blank. 

Calculate the percentage of the labeled amount of dihydroergotamine mesylate (C₃₃H₃₇N₅O₅ . CH₄O₃S) in the portion of Injection taken: 

Result = (A_u/A_s) × (C_s/C_u) × 100 

A_u = absorbance of the Sample solution 

A_s = absorbance of the Standard solution 

C_s = concentration of USP Dihydroergotamine Mesylate RS in the Standard solution (µg/mL) 

C_u = nominal concentration of dihydroergotamine mesylate in the Sample solution (µg/mL) 

Acceptance criteria: 90.0%–110.0% 

4 SPECIFIC TESTS 

Bacterial Endotoxins Test 〈85〉: NMT 175.0 USP Endotoxin Units/mg of dihydroergotamine mesylate 

pH 〈791〉: 3.4–4.9 

Other Requirements: It meets the requirements in Injections and Implanted Drug Products 〈1〉. 

5 ADDITIONAL REQUIREMENTS 

Packaging and Storage: Preserve in single-dose containers, preferably of Type I glass, and protect from light. 

USP Reference Standards 〈11〉 

USP Dihydroergotamine Mesylate RS