Ergotamine Tartrate Sublingual Tablets

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

Ergotamine Tartrate Sublingual Tablets contain NLT 90.0% and NMT 110.0% of the labeled amount of ergotamine tartrate [(C₃₃H₃₅N₅O₅)₂ · C₄H₆O₆].

2 IDENTIFICATION

A.

Solution A: Shake chloroform with ammonium hydroxide, draw off the chloroform layer, and use the chloroform saturated with ammonia.

Solution B: Combine equal volumes of glacial acetic acid and ethyl acetate.

Solution C: Combine equal volumes of ferric chloride TS and water.

Sample solution: Triturate a portion of finely powdered Tablets, equivalent to 5 mg of ergotamine tartrate, with 10 mL of solvent hexane for a few min. Allow to settle, and discard the solvent hexane extract. To the residue add 10 mL of Solution A, triturate for a few min, filter, and evaporate the filtrate on a steam bath to dryness. Dissolve the residue in 8 mL of Solution B.

Analysis

Sample: Sample solution

Part 1: To 1 mL of Sample solution add slowly, with continuous agitation and cooling, 1 mL of sulfuric acid.

Part 2: To the resulting solution from Part 1, add 0.1 mL of Solution C.

Acceptance criteria: Both criteria for Part 1 and Part 2 must be met.

Part 1: A blue color with a red tinge develops.

Part 2: The red tinge becomes less apparent and the blue color more pronounced.

3 ASSAY

PROCEDURE

Mobile phase: Acetonitrile and 0.01 M monobasic potassium phosphate (55:45)

Diluent: Acetonitrile and water (55:45)

Internal standard solution: 0.16 mg/mL of ergonovine maleate in Diluent

Standard stock solution: 0.2 mg/mL of USP Ergotamine Tartrate RS in Diluent

Standard solution: 0.02 mg/mL of USP Ergotamine Tartrate RS from Standard stock solution and 0.016 mg/mL of ergonovine maleate from Internal standard solution prepared as follows. Transfer 5.0 mL of Standard stock solution to a 50-mL volumetric flask, add 5.0 mL of Internal standard solution, and dilute with Diluent to volume.

Sample solution: Nominally 0.02 mg/mL of ergotamine tartrate from Tablets prepared as follows. Transfer a number of whole Tablets, equivalent to 10 mg of ergotamine tartrate, to a 500-mL volumetric flask. Add 50.0 mL of Internal standard solution and 300 mL of Diluent. Sonicate for 10 min, and dilute with Diluent to volume. Pass through a membrane disk of 0.45-µm pore size, discarding the first 25 mL of the filtrate.

Chromatographic system

(See Chromatography, System Suitability (621).)

Mode: LC

Detector: UV 254 nm

Column: 3.9-mm x 30-cm; packing L1

Flow rate: 1 mL/min

Injection volume: 20 µL

System suitability

Sample: Standard solution

[NOTE-The relative retention times for ergonovine maleate and ergotamine tartrate are about 0.7 and 1.0, respectively.]

Suitability requirements

Resolution: NLT 3.0 between the ergotamine tartrate and ergonovine maleate

Column eciency: NLT 3000 theoretical plates for ergotamine tartrate

Tailing factor: NMT 2.0 for ergotamine tartrate

Relative standard deviation: NMT 2.0%

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of ergotamine tartrate [(C₃₃H₃₅N₅O₅)₂ · C₄H₆O₆] in the portion of Tablets taken:

Result = (R_u /R_s ) × (C_s /C_u ) × 100

R_u = peak response ratio of ergotamine tartrate to the internal standard from the Sample solution

R_s = peak response ratio of ergotamine tartrate to the internal standard from the Standard solution

C_s = concentration of USP Ergotamine Tartrate RS in the Standard solution (mg/mL)

C_u = nominal concentration of ergotamine tartrate in the Sample solution (mg/mL)

Acceptance criteria: 90.0%–110.0%

4 PERFORMANCE TESTS

DISINTEGRATION (701): 5 min

UNIFORMITY OF DOSAGE UNITS (905): Meet the requirements

ADDITIONAL REQUIREMENTS

PACKAGING AND STORAGE: Preserve in well-closed, light-resistant containers. Store at 25^o, excursions permitted between 15° and 30°.

LABELING: Label Tablets to indicate that they are intended for sublingual administration.

USP REFERENCE STANDARDS (11)

USP Ergotamine Tartrate RS