Ergotamine Tartrate Tablets
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This article is compiled based on the United States Pharmacopeia (USP) – 2025 Edition
Issued and maintained by the United States Pharmacopeial Convention (USP)
1 DEFINITION
Ergotamine Tartrate Tablets contain NLT 90.0% and NMT 110.0% of the labeled amount of ergotamine tartrate [(C33H35N5O5)2 · C4H6O6].
2 IDENTIFICATION
PROCEDURE
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 and 0.016 mg/mL of ergonovine maleate from Internal standard solution 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, and sonicate for 10 min. 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 (621), System Suitability.)
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 0.7 and 1.0, respectively.]
Suitability requirements
Resolution: NLT 3.0 between ergonovine maleate and ergotamine tartrate
Column efficiency: NLT 3000 theoretical plates
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 = (Ru /Rs ) × (Cs /Cu ) × 100
Ru = peak response ratio of ergotamine tartrate to the internal standard from the Sample solution
Rs = peak response ratio of ergotamine tartrate to the internal standard from the Standard solution
Cs = concentration of USP Ergotamine Tartrate RS in the Standard solution (mg/mL)
Cu = nominal concentration of ergotamine tartrate from the Sample solution (mg/mL)
Acceptance criteria: 90.0%–110.0%
4 PERFORMANCE TESTS
DISSOLUTION (711)
Medium: 10 g/L of tartaric acid in water; 1000 mL
Apparatus 2: 75 rpm
Time: 30 min
Instrumental conditions
Mode: Fluorescence
Analytical wavelengths
Excitation: Maximum excitation at 327 nm.
Emission: Maximum emission at 427 nm
Standard solution: USP Ergotamine Tartrate RS in Medium
Sample solution: Dilute a portion of the solution under test with Medium to a concentration that is similar to that of the Standard solution.
Analysis
Samples: Standard solution and Sample solution
Determine the percentage of the labeled amount of ergotamine tartrate [(C33H35N5O5)2 · C4H6O6] dissolved.
Tolerances: NLT 75% (Q) of the labeled amount of ergotamine tartrate [(C33H35N5O5)2 · C4H6O6] is dissolved.
UNIFORMITY OF DOSAGE UNITS (905): Meet the requirements.
5 ADDITIONAL REQUIREMENTS
PACKAGING AND STORAGE: Preserve in well-closed, light-resistant containers. Store at 25°, excursions permitted between 15° and 30°.
LABELING: Label the Tablets to indicate that they are intended for swallowing intact.
USP REFERENCE STANDARDS (11)
USP Ergotamine Tartrate RS
