Ergoline-8-carboxamide, 9,10-didehydro-N-[1-(hydroxymethyl)propyl]-1,6]-dimethyl-, (8)-, (Z)-2-butenedioate (1:1) (salt).
9,10-Didehydro-N-[1-(hydroxymethyl)propyl-1,6]-dimethylergoline-8-carboxamide maleate (1:1) (salt) [129-49-7].
» Methysergide Maleate contains not less than 97.0 percent and not more than 103.0 percent of C21H27N3O2·C4H4O4, calculated on the dried basis.
Packaging and storage Preserve in tight, light-resistant containers, in a cold place.
B: [noteConduct this test without exposure to daylight, and with the minimum exposure to artificial light.] In a suitable chromatographic chamber, arranged for thin-layer chromatography (see Chromatography 621), place a volume of a solvent system consisting of a mixture of chloroform and methanol (20:1) sufficient to develop the chromatogram. Place a beaker containing 25 mL of ammonium hydroxide in the chamber, cover, and allow to equilibrate for 30 minutes. Prepare a test solution of Methysergide Maleate in methanol containing 5 mg per mL. Apply 25 µL of this solution and 25 µL of a Standard solution of USP Methysergide Maleate RS in methanol containing 5 mg per mL to a suitable thin-layer chromatographic plate (see Chromatography 621) coated with a 0.25-mm layer of chromatographic silica gel. Develop the chromatogram until the solvent front has moved about three-fourths of the length of the plate. Remove the plate from the developing chamber, mark the solvent front, and allow the solvent to evaporate. Locate the spots on the plate by lightly spraying with a solution prepared by dissolving 800 mg of p-dimethylaminobenzaldehyde in a cooled mixture of 80 mL of alcohol and 20 mL of sulfuric acid, allow the plate to dry, then expose it briefly to fumes of a mixture of nitric and hydrochloric acids: the RF value of the principal spot obtained from the test solution corresponds to that obtained from the Standard solution.
Specific rotation 781S: between +35 and +45.
Test solution: 2.5 mg per mL, in water.
pH 791: between 3.7 and 4.7, in a 1 in 500 solution in carbon dioxide-free water.
Loss on drying 731 Dry it in vacuum at 120 for 2 hours: it loses not more than 7.0% of its weight.
Ordinary impurities 466
Test solution: methanol.
Standard solution: methanol.
Eluant: prepare as directed under Identification test B.
Assay Dissolve about 200 mg of Methysergide Maleate, accurately weighed, in 30 mL of glacial acetic acid, add 1 drop of crystal violet TS, and titrate with 0.1 N perchloric acid VS to a blue endpoint. Perform a blank determination, and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 46.95 mg of C21H27N3O2·C4H4O4.
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USP32NF27 Page 2958