A: Infrared Absorption á197Kñ.

B: [NOTE—Conduct 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 á621ñ),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 25mLof ammonium hydroxide in the chamber,cover,and allow to equilibrate for 30minutes.Prepare a test solution of Methysergide Maleate in methanol containing 5mg per mL.Apply 25µLof this solution and 25µLof a Standard solution of USP Methysergide Maleate RSin methanol containing 5mg per mLto a suitable thin-layer chromatographic plate (see Chromatography á621ñ)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 800mg of p-dimethylaminobenzaldehyde in a cooled mixture of 80mLof alcohol and 20mLof sulfuric acid,allow the plate to dry,then expose it briefly to fumes of a mixture of nitric and hydrochloric acids:the RFvalue of the principal spot obtained from the test solution corresponds to that obtained from the Standard solution.

Test solution: 2.5mg per mL,in water.

Test solution: methanol.

Standard solution: methanol.

Eluant: prepare as directed under Identificationtest B.

Visualization: 1.