Ergotamine Tartrate Sublingual Tablets
» Ergotamine Tartrate Sublingual Tablets contain not less than 90.0 percent and not more than 110.0 percent of the labeled amount of (C33H35N5O5)2·C4H6O6.
Packaging and storage Preserve in well-closed, light-resistant containers. Store at 25, excursions permitted between 15 and 30.
Labeling Label Tablets to indicate that they are intended for sublingual administration.
Identification Triturate a quantity of finely powdered Sublingual Tablets, equivalent to about 5 mg of ergotamine tartrate, with 10 mL of solvent hexane for a few minutes, allow to settle, and discard the solvent hexane extract. Add to the residue 10 mL of chloroform saturated with ammonia (prepared by shaking chloroform with ammonium hydroxide, then drawing off the chloroform layer), triturate for a few minutes, filter, and evaporate the filtrate on a steam bath to dryness. Dissolve the residue in a mixture of 4 mL of glacial acetic acid and 4 mL of ethyl acetate. To 1 mL of this solution add slowly, with continuous agitation and cooling, 1 mL of sulfuric acid: a blue color with a red tinge develops. Add 0.1 mL of ferric chloride TS, previously diluted with an equal volume of water: the red tinge becomes less apparent and the blue color more pronounced.
Disintegration 701: 5 minutes.
Uniformity of dosage units 905: meet the requirements.
Mobile phase Prepare a filtered and degassed mixture of acetonitrile and 0.01 M monobasic potassium phosphate (55:45). Make adjustments if necessary (see System Suitability under Chromatography 621).
Internal standard solution Transfer about 40 mg of ergonovine maleate to a 250-mL volumetric flask, add a mixture of acetonitrile and water (55:45) to volume, and mix.
Standard preparation Transfer about 10 mg of USP Ergotamine Tartrate RS, accurately weighed, to a 50-mL volumetric flask, add a mixture of acetonitrile and water (55:45) to volume, and mix. Transfer 5.0 mL of this solution to a 50-mL volumetric flask, add 5.0 mL of Internal standard solution, dilute with the mixture of acetonitrile and water (55:45) to volume, and mix to obtain a solution having a known concentration of about 0.02 mg of USP Ergotamine Tartrate RS per mL.
Assay preparation Transfer a number of whole Sublingual Tablets, equivalent to about 10 mg of ergotamine tartrate, to a 500-mL volumetric flask. Add 50.0 mL of Internal standard solution, 300 mL of a mixture of acetonitrile and water (55:45), and sonicate for about 10 minutes. Dilute with the mixture of acetonitrile and water (55:45) to volume, and mix. Filter through a 0.45-µm membrane disk, discarding the first 25 mL of the filtrate.
Chromatographic system (see Chromatography 621) The liquid chromatograph is equipped with a 254-nm detector and a 3.9-mm × 30-cm column that contains packing L1. The flow rate is about 1 mL per minute. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the relative retention times are about 0.7 for ergonovine maleate and 1.0 for ergotamine tartrate; the resolution, R, between the analyte and internal standard peaks is not less than 3.0; the column efficiency determined from the analyte peak is not less than 3000 theoretical plates; the tailing factor for the analyte peak is not more than 2.0; and the relative standard deviation for replicate injections is not more than 2.0%.
Procedure Separately inject equal volumes (about 20 µL) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the responses for the major peaks. Calculate the quantity, in mg, of (C33H35N5O5)2·C4H6O6 in the portion of Sublingual Tablets taken by the formula:
500C(RU / RS)in which C is the concentration, in mg per mL, of USP Ergotamine Tartrate RS in the Standard preparation, and RU and RS are the peak response ratios obtained from the Assay preparation and the Standard preparation, respectively.
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USP32NF27 Page 2280Pharmacopeial Forum: Volume No. 30(4) Page 1199