(er'' goe noe' veen mal' ee ate).
Ergoline-8-carboxamide, 9,10-didehydro-N-(2-hydroxy-1-methylethyl)-6-methyl-, 8(S)-, (Z)-2-butenedioate (1:1) (salt).
9,10-Didehydro-N-[(S)-2-hydroxy-1-methylethyl]-6-methylergoline-8-carboxamide maleate (1:1) (salt) [129-51-1].
» Ergonovine Maleate contains not less than 97.0 percent and not more than 103.0 percent of C19H23N3O2·C4H4O4, calculated on the dried basis.
Packaging and storage Preserve in tight, light-resistant containers, in a cold place.
USP Reference standards 11
B: Ultraviolet Absorption 197U
Solution: 20 µg per mL.
Absorptivities at 311 nm, calculated on the dried basis, do not differ by more than 3.0%.
C: The RF value of the principal blue spot obtained from the Test preparation corresponds to that obtained from the Standard preparation in the chromatogram prepared as directed in the test for Related alkaloids.
Specific rotation 781S: between +51 and +56.
Test solution: 5 mg per mL, in water.
Loss on drying 731 Dry it in vacuum at 80 for 3 hours: it loses not more than 2.0% of its weight.
Related alkaloids [noteConduct this test promptly, without exposure to daylight and with minimum exposure to artificial light. ]
Adsorbent: 0.25-mm layer of chromatographic silica gel mixture.
Solvent mixture Prepare a mixture of alcohol and ammonium hydroxide (9:1).
Standard preparation Prepare a solution of USP Ergonovine Maleate RS in Solvent mixture having a known concentration of about 10 mg per mL.
Standard dilutions Prepare a series of dilutions of the Standard preparation in Solvent mixture having known concentrations of about 0.20, 0.10, and 0.05 mg per mL. Use immediately after preparation.
Test preparation Immediately prior to use, prepare a solution of Ergonovine Maleate in Solvent mixture having a concentration of about 10 mg per mL.
Application volume: 5 µL.
Developing solvent system: a mixture of chloroform, methanol, and water (75:25:3), equilibrated for 30 minutes.
Procedure Apply 5-µL portions of the Standard preparation, each of the three Standard dilutions, and the Test preparation, and proceed as directed for Thin-Layer Chromatography under Chromatography 621. Locate the spots on the plate by spraying thoroughly and evenly with a solution prepared by dissolving 1 g of p-dimethylaminobenzaldehyde in a cooled mixture of 50 mL of alcohol and 50 mL of hydrochloric acid. Immediately dry in a stream of nitrogen for about 2 minutes: the RF value of the principal spot obtained from the Test preparation corresponds to that obtained from the Standard preparation. Estimate the concentration of any other spots observed in the chromatogram of the Test preparation by comparison with the Standard dilutions. The spots from the 0.20, 0.10, and 0.05 mg per mL dilutions are equivalent to 2.0%, 1.0%, and 0.50% of impurities, respectively. The sum of the impurities is not greater than 2.0%.
Standard preparation Using a suitable quantity of USP Ergonovine Maleate RS, accurately weighed, prepare a solution in water having a known concentration of about 40 µg per mL.
Assay preparation Transfer about 40 mg of Ergonovine Maleate, accurately weighed, to a 100-mL volumetric flask, dilute with water to volume, and mix. Dilute 10.0 mL of this solution with water to 100.0 mL.
Procedure Transfer 5.0 mL each of the Standard preparation, the Assay preparation, and water to provide a blank, to separate conical flasks. Add 10.0 mL of p-dimethylaminobenzaldehyde TS with constant swirling to each, and allow to stand for 20 minutes. Concomitantly determine the absorbances of the solutions in 1-cm cells at the wavelength of maximum absorbance at about 555 nm, with a suitable spectrophotometer, against the blank. Calculate the quantity, in mg, of C19H23N3O2·C4H4O4 taken by the formula:
C(AU / AS)in which C is the concentration, in µg per mL, of USP Ergonovine Maleate RS in the Standard preparation, and AU and AS are the absorbances of the solutions from the Assay preparation and the Standard preparation, respectively.
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USP35NF30 Page 3070Pharmacopeial Forum: Volume No. 29(5) Page 1478