(met'' oh kloe' pra mide hye'' droe klor' ide).
Benzamide, 4-amino-5-chloro-N-[2-(diethylamino)ethyl]-2-methoxy-, monohydrochloride, monohydrate.
4-Amino-5-chloro-N-[2-(diethylamino)ethyl]-o-anisamide monohydrochloride monohydrate [54143-57-6].
» Metoclopramide Hydrochloride contains not less than 98.0 percent and not more than 101.0 percent of C14H22ClN3O2·HCl, calculated on the anhydrous basis.
Packaging and storage Preserve in tight, light-resistant containers.
USP Reference standards 11
B: Dissolve 50 mg in 5 mL of water, and add 5 mL of a 1 in 100 solution of p-dimethylaminobenzaldehyde in 1 N hydrochloric acid: a yellow-orange color is produced.
Water, Method I 921: between 4.5% and 6.0%.
Residue on ignition 281: not more than 0.1%.
Standard preparations Dissolve USP Metoclopramide Hydrochloride RS in methanol, and mix to obtain a solution having a known concentration of 1 mg per mL. Dilute quantitatively with methanol to obtain three Standard preparations, designated below by letters, having the following compositions:
Test preparation Dissolve an accurately weighed quantity of Metoclopramide Hydrochloride in methanol to obtain a solution containing 50 mg per mL.
Identification preparation Dilute a portion of the Test preparation quantitatively with methanol to obtain a solution containing 250 µg per mL.
Procedure Apply separately 10 µL of the Test preparation, 10 µL of the Identification preparation, and 10 µL of each Standard preparation to a suitable thin-layer chromatographic plate (see Chromatography 621) coated with a 0.25-mm layer of chromatographic silica gel mixture. Allow the spots to dry, position the plate in a chromatographic chamber, and develop the chromatograms in a solvent system consisting of a mixture of chloroform, methanol, toluene, and ammonium hydroxide (140:60:20:1) 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. Examine the plate under short-wavelength UV light, and compare the intensities of any secondary spots observed in the chromatogram of the Test preparation with those of the principal spots in the chromatograms of the Standard preparations. [noteDisregard any spots observed at the origins of the chromatograms. ] No secondary spot from the chromatogram of the Test preparation is larger or more intense than the principal spot obtained from Standard preparation A (0.5%), and the sum of the intensities of all secondary spots obtained from the Test preparation corresponds to not more than 1.0%.
Assay Transfer about 300 mg of Metoclopramide Hydrochloride, accurately weighed, to a stoppered, 125-mL flask, add 10 mL of mercuric acetate TS and 2 mL of acetic anhydride, and allow to stand for 3 hours. Add 80 mL of glacial acetic acid, and titrate with 0.1 N perchloric acid VS, determining the endpoint potentiometrically (see Titrimetry 541). Perform a blank determination, and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 33.63 mg of C14H22ClN3O2·HCl.
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USP35NF30 Page 3893Pharmacopeial Forum: Volume No. 29(5) Page 1536