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Metoclopramide Hydrochloride
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C14H22ClN3O2·HCl·H2O 354.27

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.
Identification—
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.
C: The RF value of the principal spot in the chromatogram of the Identification preparation corresponds to that of Standard preparation A, as obtained in the test for Chromatographic purity.
Water, Method I 921: between 4.5% and 6.0%.
Residue on ignition 281: not more than 0.1%.
Chromatographic purity—
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:
Standard
preparation		 Dilution Concentration
(µg RS
per mL)		 Percentage (%,
for comparison
with test
specimen)
A (1 in 4) 250 0.5
B (3 in 20) 150 0.3
C (1 in 20) 50 0.1
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 500 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. [NOTE—Disregard 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%.
Organic volatile impurities, Method I 467: meets the requirements.
Residual solvents 467: meets the requirements.
(Official January 1, 2007)
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.
Auxiliary Information— Staff Liaison : Elena Gonikberg, Ph.D., Scientist
Expert Committee : (MDGRE05) Monograph Development-Gastrointestinal Renal and Endocrine
USP29–NF24 Page 1414
Pharmacopeial Forum : Volume No. 29(5) Page 1536
Phone Number : 1-301-816-8251