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199 by merck1 on Sat Jul 06 12:20:46 EDT 2013

4338 Metoclopramide / Official Monographs

USP 36
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%. AssayTransfer 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.

Metoclopramide Hydrochloride
.

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 storagePreserve in tight, light-resistant containers. USP Reference standards 11 USP Metoclopramide Hydrochloride RS Identification A: Infrared Absorption 197M. 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 preparationsDissolve 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 A B C Concentration (g RS per mL) 250 150 50 Percentage (%, for comparison with test specimen) 0.5 0.3 0.1

Metoclopramide Injection
.

Metoclopramide Injection is a sterile solution of Metoclopramide Hydrochloride in Water for Injection. It contains the equivalent of not less than 90.0 percent and not more than 110.0 percent of the labeled amount of metoclopramide (C14H22ClN3O2).
Packaging and storagePreserve in single-dose or in multiple-dose containers, preferably of Type I glass, protected from light. [NOTEInjection containing an antioxidant agent does not require protection from light.] USP Reference standards 11 USP Endotoxin RS USP Metoclopramide Hydrochloride RS Identification A: The retention time of the major peak in the chromatogram of the Assay preparation corresponds to that of the Standard preparation as obtained in the Assay. B: Mix a volume of Injection, equivalent to about 50 mg of metoclopramide, with 5 mL of water and 5 mL of a 1 in 100 solution of p-dimethylaminobenzaldehyde in 1 N hydrochloric acid: a yellow-orange color is produced. Bacterial endotoxins 85It contains not more than 2.5 USP Endotoxin Units per mg of metoclopramide. pH 791: between 2.5 and 6.5. Particulate matter 788: meets the requirements under small-volume injections. Other requirementsIt meets the requirements under Injections 1. Assay Mobile phaseDissolve 2.7 g of sodium acetate in 500 mL of water, add 500 mL of acetonitrile, 2 mL of tetramethylammonium hydroxide solution in methanol (1 in 5), mix, adjust with glacial acetic acid to a pH of 6.5, filter, and degas. Make adjustments if necessary (see System Suitability under Chromatography 621). Standard preparationDissolve an accurately weighed quantity of USP Metoclopramide Hydrochloride RS in 0.01 M phosphoric acid to obtain a stock solution having a known concentration of about 0.9 mg of anhydrous metoclopramide hydrochloride per mL. Dilute quantitatively, and stepwise if necessary, a volume of this stock solution with 0.01 M phosphoric acid to obtain a Standard preparation having a known concentration of about 45 g of USP Metoclopramide Hydrochloride RS, on the anhydrous basis,

Dilution (1 in 4) (3 in 20) (1 in 20)

Test preparationDissolve an accurately weighed quantity of Metoclopramide Hydrochloride in methanol to obtain a solution containing 50 mg per mL. Identification preparationDilute a portion of the Test preparation quantitatively with methanol to obtain a solution containing 250 g per mL. ProcedureApply separately 10 L of the Test preparation, 10 L of the Identification preparation, and 10 L 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

Official from May 1, 2013 Copyright (c) 2013 The United States Pharmacopeial Convention. All rights reserved.