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4338 Metoclopramide / Official Monographs USP 36

compare the intensities of any secondary spots observed in. the chromatogram of the Test preparation with those of theMetoclopramide Hydrochloride principal spots in the chromatograms of the Standard prepa-

rations. [NOTEDisregard any spots observed at the originsof the chromatograms.] No secondary spot from the chro-matogram of the Test preparation is larger or more intensethan the principal spot obtained from Standard preparationA (0.5%), and the sum of the intensities of all secondary

spots obtained from the Test preparation corresponds to notmore than 1.0%.C14H22ClN3O2 H C l H2O 354.27

Benzamide, 4-amino-5-chloro-N-[2-(diethylamino)ethyl]- AssayTransfer about 300 mg of Metoclopramide Hydro-2-methoxy-, monohydrochloride, monohydrate. chloride, accurately weighed, to a stoppered, 125-mL flask,

4-Amino-5-chloro-N-[2-(diethylamino)ethyl]-o-anisamide add 10 mL of mercuric acetate TS and 2 mL of acetic anhy-monohydrochloride monohydrate [54143-57-6]. dride, and allow to stand for 3 hours. Add 80 mL of glacial

acetic acid, and titrate with 0.1 N perchloric acid VS, deter- Metoclopramide Hydrochloride contains not mining the endpoint potentiometrically (see Titrimetry

541). Perform a blank determination, and make any neces-less than 98.0 percent and not more thansary correction. Each mL of 0.1 N perchloric acid is equiva-101.0 percent of C14H22ClN3O2 HCl, calculatedlent to 33.63 mg of C14H22ClN3O2 HCl.on the anhydrous basis.

Packaging and storagePreserve in tight, light-resistantcontainers.

.USP Reference standards 11Metoclopramide InjectionUSP Metoclopramide Hydrochloride RS

Identification Metoclopramide Injection is a sterile solution ofA: Infrared Absorption 197M.

Metoclopramide Hydrochloride in Water for In-B: Dissolve 50 mg in 5 mL of water, and add 5 mL of a 1

jection. It contains the equivalent of not less thanin 100 solution ofp-dimethylaminobenzaldehyde in 1 N hy-drochloric acid: a yellow-orange color is produced. 90.0 percent and not more than 110.0 percent of

C: The RF value of the principal spot in the chromato- the labeled amount of metoclopramidegram of the Identification preparation corresponds to that of (C14H22ClN3O2).Standard preparation A, as obtained in the test forChromato-graphic purity. Packaging and storagePreserve in single-dose or in

multiple-dose containers, preferably of Type I glass, pro-Water, Method I921: between 4.5% and 6.0%.tected from light. [NOTEInjection containing an antioxidantResidue on ignition 281: not more than 0.1%.agent does not require protection from light.]

Chromatographic purityUSP Reference standards 11

Standard preparationsDissolve USP Metoclopramide Hy- USP Endotoxin RSdrochloride RS in methanol, and mix to obtain a solution USP Metoclopramide Hydrochloride RShaving a known concentration of 1 mg per mL. Dilute quan-

Identificationtitatively with methanol to obtain three Standard prepara- A: The retention time of the major peak in the chromato-tions, designated below by letters, having the following

gram of the Assay preparation corresponds to that of thecompositions:Standard preparation as obtained in the Assay.

B: Mix a volume of Injection, equivalent to about 50 mgConcentra- Percentage (%,of metoclopramide, with 5 mL of water and 5 mL of a 1 inStandard tion for comparison100 solution ofp-dimethylaminobenzaldehyde in 1 N hydro-prepara- (g RS with testchloric acid: a yellow-orange color is produced.tion Dilution per mL) specimen)Bacterial endotoxins 85It contains not more than 2.5A (1 in 4) 250 0.5USP Endotoxin Units per mg of metoclopramide.

B (3 in 20) 150 0.3pH 791: between 2.5 and 6.5.C (1 in 20) 50 0.1Particulate matter788: meets the requirementsunder small-volume injections.

Test preparationDissolve an accurately weighed quan-Other requirementsIt meets the requirements underIn-tity of Metoclopramide Hydrochloride in methanol to obtainjections1.a solution containing 50 mg per mL.AssayIdentification preparationDilute a portion of the Test

Mobile phaseDissolve 2.7 g of sodium acetate inpreparation quantitatively with methanol to obtain a solution500 mL of water, add 500 mL of acetonitrile, 2 mL of tetra-containing 250 g per mL.methylammonium hydroxide solution in methanol (1 in 5),ProcedureApply separately 10 L of the Test preparation,mix, adjust with glacial acetic acid to a pH of 6.5, filter, and10 L of the Identification preparation, and 10 L of eachdegas. Make adjustments if necessary (see System SuitabilityStandard preparation to a suitable thin-layer chromato-underChromatography621).graphic plate (see Chromatography621) coated with a

Standard preparationDissolve an accurately weighed0.25-mm layer of chromatographic silica gel mixture. Allowquantity of USP Metoclopramide Hydrochloride RS in 0.01the spots to dry, position the plate in a chromatographicM phosphoric acid to obtain a stock solution having achamber, and develop the chromatograms in a solvent sys-known concentration of about 0.9 mg of anhydroustem consisting of a mixture of chloroform, methanol, tolu-metoclopramide hydrochloride per mL. Dilute quantitatively,ene, and ammonium hydroxide (140:60:20:1) until the sol-and stepwise if necessary, a volume of this stock solutionvent front has moved about three-fourths of the length ofwith 0.01 M phosphoric acid to obtain a Standard prepara-the plate. Remove the plate from the developing chamber,tion having a known concentration of about 45 g of USPmark the solvent front, and allow the solvent to evaporate.Metoclopramide Hydrochloride RS, on the anhydrous basis,Examine the plate under short-wavelength UV light, and

ff c al from ay 1 2013o yr t c 2013 T e n ted States armaco e al on ent on. All r ts reser ed.

Accessed from 114.79.0.199 by merck1 on Sat Jul 06 12:20:46 EDT 2013