Meperidine Hydrochloride
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C15H21NO2·HCl 283.79

4-Piperidinecarboxylic acid,1-methyl-4-phenyl-,ethyl ester,hydrochloride.
Ethyl 1-methyl-4-phenylisonipecotate hydrochloride [50-13-5].
»Meperidine Hydrochloride contains not less than 98.0percent and not more than 102.0percent of C15H21NO2·HCl,calculated on the dried basis.
Packaging and storage— Preserve in well-closed,light-resistant containers.Store at 25,excursions permitted between 15and 30.
Identification—
A: It meets the requirements under Identification—Organic Nitrogenous Bases á181ñ.
B: Asolution (1in 100)responds to the tests for Chloride á191ñ.
C: The retention time of the major peak in the chromatogram of the Assay preparationcorresponds to that in the chromatogram of the Standard preparation,as obtained in the Assay.
Melting range á741ñ: between 186and 189,determined after drying in vacuum at 80for 4hours.
Loss on drying á731ñ— Dry it in vacuum at a pressure between 20to 40mm of mercury at 80for 4hours:it loses not more than 1.0%of its weight.
Residue on ignition á281ñ: not more than 0.1%.
Chromatographic purity— Dissolve it in water to obtain a solution containing about 10mg per mL.Inject 2.0µLof the solution into a suitable gas chromatograph equipped with a flame-ionization detector.Under typical conditions,the instrument contains a 2-mm ×2-m glass column packed with 10%phase G3on support S1A.Maintain the temperature of the column at 190,the injection port at 255,and the detector at 280.Use helium as the carrier gas at a flow rate of 28mLper minute.Calculate the area percentage of each peak observed in the chromatogram.No peak,other than the principal peak (except for the solvent peak),constitutes more than 1.0%of the total area.
Organic volatile impurities,Method Iá467ñ: meets the requirements.
Chloride content— Accurately weigh about 500mg,previously dried,and transfer to a 250-mLconical flask.Add 15mLof water,5mLof glacial acetic acid,50mLof methanol,and 0.2mLof eosin Y TS,and titrate with 0.1Nsilver nitrate VSto a rose-colored endpoint.Each mLof 0.1Nsilver nitrate is equivalent to 3.545mg of Cl.Not less than 12.2%and not more than 12.7%of Cl is found.
Assay—
Buffer solution— Transfer about 6.8g of monobasic potassium phosphate to a 1000-mLvolumetric flask.Dissolve in and dilute with water to volume.Add 10mLof triethylamine,and mix.Adjust with phosphoric acid to a pHof 7.0,and filter.
Mobile phase— Prepare a filtered and degassed mixture of acetonitrile and Buffer solution(55:45).Make adjustments if necessary (see System Suitabilityunder Chromatography á621ñ).
Standard preparation— Transfer an accurately weighed quantity of about 30mg of USP Meperidine Hydrochloride RSto a 50-mLvolumetric flask,dissolve in and dilute with water to volume,and mix.Transfer 5.0mLof this solution to a 25-mLvolumetric flask,dilute with Mobile phaseto volume,and mix.
Assay preparation— Transfer an accurately weighed quantity of about 30mg of Meperidine Hydrochloride to a 50-mLvolumetric flask,dissolve in and dilute with water to volume,and mix.Transfer 5.0mLof this solution to a 25-mLvolumetric flask,dilute with Mobile phaseto volume,and mix.
Chromatographic system(see Chromatography á621ñ)— The liquid chromatograph is equipped with a 230-nm detector and a 3.9-mm ×30-cm column that contains packing L1.The flow rate is about 1mLper minute.Chromatograph the Standard preparation,and record the peak responses as directed for Procedure:the column efficiency is not less than 2000theoretical plates;the tailing factor for the meperidine peak is not more than 2;the number of theoretical plates is not less than 2000;and the relative standard deviation for replicate injections is not more than 2%.
Procedure— Separately inject equal volumes (about 20µL)of the Standard preparationand the Assay preparationinto the chromatograph,record the chromatograms,and measure the peak responses.Calculate the quantity,in mg,of C15H21NO2·HCl in the portion of Meperidine Hydrochloride taken by the formula:
250C(rU/rS),
in which Cis the concentration,in mg per mL,of USP Meperidine Hydrochloride RSin the Standard preparation;and rUand rSare the meperidine peak responses obtained from the Assay preparationand the Standard preparation,respectively.
Auxiliary Information— Staff Liaison:Daniel K.Bempong,Ph.D.,Scientist
Expert Committee:(PA2)Pharmaceutical Analysis 2
USP28–NF23Page 1208
Pharmacopeial Forum:Volume No.29(6)Page 1924
Phone Number:1-301-816-8143