(me per' i deen hye'' droe klor' ide).
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 98.0 percent and not more than 102.0 percent of C15H21NO2·HCl, calculated on the dried basis.
Packaging and storage Preserve in well-closed, light-resistant containers, and store at room temperature.
USP Reference standards 11
A: It meets the requirements under IdentificationOrganic Nitrogenous Bases 181.
B: A solution (1 in 100) responds to the tests for Chloride 191.
C: The retention time of the major peak in the chromatogram of the Assay preparation corresponds to that in the chromatogram of the Standard preparation, as obtained in the Assay.
Melting range 741: between 186 and 189, determined after drying in vacuum at 80 for 4 hours.
Loss on drying 731 Dry it in vacuum at a pressure between 20 to 40 mm of mercury at 80 for 4 hours: it loses not more than 1.0% of its weight.
Residue on ignition 281: not more than 0.1%.
Chromatographic purity Dissolve it in water to obtain a solution containing about 10 mg per mL. Inject 2.0 µL of 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 G3 on 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 28 mL per 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.
Chloride content Accurately weigh about 500 mg, previously dried, and transfer to a 250-mL conical flask. Add 15 mL of water, 5 mL of glacial acetic acid, 50 mL of methanol, and 0.2 mL of eosin Y TS, and titrate with 0.1 N silver nitrate VS to a rose-colored endpoint. Each mL of 0.1 N silver nitrate is equivalent to 3.545 mg of Cl. Not less than 12.2% and not more than 12.7% of Cl is found.
Buffer solution Transfer about 6.8 g of monobasic potassium phosphate to a 1000-mL volumetric flask. Dissolve in and dilute with water to volume. Add 10 mL of triethylamine, and mix. Adjust with phosphoric acid to a pH of 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 Suitability under Chromatography 621).
Standard preparation Transfer an accurately weighed quantity of about 30 mg of USP Meperidine Hydrochloride RS to a 50-mL volumetric flask, dissolve in and dilute with water to volume, and mix. Transfer 5.0 mL of this solution to a 25-mL volumetric flask, dilute with Mobile phase to volume, and mix.
Assay preparation Transfer an accurately weighed quantity of about 30 mg of Meperidine Hydrochloride to a 50-mL volumetric flask, dissolve in and dilute with water to volume, and mix. Transfer 5.0 mL of this solution to a 25-mL volumetric flask, dilute with Mobile phase to volume, and mix.
Chromatographic system (see Chromatography 621) 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 1 mL per minute. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the column efficiency is not less than 2000 theoretical plates; the tailing factor for the meperidine peak is not more than 2; and the relative standard deviation for replicate injections is not more than 2%.
Procedure Separately inject equal volumes (about 20 µL) of the Standard preparation and the Assay preparation into 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 C is the concentration, in mg per mL, of USP Meperidine Hydrochloride RS in the Standard preparation; and rU and rS are the meperidine peak responses obtained from the Assay preparation and the Standard preparation, respectively.
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USP35NF30 Page 3801Pharmacopeial Forum: Volume No. 31(1) Page 62