4-Quinolinemethanol, -2-piperidinyl-2,8-bis(trifluoromethyl)-, monohydrochloride, (R*,S*)- (±)-.
dl-erythro--2-Piperidyl-2,8-bis(trifluoromethyl)-4-quinolinemethanol monohydrochloride [51773-92-3].
» Mefloquine Hydrochloride contains not less than 99.0 percent and not more than 101.0 percent of C17H16F6N2O·HCl, calculated on the anhydrous basis.
Packaging and storage Preserve in tight, light-resistant containers. Store between 15 and 30.
USP Reference standards 11
USP Mefloquine Hydrochloride RS .
USP Mefloquine Related Compound A RS .
Specific rotation 781: between 0.2 and +0.2. Use a solution prepared by dissolving about 2.5 g in methanol, and dilute with methanol to 50.0 mL.
Water, Method I 921: not more than 3.0%.
Residue on ignition 281: not more than 0.1%.
Heavy metals, Method II 231: 0.002%.
Mobile phase Dissolve 1 g of tetraheptylammonium bromide in a 1-L mixture of a 1.5 g per L solution of sodium hydrogen sulfate, acetonitrile, and methanol (2:2:1). Make adjustments if necessary (see System Suitability under Chromatography 621).
System suitability solution Transfer about 4 mg of USP Mefloquine Hydrochloride RS and 4 mg of USP Mefloquine Related Compound A RS to a 50-mL volumetric flask, dissolve in and dilute with Mobile phase to volume, and mix. [noteMefloquine related compound A is threo-mefloquine.] Transfer 5.0 mL of this solution to a 100-mL volumetric flask, dilute with Mobile phase to volume, and mix.
Test solution Transfer about 0.10 g of Mefloquine Hydrochloride, accurately weighed, to a 25-mL volumetric flask, dissolve in and dilute with Mobile phase to volume, and mix.
Diluted test solution Transfer 1.0 mL of the Test solution to a 50-mL volumetric flask, dilute with Mobile phase to volume, and mix. Transfer 1.0 mL of this solution to a 20-mL volumetric flask, dilute with Mobile phase to volume, and mix.
Chromatographic system (see Chromatography 621) The liquid chromatograph is equipped with a 280-nm detector, a 4-mm × 2.5-cm precolumn, and a 4.0-mm × 25-cm column, both containing 5-µm packing L1. The flow rate is about 0.8 mL per minute. Chromatograph the System suitability solution, and record the peak responses as directed for Procedure: the relative retention times are about 0.7 for mefloquine related compound A and 1.0 for mefloquine; the resolution, R, between mefloquine related compound A and mefloquine is not less than 2.0; and the relative standard deviation for replicate injections is not more than 2.0%.
Procedure Equilibrate the column with Mobile phase at a flow rate of about 0.8 mL per minute for about 30 minutes. Inject 20 µL of Diluted test solution. Adjust the sensitivity of the system so that the height of the major peak is at least 50% of the full scale of the recorder. Separately inject equal volumes (about 20 µL) of the Test solution and Diluted test solution into the chromatograph, record the chromatogram for a time that is 10 times the retention time of the main peak, and measure the responses of all the peaks, excluding the main peak and any other peak producing a response of less than 0.2 times (0.02%) of the main peak in the chromatogram of the Diluted test solution. The response of the mefloquine related compound A peak in the Test solution with a relative retention time of about 0.7, with reference to the main peak, is not more than twice the area of the main peak in the chromatogram of the Diluted test solution (0.2%). The response of any other individual peak, other than the main peak in the chromatogram of the Test solution, is not greater than that of the main peak in the chromatogram of the Diluted test solution (0.1%); and the sum of the responses of any such peaks in the chromatogram of the Test solution is not greater than five times the response of the main peak in the chromatogram of the Diluted test solution (0.5%).
Assay Dissolve about 0.35 g, accurately weighed, in 15 mL of anhydrous formic acid, and add 40 mL of acetic anhydride. Place the sample solution in a glass container thermostated at 20. Titrate with 0.1 N perchloric acid VS, and determine the endpoint potentiometrically. [notePerform the titration rapidly after the addition of acetic anhydride by predosing with about 60% of the expected titrant, and then slowly titrate to a potentiometric endpoint.] Perform a blank determination, and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 41.48 mg of C17H16F6N2O·HCl.
Auxiliary Information Please check for your question in the FAQs before contacting USP.Chromatographic Column
USP32NF27 Page 2865Pharmacopeial Forum: Volume No. 33(4) Page 667
Chromatographic columns text is not derived from, and not part of, USP 32 or NF 27.