Miconazole
;)
1H-Imidazole,1-2-[(2,4-dichlorophenyl)-2-[(2,4-dichlorophenyl)]methoxy]ethyl]-,(±)-.
(±)-1-[2,4-Dichloro-b-[(2,4-dichlorobenzyl)oxy]phenethyl]imidazole [22916-47-8].
»Miconazole contains not less than 98.0percent and not more than 102.0percent of C18H14Cl4N2O,calculated on the dried basis.
Packaging and storage—
Preserve in well-closed containers,protected from light.Store at 25
,excursions permitted between 15and 30.
,excursions permitted between 15and 30.
Identification—
A:Infrared Absorption á197Kñ.
B:
Transfer 40mg to a 100-mLvolumetric flask,dissolve in 50mLof isopropyl alcohol,add 10mLof 0.1Nhydrochloric acid,dilute with isopropyl alcohol to volume,and mix:the UVabsorption spectrum of this solution exhibits maxima and minima at the same wavelengths as that of a similar solution of USP Miconazole RS,concomitantly measured.
Loss on drying á731ñ—
Dry it in vacuum at 60for 4hours:it loses not more than 0.5%of its weight.
for 4hours:it loses not more than 0.5%of its weight.
Residue on ignition á281ñ:
not more than 0.2%.
Chromatographic purity—
Dissolve 30mg in 3.0mLof chloroform to obtain the Test preparation.Dissolve a suitable quantity of USP Miconazole RSin chloroform to obtain a Standard solutionhaving a concentration of 10.0mg per mL.Quantitatively dilute a portion of this solution with chloroform to obtain a Diluted standard solutionhaving a concentration of 100µg per mL.Apply separate 5-µLportions of the three solutions to the starting line of a suitable thin-layer chromatographic plate (see Chromatography á621ñ)coated with a 0.25-mm layer of chromatographic silica gel mixture.Develop the chromatogram in a suitable chamber with a freshly prepared solvent system consisting of a mixture of n-hexane,chloroform,methanol,and ammonium hydroxide (60:30:10:1)until the solvent front has moved about three-fourths of the length of the plate.Remove the plate from the chamber,and allow the solvent to evaporate.Expose the plate to iodine vapors in a closed chamber for about 30minutes,and locate the spots:the RFvalue of the principal spot obtained from the Test solutioncorresponds to that obtained from the Standard solution,and any other spot obtained from the Test solutiondoes not exceed,in size or intensity,the principal spot obtained from the Diluted standard solution(1.0%).
Assay—
Dissolve about 300mg of Miconazole,accurately weighed,in 40mLof glacial acetic acid,add 4drops of p-naphtholbenzein TS,and titrate with 0.1Nperchloric acid VSto a green endpoint.Perform a blank determination,and make any necessary correction.Each mLof 0.1Nperchloric acid is equivalent to 41.61mg of C18H14Cl4N2O.
Auxiliary Information—
Staff Liaison:Behnam Davani,Ph.D.,MBA,Senior Scientist
Expert Committee:(PA7)Pharmaceutical Analysis 7
USP28–NF23Page 1293
Pharmacopeial Forum:Volume No.29(6)Page 1934
Phone Number:1-301-816-8394