Diloxanide Furoate
;)
4-(N-methyl-2,2-dichloroacetamido)phenyl 2-furoate.
2,2-Dichloroacetamido-4-N-methylphenyl 2-furoate [3736-81-0].
»Diloxanide Furoate contains not less than 98.0percent and not more than 102.0percent of C14H11Cl2NO4,calculated on the dried basis.
Packaging and storage—
Preserve in tight,light-resistant containers at controlled room temperature.
Identification—
A:
Infrared Absorption á197Kñ.
B:
Ultraviolet Absorption á197Uñ—
Solution:
14µg per mL.
Medium:
alcohol.The solution exhibits a maximum at 258nm.
C:
Burn 20mg by employing the method under Oxygen-Flask Combustion á471ñ,using 10mLof 1Nsodium hydroxide as the absorbing liquid.When the process is complete,acidify the liquid with nitric acid,and add a solution of silver nitrate (5in 100).Awhite precipitate forms.
Acidity—
Shake 3g with 50mLof water,filter,wash the residue with three 20-mLportions of water,and combine the filtrate and washings.Titrate with 0.1Nsodium hydroxide VSusing phenolphthalein TSas the indicator:not more than 1.3mLof 0.1Nsodium hydroxide is required for neutralization.
Loss on drying á731ñ—
Dry it at 105
to constant weight:it loses not more than 0.5%.
to constant weight:it loses not more than 0.5%.
Residue on ignition á281ñ:
not more than 0.1%.
Related compounds—
Adsorbent:
0.25-mm layer of chromatographic silica gel mixture.
Test solution—
Dissolve an accurately weighed amount of Diloxanide Furoate in chloroform to obtain a solution having a concentration of about 100mg per mL.
Standard solution—
Dilute 0.5mLof Test solutionwith chloroform to 200mL.
Application volume:
5µL.
Developing solvent system:
a mixture of dichloromethane and methanol (96:4).
Procedure—
Proceed as directed for Thin-Layer Chromatographyunder Chromatography á621ñ.Examine the plate under short-wavelength UVlight:any secondary spot obtained from the Test solutionis not more intense than the spot obtained from the Standard solution.
Assay—
Dissolve about 300mg of Diloxanide Furoate,accurately weighed,in 50.0mLof dried pyridine,and titrate with 0.1Ntetrabutylammonium hydroxide VS,determining the endpoint potentiometrically using suitable electrodes (see Titrimetry á541ñ).Perform a blank determination,and make any necessary correction.Each mLof 0.1Ntetrabutylammonium hydroxide is equivalent to 32.82mg of C14H11Cl2NO4.
Auxiliary Information—
Staff Liaison:Behnam Davani,Ph.D.,MBA,Senior Scientist
Expert Committee:(PA7)Pharmaceutical Analysis 7
USP28–NF23Page 654
Pharmacopeial Forum:Volume No.27(1)Page 1778
Phone Number:1-301-816-8394