Demeclocycline Hydrochloride Capsules
»Demeclocycline Hydrochloride Capsules contain not less than 90.0percent and not more than 125.0percent of the labeled amount of demeclocycline hydrochloride (C21H21ClN2O8·HCl).
Packaging and storage— Preserve in tight,light-resistant containers.
Identification— Shake a suitable quantity of Capsule contents with methanol to obtain a solution containing about 1mg of demeclocycline hydrochloride per mL,and filter.Using the filtrate as the Test Solution,proceed as directed for Method IIunder Identification—Tetracyclines á193ñ.
Dissolution á711ñ—
Medium: water;900mL.
Apparatus 2: 75rpm.
Time: 45minutes.
Procedure— Determine the amount of C21H21ClN2O8dissolved from UVabsorption at the wavelength of maximum absorbance at about 274nm on filtered portions of the solution under test,suitably diluted with Dissolution Medium,if necessary,in comparison with a Standard solution having a known concentration of USP Demeclocycline Hydrochloride RSin the same Medium.
Tolerances— Not less than 75%(Q)of the labeled amount of demeclocycline (C21H21ClN2O8)is dissolved in 45minutes.
Uniformity of dosage units á905ñ: meet the requirements.
Loss on drying á731ñ— Dry about 100mg of Capsule contents,accurately weighed,in a capillary-stoppered bottle in vacuum at 60for 3hours:the material loses not more than 2.0%of its weight,except that if the Capsules contain starch the material loses not more than 8.0%of its weight.
Assay—
Mobile phase,Standard preparation,Resolution solution,and Chromatographic system— Prepare as directed in the Assayunder Demeclocycline.
Assay preparation— Remove,as completely as possible,the contents of not fewer than 10Capsules,and weigh.Mix,and transfer an accurately weighed portion of the powder,equivalent to about 50mg of demeclocycline hydrochloride (C21H21ClN2O8·HCl),to a 50-mLvolumetric flask,dilute with 0.01Nhydrochloric acid to volume,and mix.Sonicate for 5minutes,and centrifuge for 5minutes.Pass a portion of the supernatant through a suitable filter having a 1.5-µm or finer porosity,and use the clear filtrate as the Assay preparation.
Procedure— Proceed as directed for Procedurein the Assayunder Demeclocycline.Calculate the quantity,in mg,of demeclocycline hydrochloride (C21H21ClN2O8·HCl)in the portion of Capsule contents taken by the formula:
0.05CE(rU/rS),
in which the terms are as defined therein.
Auxiliary Information— Staff Liaison:William W.Wright,Ph.D.,Scientific Fellow
Expert Committee:(PA7)Pharmaceutical Analysis 7
USP28–NF23Page 579
Pharmacopeial Forum:Volume No.29(3)Page 625
Phone Number:1-301-816-8335