Doxycycline Hyclate Delayed-Release Capsules
»Doxycycline Hyclate Delayed-Release Capsules contain the equivalent of not less than 90.0percent and not more than 120.0percent of the labeled amount of doxycycline (C22H24N2O8).
Packaging and storage— Preserve in tight,light-resistant containers.
Labeling— The label indicates that the contents of the Capsules are enteric-coated.
Identification— Shake a suitable quantity of finely powdered Capsule contents with methanol to obtain a solution containing the equivalent of 1mg of doxycycline per mL,and filter.Using the filtrate as the Test Solution,proceed as directed for Method IIunder Identification—Tetracyclines á193ñ.
Drug release,Method Bá724ñ—
Acid stage— [NOTE—Conduct the test by transferring the contents of each Capsule to the individual basket units of the apparatus.]
Medium: 0.06Nhydrochloric acid;900mL.
Apparatus 1: 50rpm.
Time: 20minutes.
Diluting solvent: 0.1Nhydrochloric acid.
Procedure— Determine the amount of C22H24N2O8dissolved from UVabsorbances at the wavelength of maximum absorbance at about 345nm of filtered portions of the solution under test,suitably diluted with Diluting solvent,in comparison with a Standard solution having a known concentration of about 0.01mg of USP Doxycycline Hyclate RSper mLin Diluting solvent.
Tolerances—Level 1 (6Capsules tested)—No individual value exceeds 50%dissolved.Level 2(6Capsules tested)—Not more than 2individual values of 12tested are greater than 50%dissolved.
Buffer stage— [NOTE—Conduct this stage of testing on separate specimens,selecting Capsules that were not previously subjected to Acid-stage testing and transferring the contents of each Capsule to the individual basket units of the apparatus.]
Medium: pH5.5neutralized phthalate buffer (see Buffer Solutionsin the section Reagents,Indicators,and Solutions);1000mL.
Apparatus 1: 50rpm.
Time: 30minutes.
Diluting solvent: 0.1Nhydrochloric acid.
Procedure— Determine the amount of C22H24N2O8dissolved from UVabsorbances at the wavelength of maximum absorbance at about 345nm of filtered portions of the solution under test,suitably diluted with Diluting solvent,in comparison with a Standard solution having a known concentration of about 0.01mg of USP Doxycycline Hyclate RSper mLin Diluting solvent.
Tolerances— Not less than 85%(Q)of the labeled amount of C22H24N2O8is dissolved in 30minutes.
Uniformity of dosage units á905ñ: meet the requirements.
Water,Method Iá921ñ: not more than 5.0%.
Assay—
Mobile phase,Diluent,Resolution solution,Standard preparation,andChromatographic system— Proceed as directed in the Assayunder Doxycycline Hyclate.
Assay preparation— Remove,as completely as possible,the contents of not less than 20Capsules,and weigh accurately.Mix the combined contents,and transfer an accurately weighed portion of the powder,equivalent to about 100mg of doxycycline,to a 100-mLvolumetric flask,add about 75mLof Diluent,sonicate for 5minutes,shake for 15minutes,dilute with Diluentto volume,and mix.Filter through a membrane filter of 0.5-µm or finer porosity.
Procedure— Proceed as directed for Procedurein the Assayunder Doxycycline Hyclate.Calculate the quantity,in mg,of doxycycline (C22H24N2O8)in the portion of Capsules taken by the formula:
0.1CP(rU/rS),
in which Cis the concentration,in mg per mL,of USP Doxycycline Hyclate RSin the Standard preparation,Pis the designated potency,in µg of doxycycline per mg,of USP Doxycycline Hyclate RS,and rUand rSare the peak responses obtained from the Assay preparationand the Standard preparation,respectively.
Auxiliary Information— Staff Liaison:William W.Wright,Ph.D.,Scientific Fellow
Expert Committee:(PA7)Pharmaceutical Analysis 7
USP28–NF23Page 700
Phone Number:1-301-816-8335