Doxycycline Hyclate Delayed-Release Capsules
» Doxycycline Hyclate Delayed-Release Capsules contain the equivalent of not less than 90.0 percent and not more than 120.0 percent 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.
USP Reference standards 11—
USP Doxycycline Hyclate RS Click to View Structure
Identification— Shake a suitable quantity of finely powdered Capsule contents with methanol to obtain a solution containing the equivalent of 1 mg of doxycycline per mL, and filter. Using the filtrate as the Test Solution, proceed as directed for Method II under Identification—Tetracyclines 193.
Dissolution 711— Proceed as directed for Procedure for Method B under Apparatus 1 and Apparatus 2, Delayed-Release Dosage Forms.
acid stage— [note—Conduct the test by transferring the contents of each Capsule to the individual basket units of the apparatus. ]
Medium: 0.06 N hydrochloric acid; 900 mL.
Apparatus 1: 50 rpm.
Time: 20 minutes.
Diluting solvent: 0.1 N hydrochloric acid.
Procedure— Determine the amount of C22H24N2O8 dissolved from UV absorbances at the wavelength of maximum absorbance at about 345 nm on filtered portions of the solution under test, suitably diluted with Diluting solvent, in comparison with a Standard solution having a known concentration of about 0.01 mg of USP Doxycycline Hyclate RS per mL in Diluting solvent.
Tolerances—Level 1 (6 Capsules tested): No individual value exceeds 50% dissolved. Level 2 (6 Capsules tested): Not more than 2 individual values of 12 tested 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: pH 5.5 neutralized phthalate buffer (see Buffer Solutions in the section Reagents, Indicators, and Solutions); 1000 mL.
Apparatus 1: 50 rpm.
Time: 30 minutes.
Diluting solvent: 0.1 N hydrochloric acid.
Procedure— Determine the amount of C22H24N2O8 dissolved from UV absorbances at the wavelength of maximum absorbance at about 345 nm on filtered portions of the solution under test, suitably diluted with Diluting solvent, in comparison with a Standard solution having a known concentration of about 0.01 mg of USP Doxycycline Hyclate RS per mL in Diluting solvent.
Tolerances— Not less than 85% (Q) of the labeled amount of C22H24N2O8 is dissolved in 30 minutes.
Uniformity of dosage units 905: meet the requirements.
Water, Method I 921: not more than 5.0%.
Assay—
Mobile phase, Diluent, Resolution solution, Standard preparation, and Chromatographic system— Proceed as directed in the Assay under Doxycycline Hyclate.
Assay preparation— Remove, as completely as possible, the contents of not fewer than 20 Capsules, and weigh accurately. Mix the combined contents, and transfer an accurately weighed portion of the powder, equivalent to about 100 mg of doxycycline, to a 100-mL volumetric flask, add about 75 mL of Diluent, sonicate for 5 minutes, shake for 15 minutes, dilute with Diluent to volume, and mix. Pass through a membrane filter having a 0.5-µm or finer porosity.
Procedure— Proceed as directed for Procedure in the Assay under 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 C is the concentration, in mg per mL, of USP Doxycycline Hyclate RS in the Standard preparation; P is the designated potency, in µg of doxycycline per mg, of USP Doxycycline Hyclate RS; and rU and rS are the peak responses obtained from the Assay preparation and the Standard preparation, respectively.
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