Calcifediol Capsules
»Calcifediol Capsules contain not less than 90.0percent and not more than 120.0percent of the labeled amount of C27H44O2·H2O.
Packaging and storage— Preserve in tight,light-resistant containers.
Identification— Transfer the contents of a number of Capsules,equivalent to about 150µg of calcifediol,to a suitable container,add 1mLof methanol,and shake vigorously for 1minute.Separate the layers by centrifugation,and transfer as much of the top,methanol layer as possible to a second container.Evaporate this extract to dryness,and dissolve the residue in about 1mLof chloroform.Proceed as directed under Thin-layer Chromatographic Identification Test á201ñ,applying 20µLof this solution and 20µLof a solution containing about the same concentration of USP Calcifediol RSin chloroform,and using a solvent system consisting of 60parts of cyclohexane and 40parts of ethyl acetate.
Dissolution á711ñ—
Medium: water;500mL.
Apparatus 2: 50rpm.
Time: 15minutes.
Procedure— Place 1Capsule in each vessel,and allow the Capsule to sink to the bottom of the vessel before starting rotation of the blade.Observe the Capsules,and record the time taken for each capsule shell to rupture.
Tolerances— The requirements are met if all of the Capsules tested rupture in not more than 15minutes.If 1or 2of the Capsules rupture in more than 15but not more than 30minutes,repeat the test on 12additional Capsules.Not more than 2of the total of 18Capsules tested rupture in more than 15but not more than 30minutes.
Uniformity of dosage units á905ñ: meet the requirements.
Assay—
Internal standard solution— Dissolve testosterone in ethyl acetate to obtain a solution having a concentration of about 35µg per mL.
Mobile phase— Prepare as directed in the Assayunder Calcifediol.
Standard preparation— Dissolve an accurately weighed quantity of USP Calcifediol RSin Internal standard solution,and dilute quantitatively and stepwise with Internal standard solutionto obtain a solution having a known concentration of about 7µg of USP Calcifediol RSper mL.
Assay preparation— Transfer a number of Calcifediol Capsules to a suitable container.Using a suitable implement,shear open a number of Capsules inside the container.Wash the implement with an accurately measured volume of Internal standard solutionthat will yield a solution having a concentration of about 7µg of calcifediol per mL.Collect the rinsings in the container,and mix to obtain a homogeneous solution of the Capsule contents.
Chromatographic system and System suitability—Proceed as directed in the Assayunder Calcifediol.
Procedure— Proceed as directed for Procedurein the Assayunder Calcifediol.Calculate the quantity,in µg,of C27H44O2·H2Oin the portion of Capsule contents taken by the formula:
CVU(RU/RS),
in which Cis the concentration,in µg per mL,of USP Calcifediol RSin the Standard preparation;VUis the volume,in mL,of Internal standard solutiontaken for the Assay preparation;and RUand RSare the peak response ratios of calcifediol to testosterone obtained from the Assay preparationand the Standard preparation,respectively.
Auxiliary Information— Staff Liaison:Elena Gonikberg,Ph.D.,Scientist
Expert Committee:(PA4)Pharmaceutical Analysis 4
USP28–NF23Page 316
Phone Number:1-301-816-8251