A: Infrared Absorption 197K—

B: The retention time of the major peak in the chromatogram of the Assay preparation corresponds to that in the chromatogram of the Standard preparation, as obtained in the Assay.

test 1—

test 2— If the product complies with this test, the labeling indicates that the product meets USP Dissolution Test 2.

procedure for content uniformity—

Buffer solution pH 2.9 and Mobile phase— Prepare as directed in the Assay.

System suitability solution— Dissolve an accurately weighed quantity of USP Fenofibrate RS and USP Fenofibrate Related Compound B RS in Mobile phase to obtain a solution having concentrations of about 0.67 mg per mL and 3.35 µg per mL, respectively. [Note—Fenofibrate related compound B is 2-[4-(4-chlorobenzoyl)phenoxy]-2-methylpropanoic acid (fenofibric acid).]

Standard solution— Dissolve an accurately weighed quantity of USP Fenofibrate RS and USP Fenofibrate Related Compound B RS in Mobile phase to obtain a solution having known concentrations of about 3.35 µg per mL of each component.

Sensitivity solution— Quantitatively dilute an aliquot of the Standard solution with Mobile phase, to obtain a solution having concentrations of about 0.67 µg of each component per mL.

Test solution— Accurately weigh the contents of not fewer than 20 Capsules. Mix the contents, and transfer an accurately weighed portion of the powder, equivalent to about 67 mg of fenofibrate, to a 100-mL volumetric flask. Fill the flask to about 80% with Mobile phase, sonicate for 10 minutes, stir for 15 minutes, and dilute with Mobile phase to volume. Pass a portion of this solution through a 0.45-µm PVDF filter, discarding the first 5 mL. The final concentration is about 0.67 mg per mL.

Chromatographic system (see Chromatography 621)— Prepare as directed in the Assay. Chromatograph the System suitability solution, and record the peak responses as directed for Procedure: the resolution, R, between fenofibrate and fenofibrate related compound B is not less than 3.0; the column efficiency for the fenofibrate related compound B peak is not less than 3000 theoretical plates; and the tailing factor is not more than 2.0. Chromatograph the Sensitivity solution, and record the peak responses as directed for Procedure: the signal-to-noise ratio is not less than 10 for the fenofibrate peak. Chromatograph the Standard solution, and record the peak responses as directed for Procedure: the relative standard deviation for replicate injections is not more than 2.0% for each peak.

Procedure— Separately inject equal volumes (about 20 µL) of the Standard solution and the Test solution into the chromatograph, record the chromatograms, and measure the peak responses. Calculate the percentage of fenofibrate related compound B relative to the fenofibrate labeled content in the portion of Capsules taken by the formula: in which CS is the concentration, in mg per mL, of fenofibrate related compound B in the Standard solution; CT is the concentration, in mg per mL, of fenofibrate in the Test solution, based on the label claim; and ri and rS are the responses of fenofibrate related compound B obtained from the Test solution and the Standard solution, respectively. Calculate the percentage of any other impurity relative to the fenofibrate labeled content in the portion of Capsules taken by the formula: in which CF is the concentration, in mg per mL, of fenofibrate in the Standard solution; CT is as defined above; ri is the peak response of each impurity obtained from the Test solution; and rF is the peak response of the fenofibrate, obtained from the Standard solution. Not more than 0.5% of fenofibrate related compound B is found; not more than 0.2% of any other impurity is found; and not more than 2.0% of total impurities is found.

Buffer solution pH 2.9— Dissolve 136 g of monobasic potassium phosphate in 1000 mL of water, and adjust with dilute phosphoric acid (1 in 10) to a pH of 2.9 ± 0.05.

Mobile phase— Prepare a mixture of methanol and Buffer solution pH 2.9 (80:20). Make adjustments if necessary (see System Suitability under Chromatography 621).

Standard preparation— Dissolve an accurately weighed quantity of USP Fenofibrate RS in Mobile phase to obtain a solution having a known concentration of about 0.067 mg per mL.

Assay preparation— Accurately weigh the contents of not fewer than 20 Capsules. Mix the contents, and transfer an accurately weighed portion of the powder, equivalent to about 67 mg of fenofibrate, to a 100-mL volumetric flask. Fill the flask to about 80% with Mobile phase, sonicate for 10 minutes, stir for 15 minutes, and dilute with Mobile phase to volume. Quantitatively dilute 5.0 mL of this solution to 50 mL with Mobile phase, and pass a portion of this solution through a 0.45-µm PVDF filter, discarding the first 5 mL. The final concentration based on the label claim is about 0.067 mg per mL.

Chromatographic system (see Chromatography 621)— The liquid chromatograph is equipped with a 285-nm detector and a 4.6-mm × 15-cm column that contains 5-µm packing L1. The flow rate is about 1.0 mL per minute. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the column efficiency is not less than 6000 theoretical plates; the tailing factor is not more than 2.0; and the relative standard deviation for replicate injections is not more than 2.0%.

Procedure— Separately inject equal volumes (about 20 µL) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the responses for the major peaks. Calculate the percentage of the labeled amount of fenofibrate (C20H21ClO4) in the portion of Capsules taken by the formula: in which CS is the concentration, in mg per mL, of fenofibrate in the Standard preparation; CU is the concentration, in mg per mL, of fenofibrate in the Assay preparation, based on the label claim; and rU and rS are the peak areas obtained from the Assay preparation and the Standard preparation, respectively.USP32