Dissolution á711ñ
Medium:
sodium lauryl sulfate solution (2in 100);900mL.
Apparatus 2:
50rpm.
Time:
45minutes.
Procedure
Determine the amount of C
15H
16O
2dissolved by employing UVabsorption at the wavelengths of maximum and minimum absorbance at about 270nm and 296nm,respectively,on filtered portions of the solution under test,suitably diluted with
Medium,if necessary,in comparison with a Standard solution having a known concentration of
USP Nabumetone RSin the same
Medium.
Tolerances
Not less than 75%(Q)of the labeled amount of C15H16O2is dissolved in 45minutes.
Assay
Mobile phase
Prepare a solution of 6mLof glacial acetic acid in 350mLof water.Adjust with 1Nsodium hydroxide to a pHof 3.7,and dilute with water to obtain 400mL.Prepare a filtered and degassed mixture of acetonitrile and this solution (3:2).Make adjustments if necessary (see
System Suitabilityunder
Chromatography á621ñ).
Standard preparation
Dissolve an accurately weighed quantity of
USP Nabumetone RSin a mixture of methanol and water (9:1)to obtain a solution having a known concentration of about 0.5mg per mL.
Assay preparation
Weigh and finely powder not fewer than 20Tablets.Transfer an accurately weighed portion of the powder,equivalent to about 500mg of nabumetone,to a 1000-mLvolumetric flask,add about 100mLof water,and stir with the aid of a magnetic stirrer for 5minutes.Dilute with methanol to volume,stir for another 15minutes,and filter.
Chromatographic system (see Chromatography á621ñ)
The liquid chromatograph is equipped with a 280-nm detector and an 8-mm ×10-cm column that contains 10-µm packing L1.The flow rate is about 2mLper minute.Chromatograph the
Standard preparation,and record the peak responses as directed for
Procedure:the column efficiency is not less than 1500theoretical plates;the tailing factor is not more than 1.5;and the relative standard deviation for replicate injections is not more than 2.0%.
Procedure
Separately inject equal volumes (about 20µL)of the
Standard preparationand the
Assay preparationinto the chromatograph,record the chromatograms,and measure the responses for the major peaks.Calculate the quantity,in mg,of nabumetone (C
15H
16O
2)in the portion of Tablets taken by the formula:
1000C(rU/rS),
in which
Cis the concentration,in mg per mL,of
USP Nabumetone RSin the
Standard preparation;and
rUand
rSare the peak responses obtained from the
Assay preparationand the
Standard preparation,respectively.