Dissolution á711ñ
[NOTEProtect solutions from light throughout this test.
]
Medium:
0.01Nhydrochloric acid;900mL.
Apparatus 2:
50rpm.
Time:
45minutes.
Procedure
Determine the amount of C
15H
14F
3N
3O
4S
2dissolved by employing UVabsorption at the wavelength of maximum absorbance at about 271nm on filtered portions of the solution under test,suitably diluted with water,if necessary,in comparison with a Standard solution having a known concentration of
USP Bendroflumethiazide RSin the same
Medium.
Tolerances
Not less than 75%(Q)of the labeled amount of C15H14F3N3O4S2is dissolved in 45minutes.
Assay
[NOTEUse low-actinic glassware for the
Assay preparation and the
Standard preparation.]
Mobile phase
Dissolve 5.62g of sodium chloride and 1.97g of anhydrous sodium acetate in 1000mLof water in a 2-liter volumetric flask.Add 4.0mLof glacial acetic acid and 800mLof methanol,dilute with water to volume,mix,filter,and degas.
Standard preparation
Dissolve an accurately weighed quantity of
USP Bendroflumethiazide RSin methanol,and dilute quantitatively and stepwise with methanol to obtain a solution having a known concentration of about 50µg per mL.
Assay preparation
Weigh and finely powder not fewer than 20Tablets.Transfer an accurately weighed portion of the powder,equivalent to about 5mg of bendroflumethiazide,to a 100-mLvolumetric flask,add about 70mLof methanol,and sonicate for 15minutes,with occasional shaking.Dilute with methanol to volume,mix,and centrifuge a portion of the solution for 15minutes.
Chromatographic system
(see
Chromatography á621ñ)The liquid chromatograph is equipped with a 270-nm detector and a 4.6-mm ×30-cm column that contains packing L11maintained at a temperature of 35±5

.The flow rate is about 1.5mLper minute.Chromatograph five replicate injections of the
Standard preparation,and record the peak responses as directed for
Procedure:the relative standard deviation is not more than 3.0%,and the tailing factor 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 response of the major peak.Calculate the quantity,in mg,of C
15H
14F
3N
3O
4S
2in the portion of Tablets taken by the formula:
0.1C(rU/rS),
in which
Cis the concentration,in µg per mL,of
USP Bendroflumethiazide RSin the
Standard preparation,and
rUand
rSare the peak responses obtained from the
Assay preparationand the
Standard preparation,respectively.