Nadolol Tablets
»Nadolol Tablets contain not less than 90.0percent and not more than 110.0percent of the labeled amount of nadolol (C17H27NO4).
Packaging and storage— Preserve in tight containers.
Identification— Transfer a quantity of powdered Tablets,equivalent to about 50mg of nadolol,to a conical flask.Add 10mLof 0.1Nhydrochloric acid,stir for 30minutes,using a magnetic stirrer,and place in an ultrasonic bath for an additional 30minutes.Centrifuge,and use the supernatant for the test solution.Apply,as streaks,100µLof the test solution and 100µLof a Standard solution of USP Nadolol RSin 0.1Nhydrochloric acid having a concentration of about 5mg per mLto a thin-layer chromatographic plate (see Chromatography á621ñ)coated with a 0.25-mm layer of chromatographic silica gel mixture.Develop the chromatogram in a solvent system consisting of acetone,chloroform,and 2Nammonium hydroxide (8:1:1)until the solvent front has moved about three-fourths of the length of the plate.Remove the plate from the developing chamber,allow the solvent to evaporate,and examine the chromatogram under short-wavelength UVlight:the RFvalue of the principal spot obtained from the test solution corresponds to that obtained from the Standard solution.
Dissolution á711ñ
Medium: 0.01Nhydrochloric acid;900mL.
Apparatus 1: 100rpm.
Time: 50minutes.
Procedure— Determine the amount of C17H27NO4dissolved,employing the procedure set forth in the Assay,except to prepare the Mobile phaseusing 560mLof methanol and 1440mLof water instead of 700mLand 1300mL,respectively,and adjusting with 0.1Nhydrochloric acid to a pHof 2.5.Use filtered portions of the solution under test,suitably diluted with Dissolution Medium,if necessary,in comparison with a Standard solution having a known concentration of USP Nadolol RSin the same Medium.
Tolerances— Not less than 80%(Q)of the labeled amount of C17H27NO4is dissolved in 50minutes.
Uniformity of dosage units á905ñ: meet the requirements.
Mobile phase— Prepare a filtered and degassed mixture of 700mLof methanol and 1300mLof water containing 5.84g of sodium chloride and 1.0mLof 0.1Nhydrochloric acid.
Standard preparation— Dissolve an accurately weighed quantity of USP Nadolol RSin Mobile phaseto obtain a solution having a known concentration of about 0.2mg per mL.
Assay preparation— Weigh and finely powder not less than 20Tablets.Weigh accurately a portion of the powder,equivalent to about 20mg of nadolol,and transfer to a 100-mLvolumetric flask.Add about 75mLof Mobile phase,place in an ultrasonic bath for 15minutes,shaking intermittently,add Mobile phaseto volume,and mix.Clarify the solution by filtration or centrifugation.
Chromatographic system (see Chromatography á621ñ)—The liquid chromatograph is equipped with a 220-nm detector and a 4.6-mm ×25-cm column that contains packing L16.The flow rate is about 1mLper minute.Chromatograph replicate injections of the Standard preparation,and record the peak responses as directed for Procedure:the relative standard deviation is not more than 2.0%;and the tailing factor for the nadolol peak is not more than 3.
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 nadolol (C17H27NO4)in the portion of Tablets taken by the formula:
in which Cis the concentration,in mg per mL,of USP Nadolol RSin the Standard preparation;and rUand rSare the peak responses obtained from the Assay preparationand the Standard preparation,respectively.
Auxiliary Information— Staff Liaison:Andrzej Wilk,Ph.D.,Senior Scientific Associate
Expert Committee:(PA5)Pharmaceutical Analysis 5
USP28–NF23Page 1321
Phone Number:1-301-816-8305