Identification
A:
Shake well a quantity of powdered Tablets,equivalent to about 100mg of quinine sulfate,with 100mLof dilute sulfuric acid (1in 350),and filter.An appropriate dilution of the filtrate exhibits a vivid blue fluorescence.On the addition of a few drops of hydrochloric acid the fluorescence disappears.
B:
In the test for
Chromatographic purity,the
RFvalue of the principal spot obtained from the
Test preparationcorresponds to that from the
Standard preparation.
C:
Shake a quantity of powdered Tablets,equivalent to about 20mg of quinine sulfate,with 10mLof dilute hydrochloric acid (1in 100),and filter:the filtrate responds to the tests for Sulfate á191ñ.
D:
The retention time of the major peak in the chromatogram of the
Assay preparationcorresponds to that in the chromatogram of the
Standard preparation,obtained as directed in the
Assay.
Dissolution á711ñ
Medium:
0.01Nhydrochloric acid;900mL.
Apparatus 1:
100rpm.
Time:
45minutes.
Procedure
Determine the amount of (C
20H
24N
2O
2)
2·H
2SO
4·2H
2Odissolved by employing UVabsorption at the wavelength of maximum absorbance at about 248nm on filtered portions of the solution under test,suitably diluted with
Dissolution Medium,in comparison with a Standard solution having a known concentration of
USP Quinine Sulfate RSin the same
Medium.
Tolerances
Not less than 75%(Q)of the labeled amount of (C20H24N2O2)2·H2SO4·2H2Ois dissolved in 45minutes.
Chromatographic purity
Shake a quantity of powdered Tablets,equivalent to about 150mg of quinine sulfate,with 25mLof diluted alcohol for 10minutes,and filter.Using this as the test solution,proceed as directed in the test for
Chromatographic purityunder
Quinine Sulfate.
Assay
Standard preparation
Transfer about 20mg of
USP Quinine Sulfate RS,accurately weighed,to a 100-mLvolumetric flask,dissolve in and dilute with
Mobile phaseto volume,and mix.
Assay preparation
Weigh and finely powder not less than 20Tablets.Transfer an accurately weighed portion of the powder,equivalent to about 160mg of quinine sulfate,to a 100-mLvolumetric flask,add 80mLof methanol,and shake the flask by mechanical means for 30minutes.Dilute with methanol to volume,and filter,discarding the first 10mLof the filtrate.Transfer 3.0mLof the filtrate to a 25-mLvolumetric flask,dilute with Mobile phaseto volume,and mix.
Procedure
(see
Chromatography á621ñ)Inject equal volumes (about 50µL)of the
Standard preparationand the
Assay preparationinto a chromatograph equipped with a 235-nm detector and a 3.9-mm ×30-cm column that contains packing L1.Calculate the quantity,in mg,of the sum of quinine sulfate and dihydroquinine sulfate in the portion of Tablets taken by the formula:
(2500/3)C(rb,U+rd,U)/(rb,S+rd,S),
in which
Cis the concentration,in mg per mL,of
USP Quinine Sulfate RSin the
Standard preparation,
rb,Uand
rb,Sare the peak area responses of quinine obtained from the
Assay preparationand the
Standard preparation,respectively,and
rd,Uand
rd,Sare the peak area responses of dihydroquinine obtained from the
Assay preparationand the
Standard preparation,respectively.