Printed on: Tue Aug 03 2021, 07:24:12 AM Official Status: Currently Official on 03-Aug-2021 DocId: 1_GUID-246E8105-39F4-49F7-B242-025D04DAD23C_4_en-US

(EST)
Printed by: Le Tran Official Date: Official as of 01-Dec-2017 Document Type: USP @2021 USPC
1

phosphoric acid as required to a pH of 6.8; 1000 mL

Valsartan Tablets degassed.
DEFINITION Apparatus 2: 50 rpm
Valsartan Tablets contain NLT 95.0% and NMT 105.0% of the Time: 30 min
labeled amount of valsartan (C24H29N5O3). Standard solution: (L/1000) mg/mL of USP Valsartan RS
in Medium, where L is the label claim, in mg/Tablet.
IDENTIFICATION [NOTE—Dilute with Medium as needed.]
• A. The retention time of the major peak of the Sample Sample solution: Pass a portion of the solution under test
solution corresponds to that of the Standard solution, as through a suitable filter.
obtained in the Assay. Analysis
Analytical wavelength: UV 250 nm
ASSAY Blank: Medium
• PROCEDURE Samples: Standard solution and Sample solution
Mobile phase: Acetonitrile, water, and glacial acetic acid Calculate the percentage of the labeled amount of
(50: 50: 0.1) valsartan (C24H29N5O3) dissolved:
Diluent: Acetonitrile and water (50:50)
System suitability solution: 2 µg/mL of USP Valsartan Result = (A U/A S) × (C S/L) × V × 100
Related Compound B RS and 20 µg/mL of USP Valsartan RS
in Diluent AU = absorbance of the Sample solution
Standard solution: 0.20 mg/mL of USP Valsartan RS in AS = absorbance of the Standard solution
Diluent CS = concentration of USP Valsartan RS in the Standard
Sample stock solution: Place NLT 20 Tablets in a suitable solution (mg/mL)
volumetric flask, and initially add water (10% of the volume

al
L = label claim (mg/Tablet)
of the flask). Stir or shake until the Tablets disintegrate V = volume of Medium, 1000 mL
(about 5 min). Add acetonitrile (about 80% of the volume
of the flask). Stir or shake for 30 min, and sonicate for Tolerances: NLT 80% (Q) of the labeled amount of
10 min. Cool, and dilute with acetonitrile to volume, mix, valsartan (C24H29N5O3) is dissolved.
and centrifuge a portion of the suspension. Test 2: If the product complies with this test, the labeling
Sample solution: Nominally 0.2 mg/mL of valsartan from
the Sample stock solution in Diluent
Chromatographic system
ci indicates that it meets USP Dissolution Test 2.
Medium: 0.067 M phosphate buffer prepared as follows.
Dissolve 91.2 g of monobasic potassium phosphate and
(See Chromatography á621ñ, System Suitability.) 12 g of sodium hydroxide in 10 L of water. Adjust with
Mode: LC 1 N sodium hydroxide or 1 N orthophosphoric acid to a
ffi
Detector: UV 230 nm pH of 6.8; 1000 mL.
Column: 4.6-mm × 25-cm; 10-µm packing L1 Apparatus 2: 50 rpm
Column temperature: 30° Time: 30 min
Flow rate: 1.0 mL/min Standard stock solution: 0.4 mg/mL of USP Valsartan RS
Injection size: 20 µL prepared as follows. Transfer an appropriate quantity of
System suitability USP Valsartan RS into a suitable volumetric flask, and add
O

Samples: System suitability solution and Standard solution methanol to about 5% of the volume of the flask. Sonicate
Suitability requirements to dissolve. Dilute with Medium to volume.
Resolution: NLT 1.5 between valsartan related Standard solution: 0.02 mg/mL of USP Valsartan RS in
compound B and valsartan, System suitability solution Medium from Standard stock solution
Relative standard deviation: NMT 2.0%, Standard Sample solution: Withdraw 10 mL of the solution under
solution test and pass through a suitable filter. Dilute a portion of
Analysis the solution with Medium to the concentration similar to
Samples: Standard solution and Sample solution that in the Standard solution.
Calculate the percentage of the labeled amount of valsartan Instrumental conditions
(C24H29N5O3) in the portion of Tablets taken: Mode: UV-Vis
Analytical wavelength: 250 nm
Result = (r U/r S) × (C S/C U) × 100 Cell: 1.0 cm
Blank: Medium
rU = peak response of valsartan from the Sample
System suitability
solution
rS = peak response of valsartan from the Standard Sample: Standard solution
solution Relative standard deviation: NMT 2.0%
CS = concentration of USP Valsartan RS in the Standard Analysis
solution (mg/mL) Samples: Standard solution and Sample solution
CU = nominal concentration of valsartan the Sample Calculate the percentage of the labeled amount of
solution (mg/mL) valsartan (C24H29N5O3) dissolved:

Acceptance criteria: 95.0%–105.0% Result = (A U/A S) × C S × V × D × (1/L) × 100

PERFORMANCE TESTS AU = absorbance of the Sample solution

• DISSOLUTION á711ñ AS = absorbance of the Standard solution
Test 1 CS = concentration of USP Valsartan RS in the Standard
Medium: pH 6.8 phosphate buffer prepared as follows. solution (mg/mL)
Dissolve 6.805 g of monobasic potassium phosphate and V = volume of Medium, 1000 mL
0.896 g of sodium hydroxide in and dilute with water to D = dilution factor
1000 mL. Adjust with 0.2 M sodium hydroxide or 1 M L = label claim (mg/Tablet)

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Printed on: Tue Aug 03 2021, 07:24:12 AM Official Status: Currently Official on 03-Aug-2021 DocId: 1_GUID-246E8105-39F4-49F7-B242-025D04DAD23C_4_en-US
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Printed by: Le Tran Official Date: Official as of 01-Dec-2017 Document Type: USP @2021 USPC
2

Tolerances: NLT 80% (Q) of the labeled amount of rS = peak response of valsartan from the Standard
valsartan (C24H29N5O3) is dissolved. solution
• UNIFORMITY OF DOSAGE UNITS á905ñ: Meet the CS = concentration of USP Valsartan RS in the Standard
requirements solution (µg/mL)
CU = nominal concentration of valsartan in the Sample
IMPURITIES solution (µg/mL)
• ORGANIC IMPURITIES
Mobile phase, Diluent, System suitability solution, Acceptance criteria
Sample solution, and Chromatographic system: Each individual impurity: NMT 0.2%
Proceed as directed in the Assay. Total impurities: NMT 0.4%. [NOTE—Calculate the total
Standard solution: 0.4 µg/mL of USP Valsartan RS in Diluent impurities from the sum of all individual impurity peaks.
Sensitivity solution: 0.1 µg/mL of USP Valsartan RS in Disregard any peak due to valsartan related compound B
Diluent, from the Standard solution and any peaks ≤0.05%.]
System suitability
Samples: Standard solution, Sensitivity solution, and System ADDITIONAL REQUIREMENTS
suitability solution • PACKAGING AND STORAGE: Preserve in tight containers.
Suitability requirements • LABELING: When more than one test for Dissolution is given,
Resolution: NLT 1.5 between valsartan related the labeling states the Dissolution test used only if Test 1 is
compound B and valsartan, System suitability solution not used.
Relative standard deviation: NMT 10.0%, Standard • USP REFERENCE STANDARDS á11ñ
solution USP Valsartan RS
Signal-to-noise ratio: NLT 10, Sensitivity solution USP Valsartan Related Compound B RS
Analysis N-Butyryl-N-{[2’-(1H-tetrazole-5-yl)biphenyl-4-yl]

al
Samples: Sample solution and Standard solution methyl}-L-valine.
Calculate the percentage of each individual impurity in the C23H27N5O3 421.49
portion of Tablets taken:

Result = (r U/r S) × (C S/C U) × 100 ci

rU = peak response of each impurity from the Sample
solution
ffi
O

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