Valsartan Tablets

This article is compiled based on the United States Pharmacopeia (USP) – 2025 Edition

Issued and maintained by the United States Pharmacopeial Convention (USP)

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1 DEFINITION

Valsartan Tablets contain NLT 95.0% and NMT 105.0% of the labeled amount of valsartan (C₂₄H₂₉N₅O₃).

2 IDENTIFICATION

A. The retention time of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.

Add the following:

B. The UV spectrum of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.

3 ASSAY

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3.1 Procedure

Mobile phase: Acetonitrile, water, and glacial acetic acid (50:50:0.1)

Diluent: Acetonitrile and water (50:50)

System suitability solution: 2 µg/mL of USP Valsartan Related Compound B RS and 20 µg/mL of USP Valsartan RS in Diluent

Standard solution: 0.20 mg/mL of USP Valsartan RS in Diluent

Sample stock solution: Place NLT 20 Tablets in a suitable volumetric flask and add 10% of the flask volume of water. Stir or shake until the Tablets disintegrate (about 5 min). Add 80% of the flask volume of acetonitrile. Stir or shake for 30 min, and sonicate for 10 min. Cool, and dilute with acetonitrile to volume, mix, and centrifuge a portion of the suspension.

Sample solution: Nominally 0.2 mg/mL of valsartan from the Sample stock solution in Diluent

Chromatographic system

• (See Chromatography 〈621〉, System Suitability.)
• Mode: LC
• Detector: UV 230 nm. For Identification B, use a diode array detector in the range of 200–400 nm.
• Column: 4.6-mm × 25-cm; 10-µm packing L1
• Column temperature: 30°
• Flow rate: 1 mL/min
• Injection volume: 20 µL
• Run time: NLT 2 times the retention time of valsartan

System suitability

• Samples: System suitability solution and Standard solution
• Suitability requirements
• Resolution: NLT 1.5 between valsartan related compound B and valsartan, System suitability solution. [Note-The relative retention times for valsartan related compound B and valsartan are about 0.8 and 1.0, respectively.]
• Relative standard deviation: NMT 1.0 %, Standard solution

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of valsartan (C₂₄H₂₉N₅O₃) in the portion of Tablets taken:

Result = (rᵤ/rₛ) × (Cₛ/Cᵤ) × 100

rᵤ = peak response of valsartan from the Sample solution

rₛ = peak response of valsartan from the Standard solution

Cₛ = concentration of USP Valsartan RS in the Standard solution (mg/mL)

Cᵤ = nominal concentration of valsartan in the Sample solution (mg/mL)

Acceptance criteria: 95.0%–105.0%

4 PERFORMANCE TESTS

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4.1 Dissolution 〈711〉

4.1.1 Test 1

Medium: pH 6.8 phosphate buffer prepared as follows. Dissolve 6.805 g of monobasic potassium phosphate and 0.896 g of sodium hydroxide in water and dilute with water to 1000 mL. Adjust with 0.2 M sodium hydroxide or 1 M phosphoric acid as required to a pH of 6.8; 1000 mL degassed.

Apparatus 2: 50 rpm

Time: 30 min

Standard solution: (L/1000) mg/mL of USP Valsartan RS in Medium, where L is the label claim, in mg/Tablet. [Note-Dilute with Medium as needed.]

Sample solution: Pass a portion of the solution under test through a suitable filter.

Instrumental conditions

• Mode: UV
• Analytical wavelength: 250 nm
• Blank: Medium

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of valsartan (C₂₄H₂₉N₅O₃) dissolved:

Result = (Aᵤ/Aₛ) × (Cₛ/L) × V × 100

Aᵤ = absorbance of the Sample solution

Aₛ = absorbance of the Standard solution

C = concentration of USP Valsartan RS in the Standard solution (mg/mL)

L = label claim (mg/Tablet)

V = volume of Medium, 1000 mL

Tolerances: NLT 80% (Q) of the labeled amount of valsartan (C₂₄H₂₉N₅O₃) is dissolved.

4.1.2 Test 2 If the product complies with this test, the labeling 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 12 g of sodium hydroxide in 10 L of water. Adjust with 1 N sodium hydroxide or 1 N phosphoric acid to a pH of 6.8; 1000 mL.

Apparatus 2: 50 rpm

Time: 30 min

Standard stock solution: 0.4 mg/mL of USP Valsartan RS prepared as follows. Transfer an appropriate quantity of USP Valsartan RS into a suitable volumetric flask, and add methanol to about 5% of the volume of the flask. Sonicate to dissolve. Dilute with Medium to volume.

Standard solution: 0.02 mg/mL of USP Valsartan RS in Medium from Standard stock solution

Sample solution: Withdraw 10 mL of the solution under test and pass through a suitable filter. Dilute a portion of the solution with Medium to the concentration similar to that in the Standard solution.

Instrumental conditions

• Mode: UV
• Analytical wavelength: 250 nm
• Cell: 1.0 cm
• Blank: Medium
• System suitability
• Sample: Standard solution
• Relative standard deviation: NMT 2.0%

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of valsartan (C₂₄H₂₉N₅O₃) dissolved:

Result = (Aᵤ/Aₛ) × Cₛ × V × D × (1 / L) × 100

Aᵤ = absorbance of the Sample solution

Aₛ = absorbance of the Standard solution

Cₛ = concentration of USP Valsartan RS in the Standard solution (mg/mL)

V = volume of Medium, 1000 mL

D = dilution factor

L = label claim (mg/Tablet)

Tolerances: NLT 80% (Q) of the labeled amount of valsartan (C₂₄H₂₉N₅O₃) is dissolved.

4.2 Uniformity of Dosage Units 〈905〉

Meet the requirements

5 IMPURITIES

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5.1 Organic Impurities

Mobile phase, Diluent, System suitability solution, Sample solution, and Chromatographic system: Proceed as directed in the Assay.

Standard solution: 0.4 µg/mL of USP Valsartan RS in Diluent

Sensitivity solution: 0.1 µg/mL of USP Valsartan RS in Diluent, from the Standard solution

System suitability

• Samples: System suitability solution, Standard solution, and Sensitivity solution
• Suitability requirements
• Resolution: NLT 1.5 between valsartan related compound B and valsartan, System suitability solution. [Note-The relative retention times for valsartan related compound B and valsartan are about 0.8 and 1.0, respectively.]
• Relative standard deviation: NMT 5.0 %, Standard solution
• Signal-to-noise ratio: NLT 10, Sensitivity solution

Analysis

Samples: Sample solution and Standard solution

Calculate the percentage of each degradation product in the portion of Tablets taken:

Result = (rᵤ/rₛ) × (Cₛ/Cᵤ) × 100

rᵤ = peak response of each degradation product from the Sample solution

rₛ = peak response of valsartan from the Standard solution

Cₛ = concentration of USP Valsartan RS in the Standard solution (µg/mL)

Cᵤ = nominal concentration of valsartan in the Sample solution (µg/mL)

Acceptance criteria: See Table 1. Calculate the total degradation products from the sum of all individual degradation products. Disregard any peak due to valsartan related compound B. The reporting threshold is 0.05%.

Table 1

6 ADDITIONAL REQUIREMENTS

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Packaging and Storage: Preserve in tight containers. Store at controlled room temperature.

Labeling: When more than one test for Dissolution is given, the labeling states the Dissolution test used only if Test 1 is not used.

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USP Reference Standards 〈11〉

USP Valsartan RS

USP Valsartan Related Compound B RS

N-{[2’-(1H-Tetrazol-5-yl)biphenyl-4-yl]methyl}-N-butyryl-l-valine; Also known as N-Butyryl-N-{[2'-(1H-tetrazole-5-yl)biphenyl-4-yl]methyl}-l-valine.

C₂₃H₂₇N₅O₂  421.50