Simultaneous Estimation of Six Nitrosamine Impurities in Valsartan Using Liquid Chromatographic Method

Area of Science:

• Pharmaceutical Analysis
• Analytical Chemistry
• Drug Safety

Background:

• Nitrosamine impurities are carcinogenic and pose risks to human health.
• Effective analytical methods are crucial for detecting and controlling these impurities in pharmaceuticals.
• Ensuring drug safety and quality necessitates rapid and reliable detection solutions.

Purpose of the Study:

• To develop and validate a liquid chromatographic method for quantifying six specific nitrosamine impurities in valsartan.
• To establish a reliable analytical tool for assessing the safety of valsartan active pharmaceutical ingredient (API) and its formulations.
• To provide a method for the simultaneous estimation of multiple nitrosamine impurities.

Main Methods:

• Utilized a C18 column with a mobile phase of acetonitrile, water (pH 3.2), and methanol using gradient elution.
• Employed a detection wavelength of 228 nm.
• Validated the method according to International Conference on Harmonization Q2(R1) guidelines.

Main Results:

• The method achieved excellent separation of impurities and valsartan with sharp peaks.
• Demonstrated linearity (R² > 0.9996), precision (RSD < 2%), accuracy (99.02–100.16% recovery), and sensitivity (low LOD/LOQ).
• Successfully applied to estimate nitrosamine impurities in valsartan API and tablet formulations.

Conclusions:

• The developed HPLC method is suitable for simultaneous estimation of six nitrosamine impurities.
• The method is effective for valsartan raw material, tablets, and fixed-dose combinations.
• This validated method contributes to ensuring the safety and quality of valsartan products.