• S. Senthil Kumar Faculty of Pharmacy, Pacific Academy of Higher Education and Research University, Udaipur-313004, Rajasthan, India
  • Ritesh Kumar Srivastava Macleod’s Pharmaceuticals Limited, R&D center, Andheri-400059, Mumbai, India
  • V. Srinivasrao Faculty of Pharmacy, Pacific Academy of Higher Education and Research University, Udaipur-313004, Rajasthan



Impurity, HPLC, TTC, Validation, ICH guidelines


Objective: The objective of the present study was to develop and validate a specific and sensitive analytical method, which separate the genotoxic impurity 4, 4'-bis (bromomethyl) biphenyl from valsartan antihypertensive drug substance using HPLC method.

Methods: The development activity was conducted by HPLC with UV detector. The impurity was separated on Inertsil ODS 3V 250 x 4.6 mm, 5 µm analytical column with a mobile phase consisting of 5.5 pH buffer and acetonitrile with the gradient program at a flow rate 1.0 ml/min. The effluent was detected using UV detector attached with HPLC system at 275 nm meanwhile column temperature and injection volume was maintained to 35 °C and 50 μl respectively. Acetonitrile was selected as diluent for performing the experiment.

Results: Whole experiment and validation process was performed as per the ICH guideline. The LOD and LOQ value were found to be 0.153 µg/g and 0.463 µg/g respectively, while accuracy results were well in the range 97.62 to 104.59%. The linearity curve showed a correlation coefficient of 0.9994 and method was very sensitive.

Conclusion: From validation data, it was confirmed that the developed method is specific, sensitive, linear, precise and accurate for the determination of 4, 4'-bis (bromomethyl) biphenyl genotoxic impurity in valsartan drug substances.


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How to Cite

Kumar, S. S., R. K. Srivastava, and V. Srinivasrao. “DETERMINATION OF 4, 4′-BIS (BROMOMETHYL) BIPHENYL GENOTOXIC IMPURITY IN VALSARTAN DRUG SUBSTANCES BY HPLC”. International Journal of Pharmacy and Pharmaceutical Sciences, vol. 8, no. 11, Nov. 2016, pp. 209-15, doi:10.22159/ijpps.2016v8i11.14614.



Original Article(s)