DETERMINATION OF 4, 4′-BIS (BROMOMETHYL) BIPHENYL GENOTOXIC IMPURITY IN VALSARTAN DRUG SUBSTANCES BY HPLC
DOI:
https://doi.org/10.22159/ijpps.2016v8i11.14614Keywords:
Impurity, HPLC, TTC, Validation, ICH guidelinesAbstract
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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