BIOANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF ENTRECTINIB IN RAT PLASMA BY LIQUID CHROMATOGRAPHY–TANDEM MASS SPECTROMETRY

  • PRAVALLIKA KE Department of , University College of Pharmaceutical Sciences, Acharya Nagarjuna University, Andhra Pradesh, India.
  • PRAMEELA RANI A Department of , University College of Pharmaceutical Sciences, Acharya Nagarjuna University, Andhra Pradesh, India.
  • RATNA KUMAR M Department of , University College of Pharmaceutical Sciences, Acharya Nagarjuna University, Andhra Pradesh, India.

Abstract

Objective: The objective of the study was to develop and validate the bioanalytical liquid chromatography–mass spectrometry (LCMS/MS) method for the estimation of entrectinib in bulk and pharmaceutical drugs in rat plasma.


Methods: Chromatographic separation of entrectinib with D4-entrectinib as internal standard (IS) was achieved using Waters Alliance high-performance liquid chromatography system, quaternary gradient pump of e2695, using Luna, 250×4.6 mm, 5 μm column and the mobile phase containing 0.1% formic acid and acetonitrile (ACN) within the ratio of 70:30% v/v. The flow was 1.0 ml/min; detection was carried out by absorption at 294 nm using a photodiode array detector at ambient temperature.


Results: The peak of entrectinib was eluted at retention times of 5.225 min. The multiple reaction monitoring was 560.6/475.1 (m/z) for entrectinib and 580.6/496.3 (m/z) for IS entrectinib (D4). The linearity range was 1–20 ng/ml with a regression coefficient of 0.999. % relative standard deviation of peak areas of all measurements always <2.0.


Conclusion: The method was successfully validated and it had been found to be within limits for accuracy, precision, and linearity and it is stable under analytical conditions used.

Keywords: Liquid chromatography–mass spectrometry, Entrectinib, D4 - entrectinib

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KE, P., P. RANI A, and R. KUMAR M. “BIOANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF ENTRECTINIB IN RAT PLASMA BY LIQUID CHROMATOGRAPHY–TANDEM MASS SPECTROMETRY”. Asian Journal of Pharmaceutical and Clinical Research, Vol. 13, no. 11, Oct. 2020, pp. 155-63, doi:10.22159/ajpcr.2020.v13i11.39005.
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