Development and Validation of an LC-MS/MS Method for Quantitative Analysis of Tamsulosin in Human Plasma Using Propranolol as an Internal Standard: Application to Pharmacokinetic Studies

Abstract

This study presents the development and validation of a robust analytical method for quantifying Tamsulosin in human plasma using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Propranolol was utilized as an internal standard (IS) to improve analytical precision and accuracy. Method validation followed ICH M10 guidelines, including specificity, linearity, accuracy, precision, matrix effect, and recovery assessments. Plasma samples were prepared via protein precipitation with acetonitrile and analyzed using an Agilent Zorbax SB-C18 column with a gradient mobile phase of 0.3% formic acid in water and methanol. The detection utilized a Quattro Micro triple-quadrupole mass spectrometer operating in positive electrospray ionization (ESI) mode. Calibration curves demonstrated linearity over a range of 0.125–32 ppb with a correlation coefficient (r²) greater than 0.99. Inter- and intra-day precision and accuracy met acceptance criteria, with percent relative standard deviation (RSD%) and deviation within ±15% across all quality control (QC) levels. Specificity tests confirmed negligible interference from blank plasma, and matrix effects were within acceptable limits. The method demonstrated excellent recovery rates for both Tamsulosin and Propranolol. Application of the validated method to a pharmacokinetic study in healthy volunteers revealed the time-concentration profile of Tamsulosin following oral administration. The developed method is efficient, sensitive, and suitable for routine clinical and bioequivalence studies of Tamsulosin.