method validation of drug quantification poster

Abstract

A lowest detection limit with straight linearity were obtained by developing a method to analyze Phenacetin (Phe) in both aqueous and organic extraction by using Liquid chromatography Triple Quoadrpole mass with electrospray ionization (LCMSMS/ESI). The validation of the developed method was carried out according to ICH Harmonized Tripartite guideline. Validation criteria obtained were; the method detection limit MDL is 0.089 ng/ml, method quantification limit MQL is 0.19 ng/ml while the calibration curve linear from 0.1 to 1000 ng/mL with correlation coefficient R2 is 0.9994, Accuracy and precision up to 97% and the repeatability inter and intraday for six replicates of three concentration with RSD 2.1%. Separation occurred using Nova Pack C18 4 um, 150 x 3.9 mm column, using acetonitrile : 0.1% Formic acid 60:40% (v:v) at flow rate 1ml/min. the detector was triple quad mass spectrometry at multi-reaction mode MRM to detect parent mass 180.1 at frag 97 to transition fragments 110 and 138 at collision voltages 16 and 12 respectively.