This paper investigates the possibility of utilizing ninhydrin as a reagent to help simultaneously detect metformin and glibenclamide from a core/shell system of PCL-PEG/PEG nanofibers. For this estimation, core/shell nanofibers of PEG-PCL/PEG were produced using coaxial electrospinning setup. Reagent ninhydrin was used to shift the absorbance maxima to visible wavelength. Q-Analysis method was employed to simultaneously detect release concentration of both metformin and glibenclamide at absorbance maximum of 570 and 300 nm. Calibration curves and Absorptivities of each sample was calculated and statistical analysis shows that the method is viable to simultaneously determine metformin and glibenclamide from release system.