In this article we proposed a method for quantitative determination of active substance in pharmaceuticals via Raman scattering using potassium ferricyanide as internal standard. We approved this method in ketoprophenum quantitative determination in drug for veterinary use “Ketojekt”. The calculation of metrological requirements of procedures are established proposed method of calibration. Either we demonstrated the focalisation factor of laser beam affects on the method reproducibility. The method provides a precise, rapid, convenient to quantitative analysis that is more effective than the standard HPLC assay.