Spectrofluorimetric determination of vitamin K3 by a solid-phase zinc reactor immobilized in a flow injection...

The spectrofluorimetric determination of vitamin K3 (menadione) using a flow injection (FI) assembly provided with a solid-phase reactor with immobilized zinc is described. The naphthohydroquinone was produced by means of two coupled steps in the FI system: hydrolysis of the sodium sulfite derivative of the menadione in a basic medium and reduction of the generated menadione in the zinc reactor in an acidic medium. The fluorescent product was monitored spectrofluorimetrically (lambda ex 325 nm; lambda em 425 nm). The calibration graph was linear over the range 0.1-18 micrograms ml-1 with a reproducibility of 1.6%; the limit of detection was 0.005 microgram ml-1 and the sample throughput was 70 h-1. The influence of foreign compounds was studied and the procedure was applied to the determination of vitamin K3 in three different pharmaceutical formulations.