M. Horie et al., SIMULTANEOUS DETERMINATION OF ENROFLOXACI N AND ITS PRIMARY METABOLITE CIPROFLOXACIN IN MEAT AND FISH BY HPLC, Shokuhin Eiseigaku Zasshi, 38(5), 1997, pp. 329-334
A simple, reliable and sensitive method for the simultaneous determina
tion of residual enrofloxacin and its primary metabolite, ciprofloxaci
n, in meat and fish by HPLC has been developed. The drugs were extract
ed with 0.3% metaphosphoric acid-acetonitrile (6:4), and the extracts
were cleaned up on an Oasis HLB cartridge. The HPLC separation was car
ried out on a TSK-GEL Super ODS column(100 x 4.6 mm i.d.) with 0.05 mo
l/L phosphate buffer (pH 2.5)-acetonitrile (70 : 30) containing 1.0 mm
ol/L sodium dodecyl sulfate (SDS) as the mobile phase at a flow rate o
f 0.5 mL/min. A fluorescence detector was operated at an excitation wa
velength of 278 nm and an emission wavelength of 445 nm. The calibrati
on graphs were rectilinear from 0.5 to 20 ng for both drugs. The recov
eries of the drugs from tissues fortified at the level of 0.2 mu g/g w
ere greater than 80%, and the detection limits were 0.005 mu g/g for b
oth drugs. The influence of baking on enrofloxacin and ciprofloxacin r
esidues in flatfish was investigated. Both drugs showed excellent ther
mal stability.