Y. Nagaosa et T. Kobayashi, COMPARISON OF ON-COLUMN AND PRECOLUMN DERIVATIZATION FOR LIQUID-CHROMATOGRAPHIC DETERMINATION OF MOLYBDENUM IN SEAWATER AND BOVINE LIVER, Journal of AOAC International, 78(5), 1995, pp. 1307-1311
A rapid, accurate, and sensitive method was developed for the determin
ation of molybdenum in seawater and bovine liver-samples by reversed-p
hase liquid chromatography (LC) using a C-18 column, The method was;ba
sed on chelation of the metal with 8-hydroxyquinoline by on-column or
precolumn derivatization followed by LC elution with acetonitrile-0.02
M acetate buffer (3 + 2; pH 4.7) and 1 x 10-(3)M of the ligand as the
mobile phase. The spectrophotometric detection was made at 390 nm. Dat
a obtained from the 2 derivatizations (on- and precolumn chelation) we
re compared in terms of detection limit, precision, accuracy, and ease
of LC determination of molybdenum. No significant difference exists i
n the detection limit and the sensitivity of the 2 methods. However, t
he on-column chelation method, that is, the direct injection of aqueou
s samples onto the column, showed relatively less interference from ma
nganese and greater simplicity in operation compared with precolumn ch
elation; therefore, on-column chelation is preferable for routine anal
yses. The on-column method produced mean levels of 9.6 +/- 0.4 mu g/L
for the seawater sample and 3.6 +/- 0.2 mu g/g (certified value, 3.5 /- 0.5 mu g/g) for bovine liver.