SIMULTANEOUS DETERMINATION OF HEAVY-METAL S AT PPM LEVEL IN BOVINE LIVER BY AUTOMATED REVERSED-PHASE HPLC INVOLVING PRECOLUMN CHELATION WITH HEXAMETHYLENEDITHIOCARBAMATE AND ONLINE COLUMN ENRICHMENT
S. Ichinoki et al., SIMULTANEOUS DETERMINATION OF HEAVY-METAL S AT PPM LEVEL IN BOVINE LIVER BY AUTOMATED REVERSED-PHASE HPLC INVOLVING PRECOLUMN CHELATION WITH HEXAMETHYLENEDITHIOCARBAMATE AND ONLINE COLUMN ENRICHMENT, Bunseki Kagaku, 45(9), 1996, pp. 837-844
Various procedures for reversed-phase HPLC determination of Cd, Ni, Pb
, Zn, Cu, Hg, Co, and Bi as their hexamethylenedithiocarbamate (HMDC)
chelates have been automated. The optimum analytical conditions were i
nvestigated for determination of the heavy metals in the standard refe
rence material (Bovine Liver) of National Institute of Standards and T
echnology (NIST). A 100 mg sample was ashed with nitric and perchloric
acid, and the residual acids evaporated. The resulting residue was th
en dissolved with diluted hydrochloric acid, and an aliquot of the sol
ution was used for the HPLC analysis. The preparation of the standard
solutions for calibration curves, chelation of metal ions, on-line enr
ichment of the HMDC chelates on a Capcell C-18 mini-column (10 X 4.0 m
m i.d.), separation of the chelates on a Cosmosil 5C(18)-MS analytical
column (250 X 4.6 mm i.d.), and detection at 260 nm were all carried
out with an optimum pretreatment program and a rime program. The analy
tical results of Zn and Cu (Zn: 124 +/- 2, Cu: 156 +/- 3 mu g/g) were
in good agreement with the certified values of NIST (Zn: 123 +/- 8, Cu
: 158 +/- 7 mu g/g), and the precision of the present method was also
good (about 2%).