Page 41 - Modern Derivatization Methods for Separation Sciences

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Analytical parameters: Range, 0.25-4.0 ng/ml; recoveries of digoxin and its metabolites from serum
ranged from 62-86%; coefficients of variance, 5.8%-20.9%.
GABA-Agonists

Baclofen in human plasma [34].

Derivatization: Precolumn derivatization with o phthalaldehyde-tert.-butanethiol

Clean-up: SCX solid-phase extraction

Detection: Electrochemical

Analytical parameters: LOQ, 10 ng/ml; within and between-day R.S.D., <10%; inaccuracy, <7%.

Excitatory Amino Acid Antagonists

Enantioselective determination of eliprodil in human plasma and urine [35].

Derivatization: Precolumn derivatization with (S)(+)-naphthylethyl isocyanate

Clean-up: Liquid-liquid extraction and columnswitching HPLC

Detection: Fluorescence, Ex. 275 nm and Em. 336 nm

Analytical parameters: Range, 0.15-10 ng/ml for unchanged eliprodil enantiomers in plasma; 50-25
000 ng/ml for total (conjugated) eliprodil enantiomers in urine; LOQ, 0.15 ng/ml for each unchanged
enantiomer in plasma; 50 ng/ml for each unchanged enantiomer in urine.

Serotonin Uptake Inhibitors

Simultaneous determination of D-fenfluramine (FEN), D-norfenfluramine (NF) and fluoxetine
(FLX) in plasma, brain tissue and brain microdialysate [36].
Derivatization: Precolumn derivatization with dansylchloride

Analytical parameters: LOQ, 200 fmol for FEN and NF; 500 fmol for FLX in brain microdialysate, and
1 pmol for NF and FEN and 2 pmol for FLX in plasma; inter-assay variability (relative standard
deviation), 6.6%, 6.9% and 9.3% for FEN, 4.6%, 3.7% and 7.9% for NF and 10.4%, 4.9% and 12.2%
for FLX; for brain microdialysate (2 pmol/µL), plasma (2 pmol/µL) and brain tissue (50 pmol /mg);
extraction recovery, 108% and 48% for FEN, 105% and 78% for NF and 94% and 45% for FLX; in
plasma (2 pmol/µL) and brain tissue (5 pmol/mg).

Analgesics

Enantioselective determination of eliprodil in human plasma [37].

Derivatization: Precolumn derivatization with R(+)-1-(1-naphthyl)ethylamine

Detection: Fluorescence

Analytical parameters: Range, 20-2000 ng/ml for each enantiomer; LOQ, 20 ng/ml for each enantiomer;

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