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Published:
Journal of Analytical Toxicology,
ISSN 0146-4760,
Volume 25,
Number 4, May/June 2001, pp. 250-257
Here is where the title stuff goes
HPLC
with Simultaneous UV and Reductive Electrochemical Detection at the Hanging
Mercury Drop Electrode: A Highly Sensitive and Selective Tool for the Determination
of Benzodiazepines in Forensic Samples
Maria Wilhelm1, Hans-Jürgen Battista2, and Dagmar Obendorf1
1 Institute of Analytical Chemistry and Radiochemistry and
2 Institute of Forensic Medicine, University of Innsbruck, Innrain 52a, A-6020
Innsbruck, Austria
A versatile, sensitive, and selective high-performance liquid
chromatographic (HPLC) procedure for the determination of common benzodiazepines
and some of their most frequently occurring metabolites in forensic samples
was developed and optimized with respect to effective and rapid sample preparation
and high selectivity of the analytical assay. The optimized method includes
liquid–liquid extraction of the drugs with chloroform followed by isocratic
reversed-phase chromatography on a LiChrospher-100 RP-8ec column (150 ¥
4.6-mm i.d.) with a mobile phase consisting of 0.03 mol/L acetate buffer (pH
4.6)/acetonitrile (55:45, v/v). The use of dual-mode detection made up of UV-detection
(250 nm) in series with reductive electrochemical detection (–1.4 V vs.
Ag/AgCl) at the hanging mercury drop electrode permits the detection and quantitation
of benzodiazepines even in degraded samples with higher selectivities than usually
reached with conventional HPLC techniques. Depending on the actual benzodiazepine
species, detection limits are in the range of 2.0 to 14.1 ng/mL. Mean recovery
values of the drugs from blood range from 82 to 92%; within-day and day-to-day
repeatabilities typically lie between 3 and 9%. Several case work examples demonstrate
the high selectivity and remarkably low matrix sensitivity of the described
assay.
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