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Published:
Journal of Analytical Toxicology,
ISSN 0146-4760,
Volume 25,
Number 2, March 2001, pp. 137-143
Improved Solid-Phase
Extraction Method for Systematic Toxicological Analysis in Biological Fluids
T. Soriano*,
C. Jurado, M. Menéndez, and M. Repetto
Instituto Nacional de Toxicología, P.O. Box 863, E-41080 Sevilla, Spain
A
method for the simultaneous qualitative and quantitative determination of drugs
of abuse (opiates, cocaine, or amphetamines) and prescribed drugs (tricyclic
antidepressants, phenotiazines, benzodiazepines, etc.) in biological fluids—
blood, urine, bile, and gastric contents—was developed. This procedure
involves solid-phase extraction with Bond-Elut Certify columns followed by analysis
by gas chromatography– nitrogen-phosphorus detection (GC–NPD) and
confirmation by gas chromatography–mass spectrometry (GC–MS), after
derivatization, when necessary. Pretreatment was performed on all samples: sonication
for 15 min plus enzymatic hydrolysis with b-glucuronidase in urine. With respect
to the internal standards, nalorphine and trihexylamine were used for basic
substances, allobarbital for acidic drugs, and prazepam for benzodiazepines.
Acidic and basic compounds were extracted from different aliquots of samples
at different pH levels: 6–6.5 for the acidic and neutral and 8–8.5
for the basic and the benzodiazepines. Several areas of experimental design
were considered in the process of method optimization. These included internal
standards, pH, sonication, flow rate and washing solvents. It was found that
systematic analysis could be reliably performed using optimized extraction conditions.
The recovery rates for the compounds tested were always higher than 61.02%. Reproduction
of editorial content of this journal is prohibited without publisher’s
permission.
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