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Published:
Journal of Analytical Toxicology,
ISSN 0146-4760,
Volume 26, Number 5, July/August 2002,
pp. 296-302
Simultaneous Determination of Viloxazine, Venlafaxine,
Imipramine, Desipramine, Sertraline, and Amoxapine in Whole Blood: Comparison
of Two Extraction/Cleanup Procedures for Capillary Gas Chromatography with Nitrogen-Phosphorus
Detection
M.A. Martínez, C. Sánchez de la Torre,
and E. Almarza
Department of Chemistry, National Institute of Toxicology, Ministry of Justice,
C/Luis Cabrera 9, 28002 Madrid, Spain
A comparative study for the
simultaneous gas chromatographic (GC) resolution and detection of the six antidepressants
viloxazine, venlafaxine, imipramine, desipramine, sertraline, and amoxapine
in whole blood at concentration levels of 100–2000 ng/mL was developed.
Two extraction/cleanup analytical procedures were compared regarding their recovery,
precision, sensitivity and matrix purification efficiency. The first procedure
consists of the employment of Chem Elut columns (diatomaceous earth) and is
based on the principle of liquid–solid absorption extraction that is closely
related to conventional liquid–liquid extraction. The second focuses on
the use of Bond Elut Certify columns and a mixed SPE, reversed-phase and cation-exchange
sorbent, more recently developed for the market. Each procedure required 2.0
mL of whole blood extraction and injection into a capillary GC equipped with
a nitrogen-phosphorus detector. Mepivacaine was used as the extraction standard
(surrogate), and prazepam was used as the chromatographic standard. No interferences
were found, and the time for the chromatographic analysis was 16 min for one
sample. Recoveries of the compounds using Chem Elut columns at 500 ng/mL were
in the range of 28–74% with intra-assay and interassay precisions of less
than 7% and 19%, respectively. Limits of detection (LOD) and quantitation (LOQ)
ranged from 39 to 153 ng/mL and from 128 to 504 ng/mL, respectively. Recoveries
of the compounds using Bond Elut Certify columns at 500 ng/mL were in the range
of 64–86% with intra-assay and interassay precisions of less than 4% and
10%, respectively. LODs and LOQs ranged from 21 to 100 ng/mL and from 70 to
330 ng/mL, respectively. An excellent linearity was observed with both procedures
from the LOQs up to 2000 ng/mL. The use of the reversed-phase and cation-exchange
sorbent Bond Elut Certify showed advantages compared with Chem Elut columns
for the screening of these antidepressants such as higher recoveries, cleaner
extracts, better sensitivity, better precision, and less solvent consumption
and disposal. Reproduction
of editorial content of this journal is prohibited without publisher’s
permission.
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