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Ivan110 » Пт июн 26, 2015 6:14 pm
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Results:
Therapeutic Drug Monitoring
Issue: Volume 21(4), August 1999, p 484
Copyright: © 1999 Lippincott Williams & Wilkins, Inc.
Publication Type: [Abstracts: Sixth International Congress Of Therapeutic
Drug Monitoring And Clinical Toxicology]
ISSN: 0163-4356
Accession: 00007691-199908000-00233
[Abstracts: Sixth International Congress Of Therapeutic Drug Monitoring And
Clinical Toxicology]
DETERMINATION OF DEXAMETHASONE IN HUMAN AQUEOUS HUMOUR BY LC-MS
Larsson, T.1; Nordin, J.2*; Meurling, L.2
Author Information
1Tika Lakemedel AB, Box 2, S-221 000 Lund and 2Department of Clinical
Pharmacology, Huddinge University Hospital, S-141 86 Huddinge, *Chemalys AB,
Haninge, Sweden.
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Outline
Section Description
Abstract 225
The penetration of synthetic corticosteroids into human aqueous humour following
topical application has earlier been determined using the sensitive and specific
technique of GC-MS. However, this procedure demands a troublesome derivatization
procedure, which can be difficult to perform in a reproducible way, due to the
limited sample volumes available. We have developed a liquid chromatography mass
spectrometric method, working in positive chemical ionization mode. After the
addition of internal standard, 6-methyl-prednisolone, the sample was injected
directly on an RP-18 column, using 23 % tetrahydrofuran in water as an eluent.
The triple quadrupole of a Finnigan TSQ 700 Mass Spectrometer was used in
selective ionization mode with detection of m/z 465 for dexamethasone and m/z
447 for the internal standard.
The method was found to be specific i.e. no endogenous material was found to
interfere with the analysis and the assay was linear within the range 0.45 to 32
ng/mL. The variance in slope data from day to day was less than 3 %. The
sensitivity in the lower limit of detection was far below the lowest value found
in patient samples. Precision and accuracy were evaluated by running control
samples on three consecutive days in five-replicates at 2.5, 12.5 and 25 ng/mL.
Coefficient of variation and deviation data were less than 18 % at the lowest
control level and less than 10 % at the highest control level, both for intra-
and inter-day data. The method was found accurate and precise and gives an
apprehension of dexamethasone content in low volume samples (30 [mu]L). More
than 50 samples could be processed in one day.
Section Description
Cairns, Australia; September 13-17, 1999
Analytical Techniques and Quality Control
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