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Published:
Journal of Analytical Toxicology,
ISSN 0146-4760,
Volume 31, Number 2, March 2007,
pp.81-86
Electrospray LC–MS Method with Solid-Phase Extraction
for Accurate Determination of Morphine-, Codeine-, and Ethylmorphine-Glucuronides
and 6-Acetylmorphine in Urine
J.-O. Svensson, M. Andersson, E. Gustavsson, and O. Beck
Department of Medicine, Division of Clinical Pharmacology, Karolinska University
Hospital, Stockholm, Sweden
A method for the identification and quantification of morphine-
3-glucuronide, codeine-6-glucuronide, ethylmorphine-6-glucuronide, and 6-acetylmorphine
in human urine based on solid-phase extraction (SPE) and electrospray ionization
liquid chromatography–mass spectrometry (LC–MS) was validated for
use as a confirmation procedure in combination with immunochemical screening
for opiates. Three deuterium-labelled analogues were used as internal standards:
morphine-3-glucuronide-d3, codeine-d3, and 6-acetylmorphine-d3. Fifty-microliter
aliquots of urine were prepared by SPE using 30-mg Oasis HLB cartridges. The
chromatographic system consisted of a 2.0 ¥ 100-mm C18 column and the gradient
elution buffers used acetonitrile and 25 mmol/L formic acid. The protonated
molecular ions were monitored in the selected ion monitoring mode together with
one qualifier ion for each analyte. The interassay variability was less than
10% at the reporting limit 30 ng/mL for 6-acetylmorphine and 300 ng/mL for the
other analytes. The method was validated by comparison with a reference gas
chromatographic (GC)–MS method using authentic urine samples. The two
methods agreed completely regarding identified analytes, and for the quantitative
results there were slightly lower levels when measuring glucuronides directly
as compared to total determination after hydrolysis by GC–MS. This result
was to be expected because the free compounds are not measured with the LC–MS
method. This study concludes that the presented LC–MS method is robust
and reliable, and suitable for use as a confirmation method in clinical urine
drug testing for opiates.
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