Krizman-Matasic, I.; Kostanjevecki, P.; Ahel, M.; Terzić, S.
(2018)
Simultaneous analysis of opioid analgesics and their metabolites in
municipal wastewaters and river water by liquid
chromatography–tandem mass spectrometry.
Journal of Chromatography A, 1533
.
pp. 102-111.
ISSN 0021-9673
Abstract
Although published literature provides a clear demonstration of widespread occurrence of opioid analgesics (OAs) in the aquatic environment, analytical methods suitable for a systematic study of this pharmaceutical class, which would include a broad spectrum of opioid analgesics and their metabolites, are still missing. In this work, a comprehensive multiresidue method for quantitative analysis of 27 opioid analgesics and their metabolites, including 2 morphine glucuronide conjugates, was developed and validated for three matrices: raw wastewater (RW), secondary effluent (SE) and river water.
The method comprised different classes of opioid analgesics, including natural opiates (morphine and
codeine),their semi-synthetic derivatives (hydrocodone, hydromorphone, oxycodone, oxymorphone and
buprenorphine) as well as fully synthetic opioids such as methadone, fentanyl, sufentanil, propoxyphene
and tramadol. The optimized enrichment procedure involved mixed-mode, strong cation-exchange sorbent in combination with a sequential elution procedure. The extracts were analyzed by reversed-phase
liquid chromatography using a Synergy Polar column coupled to electrospray ionization tandem mass
spectrometry (LC–MS/MS). Accurate quantification of target OAs was achieved using 19 deuterated analogues as surrogate standards. Method accuracies for RW, SE and river water varied in the range from
91 to 126%, 74 to 120% and 75 to 116%, respectively. Careful optimization of the procedure allowed reliable determination of OAs with method quantification limits in the low ng/L range (RW: 0.3-3.5 ng/L;
SE: 0.2-1.9 ng/L, river water: 0.1-0.8 ng/L. The developed method was applied for analysis of RW, SE and
river water samples from Croatia. The concentrations of individual OAs in municipal wastewater varied
in a wide range (from < QL to 859 ng/L) and the most prevalent representatives were tramadol, codeine,
morphine and methadone and their derivatives. Elevated concentrations of morphine glucuronides (up
to 370 ng/L) found in raw municipal wastewater indicated their importance in the overall morphine mass
balance.
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