Simultaneous analysis of opioid analgesics and their metabolites in municipal wastewaters and river water by liquid chromatography–tandem mass spectrometry
•LC–MS/MS method for the determination of 27 opioid analgesics was developed.•Keeping SPE catridges at −20 °C was the best way to ensure stability of opioids.•Opioid analgesics are common constituents of municipal wastewater and river water.•Metabolites of opioids contributed significantly to the ov...
Saved in:
| Published in: | Journal of Chromatography A 2018-01, Vol.1533, p.102-111 |
|---|---|
| Main Authors: | , , , |
| Format: | Article |
| Language: | eng |
| Subjects: | |
| Online Access: | Get full text |
| Tags: |
Add Tag
No Tags, Be the first to tag this record!
|
| Summary: | •LC–MS/MS method for the determination of 27 opioid analgesics was developed.•Keeping SPE catridges at −20 °C was the best way to ensure stability of opioids.•Opioid analgesics are common constituents of municipal wastewater and river water.•Metabolites of opioids contributed significantly to the overall mass balance.•Conjugated opioids may represent a significant percentage of the total concentration.
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 |
|---|---|
| ISSN: | 0021-9673 |