Objective: To establish a magnetic solid-phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (MSPE-UHPLC-MS/MS) method for rapidly detecting 14 fentanyl analogs in wastewater. Methods: Wastewater samples were purified and concentrated using a novel mixed-mode weak cation exchange magnetic solid phase extraction adsorbent, Fe3O4@poly (ST/DVB/MA-COOH), followed by analysis with UHPLC-MS/MS method. Separation was performed on a Waters Acquity UPLC HSS T3 column (150 mm×2.1 mm, 1.8 μm)at 40 ℃. The mobile phase consisted of 0.1% formic acid-aqueous solution(A) and 0.1% formic acid-acetonitrile solution(B) with gradient elution. The flow rate was 0.3 mL · min-1, and an injection volume was 2.5 µL. Detection was carried out using electrospray ionization in multiple reaction monitoring mode. Results: The calibration curves for the 14 fentanyl analogs showed good linearity over the range of 0.04-4 ng · L-1 (r≥0.998 4). The limit of detection (LOD) was 0.013 ng · L-1 and the limit of quantitation (LOQ) was 0.04 ng · L-1. The recovery rates at low, medium and high spiked levels ranged from 85.4% to 114.7%. The intra-day precision(n=6) was between 2.0% and 6.4%, and the inter-day precision(n=3) was between 0.4% and 2.4%. Fentanyl was detected in five actual wastewater samples, with concentrations ranging from 0.21 to 0.46 ng · L-1. Conclusion: This method has the advantages of short pretreatment time, simple operation, low solvent consumption, high sensitivity, and good reproducibility. It is suitable for high-throughput screening and quantitative analysis of fentanyl analogs in wastewater samples.
DONG Luo-hao
,
LIU Meng
,
ZHOU Jing
,
WANG Hai-xing
,
ZHOU Kai
,
KE Xing
,
FAN Yi-lei
. Determination of 14 fentanyl analogs in wastewater by magnetic solid phase extraction combined with ultra performance liquid chromatography-tandem mass spectrometry*[J]. Chinese Journal of Pharmaceutical Analysis, 2025
, 45(7)
: 1221
-1232
.
DOI: 10.16155/j.0254-1793.2024-1139
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