The reliable identification of fentanyl and its analogs is of great significance for public security. However, with the growing prevalence of fentanyl compounds, current analytical strategies cannot fully meet the need for fast and high-throughput detection. In this study, a simple, rapid, and on-site analytical protocol was developed based on a miniature mass spectrometer. A dramatically simplified workflow was implemented using matrixassisted ionization, bypassing complex sample pretreatment and chromatographic separation. The tandem mass spectrometry (MS/ MS) capability afforded by the miniature ion trap mass spectrometer facilitated the investigation of fragmentation patterns for 49 fentanyl analogs during collision-induced dissociation, revealing valuable information on marker fragment ions and characteristic neutral loss. Calculations on Laplacian bond order values further verified the mass spectrometric behavior. A computation-assisted expandable mass spectral library was constructed in-house for fentanyl compounds. Smart suspect screening was carried out based on the full-scan MS and MS/MS data. The present study demonstrates an appealing potential for forensic applications, enabling streamlined screening for the presence of illicit fentanyl compounds at the point of seizures of suspect samples.
Green analytical chemistry aims at
developing analytical methods
with minimum use and generation of hazardous substances for the protection
of human health and the environment. To address this need, a green
analytical protocol has been developed for the analysis of anionic
compounds integrating electromembrane extraction (EME), dual-channel
nanoelectrospray ionization (nanoESI), and a miniature mass spectrometer.
Haloacetic acids (HAAs) have attracted considerable public concern
due to their adverse effects on human health and were selected as
model analytes for method development. A flat membrane EME device
was developed and assembled in-house. Optimization of fundamental
operational parameters was performed using single-factor test and
response surface methodology. Both the EME acceptor phase and an imidazolium-based
dicationic ionic liquid (DIL), 1,1-bis(3-methylimidazolium-1-yl) butylene
difluoride (C4(MIM)2F2), were subjected
to dual-channel nanoESI and miniature mass spectrometry analysis based
on a charge inversion strategy, where positively charged complexes
were formed. Enhancement in signal intensity by as much as 2 magnitudes
was achieved in the positive-ion mode compared to the negative-ion
mode in the absence of the dicationic ion-pairing agent. The developed
protocol was validated, obtaining good recoveries ranging from 82.7
to 109.9% and satisfactory sensitivity with limits of detection (LODs)
and quantitation (LOQs) in the ranges of 1–5 and 2–10
μg/L, respectively. The greenness of the analytical procedure
was assessed with a calculated score of 0.71, indicating a high degree
of greenness. The developed method was applied to the analysis of
real environmental or municipal water samples (n =
16), exhibiting appealing potential for outside-the-laboratory applications.
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