Two-dimensional nuclear magnetic resonance (2D NMR) spectroscopy was evaluated for the identification and quantification of compounds in an unknown street drug sample. Using 2D COSY and HSQC techniques, heroin was successfully quantified, and the presence of 6-monoacetylmorphine (6-MAM), xylazine, and caffeine was confirmed through partial structural elucidation. These methods demonstrated the ability to differentiate structurally similar opioid analogues without reliance on reference library databases. While gas chromatography–mass spectrometry (GC–MS) remains the standard in forensic laboratories, it has limitations in de novo structural analysis and in detecting emerging analogues absent from spectral libraries. In this study, heroin and fentanyl were quantified in both simulated and actual street samples at concentrations ranging from 0.97 to 1.80 mg/mL, with errors between 0% and 34% using a 400 MHz NMR instrument. A benchtop 60 MHz NMR system also detected and quantified 56 mg/mL of heroin with a 24% error in a simulated sample. These findings support the complementary role of 2D NMR spectroscopy in forensic drug analysis in light of the opioid epidemic and the evolving drug market.
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Differentiation and identification of fentanyl analogues using GC-IRD
Fentanyl analogues and their positional isomers have similar chemical structural configurations making them difficult to identify and differentiate. Gas chromatography coupled to a gas-phase infrared detector (GC-IRD) is a useful and powerful tool for the unambiguous identification of fentanyl compounds where traditional analytical techniques such as gas chromatography–mass spectrometry (GC–MS) offer limited information for this class of compounds. In this study, we demonstrate the utility of GC-IRD and show how this complementary information enables the identification of fentanyl analogues (2- and 3- furanylfentanyl, 2-furanylbenzylfentanyl, croto- nylfentanyl, cyclopropylfentanyl, methoxyacetylfentanyl, carfentanil, meta-fluoroisobutyryl fentanyl, para- fluoroisobutyryl fentanyl and ortho-fluoroisobutyryl fentanyl) when combined with GC–MS data. A description of the operating conditions including how the optimization of GC-IRD parameters can enhance the spectral resolution and unambiguous identification of these fentanyl analogues is presented, for the first time. In par- ticular, the effects of light pipe temperatures, acquisition resolution, the use of a programmed temperature vaporizing (PTV) inlet, and the analytical concentration of the sample were evaluated. A real-world case ex- ncountered in casework and how the implementation of GC- of these challenges in fentanyl differentiation and identification.
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- Award ID(s):
- 1739805
- PAR ID:
- 10166494
- Date Published:
- Journal Name:
- Forensic chemistry
- Volume:
- 20
- ISSN:
- 2468-1709
- Page Range / eLocation ID:
- 100255
- Format(s):
- Medium: X
- Sponsoring Org:
- National Science Foundation
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