Detection and confirmation of fentanyls in high clay‐content soil by electron ionization gas chromatography‐mass spectrometry

Journal Article · Fri Aug 11 00:00:00 EDT 2023 · Journal of Forensic Sciences

DOI:https://doi.org/10.1111/1556-4029.15354· OSTI ID:1994880

Valdez, Carlos A.  ^[1]; Rosales, José A. ^[2]; Vu, Alexander K. ^[1]; Leif, Roald N. ^[1]

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1. Global Security Directorate Lawrence Livemore National Laboratory Livermore California USA, Physical and Life Sciences Directorate Lawrence Livemore National Laboratory Livermore California USA, Nuclear and Chemical Sciences Division Lawrence Livemore National Laboratory Livermore California USA, Forensic Science Center Lawrence Livemore National Laboratory Livermore California USA
2. Global Security Directorate Lawrence Livemore National Laboratory Livermore California USA, Nuclear and Chemical Sciences Division Lawrence Livemore National Laboratory Livermore California USA, Forensic Science Center Lawrence Livemore National Laboratory Livermore California USA, NNSA‐MSIIP Summer Fellow University of Texas El Paso Texas USA

Abstract Detection of illicit drugs in the environment, particularly in soils, often suggests the present or past location of a clandestine production center for these substances. Thus, development of efficient methods for the analysis and detection of these chemicals is of paramount importance in the field of chemical forensics. In this work, a method involving the extraction and retrospective confirmation of fentanyl, acetylfentanyl, thiofentanyl, and acetylthiofentanyl using trichloroethoxycarbonylation chemistry in a high clay‐content soil is presented. The soil was spiked separately with each fentanyl at two concentrations (1 and 10 μg/g) and their extraction accomplished using ethyl acetate and aqueous NH ₄ OH (pH ~ 11.4) with extraction recoveries ranging from ~56% to 82% for the high‐concentration (10 μg/g) samples while ranging from ~68% to 83% for the low‐concentration (1 μg/g) samples. After their extraction, residues containing each fentanyl were reacted with 2,2,2‐trichloroethoxycarbonyl chloride (Troc‐Cl) to generate two unique and predictable products from each opioid that can be used to retrospectively confirm their presence and identity using EI‐GC‐MS. The method's limit of detection (MDL/LOD) for Troc‐norfentanyl and Troc‐noracetylfentanyl were estimated to be 29.4 and 31.8 ng/mL in the organic extracts. In addition, the method's limit of quantitation for Troc‐norfentanyl and Troc‐noracetylfentanyl were determined to be 88.2 and 95.5 ng/mL, respectively. Collectively, the results presented herein strengthen the use of chloroformate chemistry as an additional chemical tool to confirm the presence of these highly toxic and lethal substances in the environment.

• Sponsoring Organization: USDOE
• OSTI ID: 1994880
• Journal Information: Journal of Forensic Sciences, Journal Name: Journal of Forensic Sciences; ISSN 0022-1198
• Publisher: Wiley-Blackwell
• Country of Publication: United States
• Language: English