Chemical Attribution of Fentanyl Using Multivariate Statistical Analysis of Orthogonal Mass Spectral Data

Journal Article · Thu Mar 24 00:00:00 EDT 2016 · Analytical Chemistry

DOI:https://doi.org/10.1021/acs.analchem.5b04434· OSTI ID:1423822

Mayer, Brian P. ^[1]; DeHope, Alan J. ^[2]; Mew, Daniel A. ^[1]; Spackman, Paul E. ^[1]; Williams, Audrey M. ^[1]

---

1. Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States). Forensic Science Center
2. Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States). Materials Science Division

Attribution of the origin of an illicit drug relies on identification of compounds indicative of its clandestine production and is a key component of many modern forensic investigations. Here, the results of these studies can yield detailed information on method of manufacture, starting material source, and final product, all critical forensic evidence. In the present work, chemical attribution signatures (CAS) associated with the synthesis of the analgesic fentanyl, N-(1-phenylethylpiperidin-4-yl)-N-phenylpropanamide, were investigated. Six synthesis methods, all previously published fentanyl synthetic routes or hybrid versions thereof, were studied in an effort to identify and classify route-specific signatures. A total of 160 distinct compounds and inorganic species were identified using gas and liquid chromatographies combined with mass spectrometric methods (gas chromatography/mass spectrometry (GC/MS) and liquid chromatography–tandem mass spectrometry-time of-flight (LC–MS/MS-TOF)) in conjunction with inductively coupled plasma mass spectrometry (ICPMS). The complexity of the resultant data matrix urged the use of multivariate statistical analysis. Using partial least-squares-discriminant analysis (PLS-DA), 87 route-specific CAS were classified and a statistical model capable of predicting the method of fentanyl synthesis was validated and tested against CAS profiles from crude fentanyl products deposited and later extracted from two operationally relevant surfaces: stainless steel and vinyl tile. Finally, this work provides the most detailed fentanyl CAS investigation to date by using orthogonal mass spectral data to identify CAS of forensic significance for illicit drug detection, profiling, and attribution.

• Research Organization: Lawrence Livermore National Laboratory (LLNL), Livermore, CA (United States)
• Sponsoring Organization: USDOE National Nuclear Security Administration (NNSA)
• Grant/Contract Number: AC52-07NA27344
• OSTI ID: 1423822
• Report Number(s): LLNL-JRNL-737521
• Journal Information: Analytical Chemistry, Vol. 88, Issue 8; ISSN 0003-2700
• Publisher: American Chemical Society (ACS)
• Country of Publication: United States
• Language: English

Related Subjects

36 MATERIALS SCIENCE