Data for: Application of the Expert Algorithm for Substance Identification (EASI) to the Electron Ionization (EI) Mass Spectra of Fentanyl Isomers and Analogs

Description

The Excel spreadsheet contains 57,522 mass spectra of 76 different fentanyl analogs. The mass spectra are electron ionization mass spectra (EI-MS) taken at each scan across each GC peak of each replicate injection with no averaging. The spectra include the tails of the GC peaks, which often contain little or no signal from the eluting substance. Such spectra can serve as negative controls or background spectra. The raw counts are provided in centroid/histogram format with 1 Da bins from m/z 40-500. Details are provided in the following publication: A. I. Adeoye, G. P. Jackson, "Application of the Expert Algorithm for Substance Identification (EASI) to the Electron Ionization (EI) Mass Spectra of Fentanyl Isomers and Analogs," Forensic Chem. 2025, 44, 100660. (https://doi.org/10.1016/j.forc.2025.100660)

Steps to reproduce

The reference fentalogs used in this study were the hydrochloride salts provided by Cayman Chemical (Ann Harbor, MI) under a contract from the Center for Disease Control (CDC). The fentalogs arrived in a Fentanyl Analog Screening (FAS) Kit containing analytical reference materials for 150 fentalogs of various substitutions. Standards for Lab 1 were reconstituted in methanol per the FAS kit instructions by adding 500 μL of HPLC grade methanol (Fisher Chemical, Hampton, NH) to each vial, which provided ∼400 μg/mL of the analyte. The final concentration for analyzed standards were between 130 and 200 ppm. Standards for Lab 2 were also purchased from Cayman Chemical and diluted to 1 mg/mL in methanol. Replicate GC/MS spectra were collected for the available fentalogs from two separate laboratories. Lab 1 ran most of the isomers in the study, Lab 2 ran a large subset of the fentalogs, and other labs contributed varying numbers of replicates from their available fentalogs. To provide a more challenging inter-laboratory comparison of spectra, no attempt was made to align the conditions between the two instruments. Lab 1 ran all the reference standards on an Agilent Technologies (Santa Clara, CA) 7890B GC equipped with an Agilent HP-5 column (30 m × 0.25 mm × 0.25 μm film thickness) and an Agilent 5977 A mass spectrometer. The GC/MS parameters were as follows: injection volume was 1 μL; inlet temperature was set to 250 °C; split ratio was 10:1; split flow was 15 mL/min. The initial oven temperature was 50 °C, then ramped to 280 °C at 150C/min and held for 7.7 min. The carrier gas (helium) flow rate was set to 1.5 mL/min. The mass spectrometer scanned from m/z 35–450 after a solvent delay of 2 min. The MS quad and source temperatures were 200 °C and 250 °C, respectively. All spectra from Lab 1 were collected over a 3-month period during which the GC/MS instrument was autotuned before each sequence. Tuning ensured that the air/water levels were below specifications and that the peak ratios for the calibration compound were within the acceptable ranges of the manufacturer's manual. Lab 2 ran fewer reference standards on an Agilent Technologies (Santa Clara, CA) 6890 GC with an Agilent DB-1 column (30 m × 0.25 mm × 0.25 μm film thickness) and an Agilent 5973 N mass spectrometer. The GC parameters were as follows: injection volume was 1 μL; inlet temperature was 280 °C; split ratio was 50:1; split flow was 134.1 mL/min. The initial oven temperature was 80 °C, then ramped to 300 °C at 300C/min and held for 9 min. The carrier gas (helium) flow rate was set to 1.3 mL/min. The mass spectrometer scanned from m/z 40–500 after a solvent delay of 2 min. The MS quad and source temperatures were 150 °C and 230 °C, respectively. All data was collected in two separate 2-month periods over 2 years. The instrument also passed daily autotunes before each set of analyses.

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