Structural Characterization of Nitazene Analogs by Mass Spectrometric Methods

Description

This dataset includes Excel spreadsheets with the raw data from four studies that were completed as part of a National Institute of Standards and Technology (NIST), United States Department of Commerce (DOC), Measurement Science and Engineering (MSE) research grant (Award No. 60NANB23D092). The data were derived from the following studies: 1) electron ionization-mass spectrometry (EI-MS) characterization of 43 nitazene analogs, 2) electrospray ionization tandem mass spectrometry (ESI-MS/MS) characterization of 43 nitazene analogs, 3) a comparison of all ions fragmentation (AIF), in-source collision-induced dissociation (IS-CID), and collision-induced dissociation (CID) activation for 18 nitazene analogs analyzed with direct analysis in real time mass spectrometry (DART-MS), and 4) the characterization of oxygenated species for 18 nitazene analogs observed with DART-MS with both helium and nitrogen source gases. This data can be used for building EI, ESI, or DART mass spectral libraries and/tools for nitazene analog identification, to perform comparisons of query EI, ESI, or DART mass spectra, or be further analyzed to gain new insights into the mass spectral behavior of nitazene analogs.

Steps to reproduce

Conditions for data acquisition are provided in the corresponding publications: 1) E. K. Hardwick, J. T. Davidson. Structural characterization of nitazene analogs using electron ionization-mass spectrometry (10.1016/j.forc.2024.100605); 2) E. K. Hardwick, J. T. Davidson. Structural Characterization of Nitazene Analogs Using Electrospray Ionization–Tandem Mass Spectrometry (10.1002/dta.3921); 3) E. K. Hardwick, A. N. Couch, J. T. Davidson. Comparison of Activation Techniques for the Identification of Nitazene Analogs Using the NIST/NIJ Data Interpretation Tool (10.1002/rcm.70004) and 4) E. K. Hardwick, A. N. Couch, J. T. Davidson. Addressing the Oxygen in the Room: Exploring the Formation of Oxygenated Species for Nitazene Analogs Using DART-MS (10.1021/jasms.6c00059). An 8890 GC-5977B GC-MS was operated with a 30 m × 0.250 mm × 0.25 µm HP-5MS column using an ultra-pure helium carrier gas with a 1.5 mL/min flow rate. The inlet temperature was 250 ℃, the injection volume was 1 µL, and the split ratio was 10:1. The oven temperature began at 150 ℃ for 1 min, and was followed by a ramp of 20 ℃/min to 250 ℃ which was held for 1 min. This was followed by a ramp of 5 ℃/min to 300 ℃, with a hold time of 15 min. The mass spectrometer used a 70-eV ionization energy with a source temperature of 230 ℃ and a quadrupole temperature of 150 ℃. The scan range of m/z 50-500 began after a 2 min solvent delay. An Agilent Technologies 6530 Q-TOF mass spectrometer was used for the direct injection studies. Samples were directly infused into the source using an 18 µL/min flow rate. The source was operated in positive ionization mode with a 300 °C drying gas and a 350 °C sheath gas, both with a flow rate of 8 L/min. Nitrogen for the ESI source was generated with a Genius 3040 nitrogen generator. The nebulizer pressure was 40 psi, the capillary voltage was 3500 V, and the nozzle voltage was 1500 V. The fragmentor voltage was 150 V and the skimmer voltage was 65 V. MS/MS studies were conducted with collision-induced dissociation (CID) activation energies of 15, 25, 35, and 45-eV. A 1 Da isolation width was used for all analyses, with a 250 ms/spectrum acquisition time for approximately 30 s per activation condition. The scan range for all samples was m/z 40-500. A DART JumpShot® ionization source was coupled to an Agilent Technologies 6530 Q-TOF for the DART studies. 5 µL of sample was deposited onto the closed end of a glass capillary for analysis. The DART source was operated in positive ionization mode, using either helium nitrogen as the source gas and a source temperature of 350 °C. The grid electrode was set to 350 V. The fragmentor voltage was 150 V and the skimmer voltage was 65 V. For CID, 15, 25, and 35 eV were the collision energies chosen; IS-CID utilized different fragmentor voltages at 150, 250, and 350 V; and AIF utilized 0, 30, and 60 eV as the low, medium, and high collision energies. The scan range for all activation techniques was m/z 40-450.

Institutions

• Sam Houston State University

  Texas, Huntsville

Categories

Funders

• National Institute of Standards and Technology

  United States Department of Commerce

  Gaithersburg

  Grant ID: 60NANB23D092

Licence