Document Type



Doctor of Philosophy (PhD)



First Advisor's Name

Anthony DeCaprio

First Advisor's Committee Title

Committee Chair

Second Advisor's Name

Piero Gardinali

Second Advisor's Committee Title

Committee Member

Third Advisor's Name

Bruce McCord

Third Advisor's Committee Title

Committee Member

Fourth Advisor's Name

DeEtta Mills

Fourth Advisor's Committee Title

Committee Member

Fifth Advisor's Name

Stanislaw Wnuk

Fifth Advisor's Committee Title

Committee Member


Novel Psychoactive Substances, LC-QTOF-MS

Date of Defense



There has been an emergence of novel psychoactive substances (NPS) in forensic casework globally. Although the reported prevalence of these compounds has been relatively low in comparison to traditional drugs of abuse, published case studies suggest that some NPS have significant pharmacological effects that may cause severe impairment and/or death. Because of these effects, it is important that toxicology laboratories have the capability of identifying these compounds to complete a comprehensive toxicological analysis for human performance and post-mortem investigations.

Recently, mass spectrometry has gained favor over traditional screening assays such as immunoassays for the identification of NPS in biological specimens. This trend is mainly a result of the fact that mass spectrometry provides the required sensitivity and selectivity for a broader range of analytes. High resolution tandem mass spectrometry has been suggested for analysis of NPS, as this technique further increases selectivity by increasing mass accuracy and providing MS/MS spectral data. The main goal of the present study was to investigate the applicability of using high resolution mass spectrometry to screen for and confirm a large number of novel psychoactive substances. The present study consisted of three main tasks, which included 1) the creation of a large high resolution MS/MS spectral library and database, 2) the development of a solid phase extraction (SPE) method and acquisition methods, and 3) a collision induced dissociation (CID) study of regioisomeric NPS compounds.

The MS/MS spectral library created contains spectral data for 252 NPS. In addition, 875 NPS entities were included in the compound database. The library and database can be used by toxicology laboratories to aid in the identification of NPS in casework using MS/MS spectral data and full scan MS data, respectively. The analytical method developed used SPE and high resolution mass spectrometry (HRMS). The HRMS method demonstrated limits of detection ranging from 0.5- 5 ng/mL for NPS from various structural drug classes. The CID experiments demonstrated that relative ion abundance alone could be used to differentiate some sets of regioisomers. The present work can aid toxicology laboratories in the identification of NPS and demonstrates the applicability of HRMS for their screening and confirmation.



Included in

Chemistry Commons



Rights Statement

Rights Statement

In Copyright. URI:
This Item is protected by copyright and/or related rights. You are free to use this Item in any way that is permitted by the copyright and related rights legislation that applies to your use. For other uses you need to obtain permission from the rights-holder(s).