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The Use of Gas Chromatography with Tandem Ultra Violet and Mass Spectrometric Detection for the Analysis of Emerging Drugs. Application to Synthetic Cathinones and Fentanyl Analogs.

Award Information

Award #
2017-R2-CX-0028
Location
Status
Closed
Funding First Awarded
2017
Total funding (to date)
$275,221

Description of original award (Fiscal Year 2017, $275,221)

As submitted by the proposer:

The purpose of this project is to investigate the use of gas chromatography with tandem ultraviolet mass spectrometric detection for the analysis of emerging drugs, eg., synthetic cathinones and fentanyl analogs. Emerging drugs, for which there exist many different analogs including positional isomers, are difficult to analyze. Widely-employed gas chromatography­electron in pact mass spectrometry (GC-EI MS) suffers from lack of diagnostic fragment ions and/or molecular ions; and difficulty in distinguishing between positional isomers, especially when substitution occurs on a benzene ring.

Drug quantitation is typically achieved using GC with flame ionization detection with non-deuterated internal standards, for which no qualitative information other than retention time is obtained. Therefore, the possibility exists for erroneous quantitation of target analyte due to co-elution.

The goal of this study is to demonstrate that greatly enhanced analysis of synthetic cathinones and fentanyl homologs and analogs could be accomplished by interfacing a gas chromatograph with a vacuum ultraviolet (VUV) detector and a mass spectrometric detector. The VUV detector, which allows for absorbance in the 120-430 nm range, provides for universal detection and the ability to distinguish between most solutes, including positional isomers. The mass spectrometric detection (cold electron inpact [El]) allows for El spectrum with enhanced molecular and fragment ions. This combination of UV and MS detection would allow for significantly enhanced solute identification as well as well as precise and accurate quantitation without the need for deuterated standards. In addition, VUV detection allows for both qualitative and quantitate analysis of co-eluting peaks.

For this purpose, 22 synthetic cathinones (including five sets of positional isomers) and 15 fentanyl analogs (including six sets of positional isomers) which do not give molecular ions by classical El will be analyzed using the proposed methodology. Following interfacing a GC to both a VUV and MS detector, GC conditions will be developed for the separation of the above solutes. Subsequently for synthetic cathinones and fentanyl analogs classical El spectra, VUV spectra and cold El spectra will be generated. Figures of merit for both qualitative and quantitative analysis will be established including linearity, retention time precision, peak area precision, limits of quantitation, and limits of detection for usable spectral data. For each of the two drug classes, ten samples containing known quantities of adulterants and target analytes will be analyzed using GC-VUV-MS.

Project results will be disseminated by interim and final reports, publications (including journals) and presentations at meetings.

Note: This project contains a research and/or development component, as defined in applicable law, and complies with Part 200 Uniform Requirements - 2 CFR 200.210(a)(14).

ca/ncf

Date Created: September 30, 2017