Investigation of Ionic Liquid Phases for Chromatographic Separation of Fentanyl Analogues

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Opioid abuse and in particular fentanyl, a synthetic opioid, has been of concern in the last decade. Fentanyl is an illicit drug of concern to due to its prevalence and potency. Research to date has focused on supporting law enforcement by developing methods suitable for chemical profiling and identifying fentanyl from various matrices. However, methods geared towards analysis of fentanyl isomeric analogues are rare. Analysis of isomers is challenging due to similar mass spectral fragmentation patterns and exhibiting co-elution using common gas chromatographic columns. Developing methods to use in forensic labs utilizing already available equipment will advance current capabilities in … continued below

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Smart, Katherine Rose December 2022.

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This dissertation is part of the collection entitled: UNT Theses and Dissertations and was provided by the UNT Libraries to the UNT Digital Library, a digital repository hosted by the UNT Libraries. It has been viewed 32 times. More information about this dissertation can be viewed below.

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  • Smart, Katherine Rose

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Opioid abuse and in particular fentanyl, a synthetic opioid, has been of concern in the last decade. Fentanyl is an illicit drug of concern to due to its prevalence and potency. Research to date has focused on supporting law enforcement by developing methods suitable for chemical profiling and identifying fentanyl from various matrices. However, methods geared towards analysis of fentanyl isomeric analogues are rare. Analysis of isomers is challenging due to similar mass spectral fragmentation patterns and exhibiting co-elution using common gas chromatographic columns. Developing methods to use in forensic labs utilizing already available equipment will advance current capabilities in the detection of fentanyl compounds. Thus, investigation into alternative stationary phases and development of special gas-liquid chromatographic (GLC) based methods for isomeric fentanyl analogues has been done. Several studies were done to investigate the use of ionic liquid chromatographic phases in analyzing fentanyl analogues. The first study focused on investigating the thermal stability of ionic liquids to identify those suitable to withstand the high oven temperatures that was needed to elute fentanyl analogues in gas chromatography. Total synchronous fluorescence spectroscopy and differential scanning calorimetry were demonstrated to be sensitive enough to detect the decomposition products of ionic liquids. In the second study, gas chromatographic analysis was done on fentanyl analogues using an ionic liquid stationary phase as well as two commonly used stationary phases for comparison purposes. The applicability of the developed methods was tested using standard fentanyl analogue samples as well as in-house synthesized samples on all three columns. In the third study, quantitative structure property relationship equations were developed to predict the retention time of fentanyl analogues on two of the gas chromatographic stationary phases used in the second study.

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  • December 2022

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  • Feb. 9, 2023, 5:19 p.m.

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  • Jan. 30, 2025, 3:42 p.m.

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Smart, Katherine Rose. Investigation of Ionic Liquid Phases for Chromatographic Separation of Fentanyl Analogues, dissertation, December 2022; Denton, Texas. (https://digital.library.unt.edu/ark:/67531/metadc2048656/: accessed April 30, 2025), University of North Texas Libraries, UNT Digital Library, https://digital.library.unt.edu; .

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