Browsing by Author "Davis, Kymeri Elizabeth"

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    Detection of Illicit Drugs in Various Matrices Via Total Vaporization Solid-Phase Microextraction
    (2019-08) Davis, Kymeri Elizabeth; Goodpaster, John; Manicke, Nicholas; Deiss, Frédérique
    In Headspace Solid-Phase Microextraction (Headspace SPME), a sample is heated to encourage a portion of the analyte into the headspace of a vial. A coated fiber is introduced into the sample headspace and the analyte is adsorbed onto the fiber coating. Total Vaporization Solid-Phase Microextraction (TV-SPME) is a technique that is derived from this technique. In TV-SPME, liquid samples are completely vaporized allowing for better adsorption and fewer matrix effects. This method does not require any sample preparation, utilizes minimal supplies and can be automated, making it both an efficient and cost-effective method. Chapter 1 will discuss the theory of SPME and TV-SPME. In Chapter 2, the detection of ɣ-hydroxybutyric acid (GHB) and ɣ-butyrolactone (GBL) in beverages is discussed. The detection of these compounds in beverages is of importance because these drugs may be used to facilitate sexual assault. This crime utilizes substances that cause sedation and memory loss. The derivatization of GHB as well as the properties that make GHB difficult to detect will be discussed. Chapter 3 will discuss the detection of methamphetamine and amphetamine (as their trifluoroacetyl derivatives), GBL, and the trimethylsilyl derivative of GHB in human urine. Amphetamine is a metabolite of methamphetamine, therefore, both drugs should be identified within biological samples. GHB and GBL are metabolites of one another and interconvert when in aqueous solution. This interconversion will be discussed. Chapter 4 will cover method optimization of the Total Vaporization Solid-Phase Microextraction method. Analytes of interest for these analyses were methamphetamine, amphetamine, GHB, and GBL. The optimal extraction temperature ranging from 60-160°C of each drug will be discussed as well as why higher temperatures may not be suitable for this method. A limit of detection study for methamphetamine and amphetamine will also be covered. Chapter 5, the future work chapter, will discuss future analyses using the Total Vaporization Solid-Phase Microextraction method including the analysis of powder materials, plant material, and toxicological samples. Powder material will include the analysis of individual powdered drugs as well as realistic drug mixtures. Some analyses on individual powder samples has already been completed and will be shown. Plant material will include the analysis of naturally occurring compounds found in marijuana plants as well as synthetic cannabinoids. Toxicological samples will expand on previously mentioned urine samples to include drugs such as benzoylecgonine and THC-COOH.
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    Solid-Phase Microextraction of Volatile Organic Compounds for Analytical and Forensic Applications
    (2023-12) Davis, Kymeri Elizabeth; Goodpaster, John; Frédérique, Deiss; Nicholas , Manicke; Sébastien , Laulhé
    Gas chromatography-mass spectrometry (GC-MS) is a frequently used technique in forensic chemistry for the identification of controlled substances and explosives. GC-MS can be coupled with solid-phase microextraction (SPME), in which a fiber with a sorptive coating is placed into the headspace above a sample or directly immersed in a liquid sample. Analytes are adsorbed onto the fiber which is then placed inside the heated GC inlet for desorption. Illicit drugs are often found in the form of impure solids, mixed with other drugs, adulterants, and diluents. A simple method for the quick identification of drugs including methamphetamine, cocaine, heroin, fentanyl, and pharmaceutical tablets was developed. Headspace SPME methods were utilized with an elevated extraction temperature for the detection of various drugs in powder and tablet form. An extraction temperature of 120oC was used to encourage analytes into the headspace of the vial. A sample of the solid drug was placed in a headspace vial with no prior sample preparation or clean-up. This vial was then heated inside of an agitator where the sample was extracted. It was found that drugs in solid and tablet form can be detected using this high temperature headspace SPME method at the temperature of 120oC with no prior sample preparation. This method is simple, efficient, and cost effective for the detection of legal and illicit drugs in solid form. Headspace SPME may also be used for the analysis of explosive materials. Canines trained at detecting hidden explosives should be trained using real explosive materials that have minimal contamination by other explosive odors to ensure accurate identification of potential threats. Therefore, the potential for cross-contamination between training aids is of importance. There are various storage methods in use by canine handlers such as plastic and cloth bags, but these can lead to cross-contamination between training aids during storage. Alternatively, odor-permeable membrane devices (OPMDs) may store training aides and be used as a delivery device. A membrane in the OPMD allows for volatile compounds from the training aids to be released during training while helping to prevent contaminants from entering the device. OPMDs were used in addition to traditional storage containers to monitor the contamination and degradation of 14 explosives used as canine training aids. Samples included explosives that contain highly volatile compounds like dynamite and explosives with less volatile compounds like RDX. Explosives were stored individually using traditional storage bags or inside of an OPMD at two locations, IUPUI and an Indianapolis Metropolitan Police Department. The police department actively used the training aids during canine trainings. Samples from each storage type at both locations were collected at 0, 3, 6, and 9 months and analyzed using Fourier transform infrared (FTIR) spectroscopy and GC-MS with SPME. FTIR analyses showed no signs of degradation of the training aids from any timepoint or location. GC-MS identified cross-contamination from ethylene glycol dinitrate and/or 2,3-dimethyl-2,3-dinitrobutane across almost all samples regardless of storage condition. The contamination was found to be higher among training aids that were stored in traditional ways and were in active use by canine teams. Additionally, Time 0 had the highest level of contamination, indicating that explosive training aids are received from the vendors with initial cross-contamination. To test the initial cross-contamination levels of training aids, 11 explosive materials were ordered from three different vendors. A 1-gram sample of each was collected and analyzed using SPME with GC-MS. In several cases, explosive materials that are commercially available already exhibit elevated levels of contamination. This indicates that training aids must be acquiring contamination during manufacturing and/or storage at the vendor facility. The cross-contamination of explosive canine training aids stored in OPMDs was further evaluated and compared to traditional storage methods. This was done by storing various combinations of storage containers such as cloth bags, velcro bags, and OPMDs along with explosives and using activated charcoal strips to collect the volatile compounds such as 2,3-dimethyl-2,3-dinitrobutane and ethylene glycol dinitrate. Only one type of storage container, a velcro bag, showed evidence of contamination, indicating that OPMDs may not further prevent cross-contamination of explosive training aids.