Development and application of high-throughput sample preparation methods for solid matrices.




Aguilar Lázaro, Lissette.

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This research presents the development and application of high-throughput sample preparation methods for the analysis of organic and inorganic contaminants from solid samples. The approach presented evaluates conventional methods to identify potential areas of improvement. In this sense, conventional methods serve as a framework for the development of high-throughput sample preparation methods. In general, improvements include expansion of target analyte list thereby increase the environmental applicability, reduction of sample preparation steps, and as a result, reduction of sample preparation time. The analytical bottleneck is often associated with sample preparation, especially in the analysis of organic contaminants from environmental samples. Many environmental analytical chemistry methods can be broken down into one or more sample preparation steps followed by one or more chemical analysis steps. Improvement of historical methods has focused on the development of advance instrumentation (i.e. focusing on the chemical analysis). However, recent efforts have focused on the overall reduction of time and/or steps associated with sample preparation. For example, post-extraction cleanup adsorbents can be incorporated into the pressurized liquid extraction step to perform a selective pressurized liquid extraction (SPLE). SPLE methods significantly reduced sample preparation time, solvent requirements, and waste production. Specific examples presented in this dissertation include: 1) the development and application of SPLE methods for the analysis of organic contaminants from sediments and biological tissues; 2) the development and application of a simplified acid digestion method for the analysis of mercury and selenium in rare samples of Pacific walrus (Odobenus rosmarus divergens) muscle (L. dorsi). These examples illustrate the approach for the development of high-throughput sample preparation methods that have successfully combined techniques into a single method, and/or eliminated post-extraction cleanup steps. The availability of these methods increases laboratory’s capacity and preparedness to analyze rapidly large volumes of samples. These methods could find use in routine analysis and monitoring studies of environmental samples, food and pharmaceutical industries, agriculture, toxicology studies, and forensic sciences among others. Lastly, this dissertation discusses a few opportunities that lay ahead for improvement and development in sample preparation.



Selective pressurized liquid extraction., High-throughput sample preparation., Dioxins and furans., Superfund site., Walrus., Mercury., Arctic marine mammals., Sediment., PCBs.


Aguilar, Lissette, Williams, E. Spencer, Brooks, Bryan W., Usenko, Sascha. "Development and application of a novel method for high-throughput determination of PCDD/Fs and PCBs in sediments." Environmental toxicology and chemistry 33, 7 (2014): 1529-1536.
Oziolor, Elias M., Bigorgne, Emilie, Aguilar, Lissette, Usenko, Sascha, Matson, Cole W. "Evolved resistance to PCB- and PAH-induced cardiac teratogenesis, and reduced CYP1A activity in Gulf killifish (Fundulus grandis) populations from the Houston ship channel, Texas." Aquatic toxicology 150 (2014): 210-219.
Usenko, Sascha, Subedi, Bikram, Aguilar, Lissette, Robinson, Eleanor M. "High-throughput analysis of PCDD/Fs, and PCBs in biological matrices using GC–MS/MS." Advanced techniques in gas chromatography-mass spectrometry (GC-MS-MS and GC-TOF-MS) for environmental chemistry 61 (2013): 143-158.
Subedi, Bikram, Aguilar, Lissette, Williams, E. Spencer, Brooks, Bryan W., Usenko, S. "Selective pressurized liquid extraction technique capable of analyzing dioxins, furans, and PCBs in clams and crab tissue." Bulletin of environmental contamination and toxicology 92 (2014): 460-465.