Bioanalytical applications of matrix compatible Solid Phase Microextraction

Janusz Pawliszyn, Chemistry, University of Waterloo, Waterloo, Canada (Janusz@uwaterloo.ca)

Development of matrix compatible coatings for solid-phase microextraction (BioSPME) has enabled direct immersion microextraction of small molecules from complex matrices, including body fluids and even live tissues. Such coating consists of appropriate sorbent particles, such as HLB phases dispersed in a biocompatible binder, such PAN forming well defined wettable porous structure. The direct immersion mode of BioSPME when utilized in conjunction with such morphology extraction phases facilitates clean extraction of a wide range of analytes from complex matrices without the occurrence of fouling or coating saturation as well as elimination of matrix effects when combined with LC/MS.  Such “chemical biopsy” process isolates only small molecules from the matrix followed by introduction to the instrument clean mixtures containing target analytes without any sample matrix.

SPME workflows for automated high throughput diverse bioanalytical applications of body fluids based on 96 well plate using coated-blade format combined with LC/MS will be described.  It has been demonstrated that the approach meets the required LODs.  The clean extraction property of this approach led to diverse BioSPME-MS strategiesresulting in fast and simple determination of target compounds in diverse matrices. These technologies include Coated Blade Spray (CBS) and SPME- open-port probe (SPME-OPP). Unlike direct-sample-to-MS approaches, BioSPME-MS provides a cleaner extract which allows for long-term operation of the instrument with minimal maintenance and reliable quantification. Sampling/sample-preparation is performed either by spotting the sample onto the SPME-device, or by immersing the SPME-device on a vial containing the sample. Despite short extraction times, limits of quantitation ranging between low-pg/mL to sub-ng/mL were obtained, while good accuracy, and linearity were attained.

Important bioanalytical applications of BioSPME include in vivo investigations. In particular, tissue analysis remains the bottleneck of such studies due to the invasiveness of presently used sample collection based on biopsy, as well as the laborious and time-consuming sample preparation protocols. In the proposed BioSPME technology, the flexible metal acupuncture size needle containing recess is coated with the coating having morphology described above.  In this approach, only molecules of interests are extracted onto biocompatible sorbent from the investigated system, however no tissue is not removed.  Therefore, the direct coupling of the “chemical biopsy” probe to mass spectrometry is feasible as well.  Such hyphenation facilitates rapid quantification of the compounds of interests resulting in possibility of close to real time monitoring.  This approach has potential in biological and clinical on-site investigations including bedside medical diagnosis.

Anal. Chem. 2018, 90, 302−360

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Abstract Reference & Short Personal Biography of Presenting Author

The primary focus of Professor Pawliszyn's research program is the design of highly automated and integrated instrumentation for the isolation of analytes from complex matrices and the subsequent separation, identification and determination of these species.  The primary separation tools used by his group are Gas Chromatography, Liquid Chromatography and Capillary Electrophoresis coupled to variety of detections systems, including range of mass spectrometry techniques. Currently his research is focusing on elimination of organic solvents from the sample preparation step to facilitate on-site monitoring and in-vivo analysis.  Several alternative techniques to solvent extraction are investigated including use of coated fibers, packed needles, membranes and supercritical fluids.  Dr. Pawliszyn is exploring application of the computational and modeling techniques to enhance performance of sample preparation, chromatographic separations and detection.  The major area of his interest involves the development and application of imaging detection techniques for microcolumn chromatography, capillary electrophoresis and micro chip separation devices. 

Professor Pawliszyn Hirsch Index (H-index) is 91.  He is a Fellow of Royal Society of Canada and editor of Analytica Chimica Acta, Trends in Analytical Chemistry.  He initiated a conference, “ExTech”, focusing on new advances in sample preparation and disseminates new scientific developments in the area, which meets every year in different part of the world.  He received the 1995 McBryde Medal, the 1996 Tswett Medal, the 1996 Hyphenated Techniques in Chromatography Award, the 1996 Caledon Award, the Jubilee Medal 1998 from the Chromatographic Society, U.K., the 2000 Maxxam Award from Canadian Society for Chemistry, the 2000 Varian Lecture Award from Carleton University, the Alumni Achievement Award for 2000 from Southern Illinois University, the Humboldt Research Award for 2001, 2002 COLACRO Medal, in 2008 he received A.A. Benedetti-Pichler Award from Eastern Analytical Symposium, 2008 Andrzej Waksmundzki Medal from Polish Academy of Sciences, 2008 Manning Principal Award, 2010 Torbern Bergman Medal from the Swedish Chemical Society, 2010 Ontario Premier’s Innovation Award,2010 Marcel Golay Award, 2010 ACS Award in Separation Science and Technology, 2011 PittCon Dal Nogare Award, 2012 E.W.R. Steacie Award, 2013 CIC Environmental Research and Development Award, 2013 CICLeSueurMemorial Award, 2015 Maria Skłodowska-Curie Medal from Polish Chemical Society, 2015 Halász Medal Award from the Hungarian Society for Separation Sciences, 2017 Pittsburgh Conference Analytical Chemistry Award,  the 2017 Eastern Analytical Symposium Award for Outstanding Achievements in the Fields of Analytical Chemistry, 2018 ACS Award in Chromatography, 2018 North American Chemical Residue Workshop Excellence Award and 2019 Talanta medal.