Previously, we showed how to make and use stable zirconia RPLC media, introducing two new techniques, thermally tuned tandem column (T3C) chromatography and high temperature ultra-fast liquid chromatography (HTUFLC). We now propose to make and characterize a number of innovative highly stable silica (SiO2) phases that will use hypercrosslinked surface polymer networks confined to a monolayer on the silica surface. We will then apply these materials to the high-speed analysis of pharmaceuticals, environmental and workplace toxicants, and ultimately, in collaboration with Professor David Muddiman, to complex biological samples. Our goal is to explore all aspects of the new derivatization technology, including conventional LC, packed capillary LC and capillary electrochromatography. We will explore two general concepts in HPLC made possible by the availability of high stability phases. First, we propose to develop fast, comprehensive two-dimensional HPLC (2D-LC) based on our phases. Due to the thermal limitations of conventional supports, the advantages of using high temperatures in HPLC have hardly been explored. In particular, upon increasing the temperature to 200 degrees C, the resulting 20-fold decrease in viscosity gives a nearly 20-fold increase in analysis speed. We will use the high speed of HTUFLC to increase the speed of 2D-LC and make it a much more practical routine method. The use of higher temperatures also facilitates the use of longer columns, especially in a capillary format, particularly for microdetection. Second, we propose to extend the isocratic T3C concept to gradient elution chromatography. Both approaches are predicated on the availability of phases of high thermal stability.

Agency
National Institute of Health (NIH)
Institute
National Institute of General Medical Sciences (NIGMS)
Type
Research Project (R01)
Project #
5R01GM054585-11
Application #
7217557
Study Section
Special Emphasis Panel (ZRG1-BECM (01))
Program Officer
Edmonds, Charles G
Project Start
1996-08-01
Project End
2008-09-21
Budget Start
2007-04-01
Budget End
2008-09-21
Support Year
11
Fiscal Year
2007
Total Cost
$248,756
Indirect Cost
Name
University of Minnesota Twin Cities
Department
Chemistry
Type
Schools of Arts and Sciences
DUNS #
555917996
City
Minneapolis
State
MN
Country
United States
Zip Code
55455
Haidar Ahmad, Imad A; Soliven, Arianne; Allen, Robert C et al. (2015) Comparison of core-shell particles and sub-2?m fully porous particles for use as ultrafast second dimension columns in two-dimensional liquid chtomatography. J Chromatogr A 1386:31-8
Beyaza, Ayse; Fana, Wenzhe; Carr, Peter W et al. (2014) Instrument parameters controlling retention precision in gradient elution reversed-phase liquid. J Chromatogr A 1371:90-105
Potts, Lawrence W; Carr, Peter W (2013) Analysis of the temporal performance of one versus on-line comprehensive two-dimensional liquid chromatography. J Chromatogr A 1310:37-44
Haidar Ahmad, Imad A; Carr, Peter W (2013) Improved synthesis of carbon-clad silica stationary phases. Anal Chem 85:11765-70
Soliven, Arianne; Haidar Ahmad, Imad A; Filgueira, Marcelo R et al. (2013) Optimization of gradient reversed phase chromatographic peak capacity for low molecular weight solutes. J Chromatogr A 1273:57-65
Allen, Robert C; John, Mallory G; Rutan, Sarah C et al. (2012) Effect of background correction on peak detection and quantification in online comprehensive two-dimensional liquid chromatography using diode array detection. J Chromatogr A 1254:51-61
Filgueira, Marcelo R; Castells, Cecilia B; Carr, Peter W (2012) A simple, robust orthogonal background correction method for two-dimensional liquid chromatography. Anal Chem 84:6747-52
Allen, Robert C; Rutan, Sarah C (2012) Semi-automated alignment and quantification of peaks using parallel factor analysis for comprehensive two-dimensional liquid chromatography-diode array detector data sets. Anal Chim Acta 723:7-17
Zhang, Yu; Luo, Hao; Carr, Peter W (2012) Silica-based, hyper-crosslinked acid stable stationary phases for high performance liquid chromatography. J Chromatogr A 1228:110-24
Paek, Changyub; Huang, Yuan; Filgueira, Marcelo R et al. (2012) Development of a carbon clad core-shell silica for high speed two-dimensional liquid chromatography. J Chromatogr A 1229:129-39

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