Dr. Zuzana Zajickova
Preparation and characterization of silica-, alumina- and organo-silica-based monolithic columns for applications in capillary-liquid chromatography
The main objective of this research is to involve science majors at Barry University with preparation of various monolithic separation media for applications in capillary liquid chromatography. The specific aims of the research project are:
- In-situ sol-gel synthesis of porous silica, alumina and hybrid monoliths
- Surface modification of monoliths via photografting
- Application of prepared monoliths in normal and reverse phase microscale-liquid chromatography
Particle packed columns have been used for more than a century for the separation of components of chemical mixtures utilizing high performance liquid chromatography. Over the past two decades, a new trend has been developing towards the improvement of the speed of analysis. The goal is to achieve sufficient resolution of analytes within the shortest possible time. High-throughput analyses are needed for rapid screening of numerous samples in fields such as drug discovery and environmental analysis.
Our attention is focused on the concept of the monolithic column which has been introduced as an alternative to particle packed columns. The advantages of the monoliths include lower back pressure, enhanced diffusional mass transfer, and operation at high flow rates, which enables faster analysis. Our research is directed towards the preparation and characterization of inorganic monolithic materials such as silica, and alumina and organic-silica hybrid. These materials are further coated with various polymer stationary phases via a novel approach called photografting which can be simply described as UV initiated radical polymerization in the presence of photoinitiator. By choosing different monomer we can alternate the surface chemistry of synthesized monoliths.
We prepare these materials inside of the fused silica capillary and we evaluate their chromatographic properties using microscale-liquid chromatography. The types of compounds suitable for chromatographic separations range from simple organic compounds to proteins and peptides. Among many facilities which would benefit from the advantages of these types of materials are chemical, biological, pharmaceutical, medical, industrial and environmental laboratories.
Undergraduate students will gain:
- Hands-on experience with the preparation and characterization of monolithic columns. Capillary preparation is low-cost, safe and requires minimal number of synthetic steps.
- Understanding of principles of sol-gel transitions and inorganic chemistry which are responsible for the formation of highly porous monoliths.
- Proficiency with photografting
- Chromatographic skills through the operation and troubleshooting of a liquid chromatograph.
- Understanding of basic separation principles applied in liquid chromatography based on observation of changes in chromatographic behavior of testing mixtures with various types of polymeric coatings.
- Sense for green chemistry. Capillary liquid chromatography allows operation in flow rates in the µL/min range (instead of mL/min) therefore minimizing the amount of solvent and analyte needed for analysis.
Undergraduate Research Assistants
Montaha Abdallah; Silva Campos Thales; Rebecca Hernandez; Lucas Narciso Meirelles; Zulema Rodriguez; Gabriella Soto - dental school Howard University; Taylor Sabol - PhD program in chemistry, Florida Atlantic University; Miriam Basden; Denae Britsch - dental school NOVA Southeastern University, Fort Lauderdale, FL; Deepa Gharbharan - MS anesthesiologist assistant program, NOVA Southeastern University; Brittany Kuhl - research and development scientist, Beckman Coulter, Miami, FL; Brittny Randolph - MS program in medical sciences, University of South Florida, Tampa, FL; Launie Bruno; Anna-Marie Weed – transferred to chemical engineering program at the University of Washington, Seattle, WA; Jill Dvornik -research associate Lawrence Berkeley National Laboratory, Berkeley, CA (2011-2013), assistant specialist University of California, San Francisco, CA, currently: associate researcher II Pharmacology and Systems Therapeutics, Mount Sinai Hospital, New York; Afua Gyapong graduated from Philadelphia College of Osteopathic Medicine, Georgia; Abraham Campos; John Jacob Stefancin; Marc Knezevic - M.S. program, Public Health, Florida International University; Emir D. Rubi - Ph.D. program, City of Hope, Duarte, CA; Joao C. Luna - obtained M.S. in Geochemistry, University of Georgia, Athens, GA 2013; currently: PhD program in Geology, University of Utah, Salt Lake City, UT; Cristina Marrero-Avila - completed D.O. program, NOVA Southeastern University, Fort Lauderdale, FL; Vanessa Narciso - D.M.D. program, NOVA Southeastern University, Fort Lauderdale, FL; Rafaela Nita - Ph.D. program Florida Institute of Technology, Melbourne, FL; Mario Cisneros - D.O. program, Edward Via College of Osteopathic Medicine, Spartanburg, SC; Heather Shetler; Ryoko Horigami; Stefanie Thompson Criminalist, Forensic Laboratory, Miami-Dade Police Department
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