Florida International University (FIU) is pursuing commercial partners interesting in developing and commercializing Silica Materials for High Performance Liquid Chromatographic (HPLC), Ultra-Performance Liquid Chromatographic (UPLC), and Solid Phase Extraction (SPE).
Currently available bonded phases used in HPLC, UPLC and SPE employ silica particles as the base material. To increase the phases applicability and adaptability, the surface of the particles can further be modified by bonding a wide variety of functional groups to the surface: non-polar (e.g. C18), polar (e.g. NH2), ionic (e.g. propylsulphonic acid) or mixed-mode (e.g. C8/cation exchange). However, the state of the art approach to preparing bonded silica particles results in a number of inherent shortcomings. For example, a thin coating of the bonded phase must provide all of the required analyte/sorbent/stationary phase interactions, which imposes a requirement of a high volume of stationary phase loaded into a long column size to achieve a large sample breakthrough volume, which is the maximum sample volume that can be passed through the column without saturating the bed with the analytes. Often there is an insufficient organic group loading per unit mass of the stationary phase/SPE sorbent to achieve adequate separation or absorption. Finally, the state of the art phases display a very narrow range of pH stability, typically, at best, having a robust stationary phase when maintained within a pH range of 2 to 8.
FIU inventors have developed sol-gel synthesis of alkyl functionalized (e.g., C4, C8, C12, C18) high performance liquid chromatographic (HPLC) stationary phases and solid phase extraction (SPE) sorbents. The synthetic method employs a tetrafunctional silane and a trifunctional silane containing a sorbent functionality, for example, tetraalkoxy silane and an alkyltrialkoxy silane or their equivalents in presence of either an acid catalyst, an acid catalyst followed by a base catalyst, or a base catalyst. This method yields a chemically and structurally more stable highly porous hybrid inorganic-inorganic material. Due to the high porosity and extremely high surface area, the HPLC stationary phase and SPE sorbents offer more analyte-alkyl functional group interactions per unit mass of the stationary phases/SPE sorbents, consequently minimizing the required mass of the stationary phases/SPE sorbents to achieve target chromatographic separation and extraction efficiency. Additionally, consumption of organic solvents in chromatographic separation and sample preparation is significantly reduced.
- HPLC stationary phases in both convention columns (5 micrometer particle size)
- UHPLC columns (submicron particle size)
- SPE reverse phase sorbents
- Eliminates the use of preformed silica particles as the inert surface to graft different alkyl pendant groups via silane surface modification
- Displays high porosity and high surface area
- Offers high chromatographic selectivity, separation power, and extraction efficiency
- Displays higher thermal, chemical and solvent stability, as well as extended pH stability (pH 1-12)
- Requires less volume of solvent during chromatographic separation or SPE elution
- Eliminates solvent evaporation and sample reconstitution when used as SPE sorbents