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Published on: April 23, 2019
Evaluation of on-line solid-phase extraction parameters for hyphenated, high-performance liquid
Cailean Clarkson1, Martin Sibum, Robert Mensen
1Department of Medicinal Chemistry, Faculty of Pharmaceutical Sciences, University of Copenhagen, Universitetsparken 2, DK-2100 Copenhagen, Denmark.
Journal of Chromatography. A
|August 22, 2007
Summary
Polystyrene/divinylbenzene polymers show superior trapping efficiency for HPLC-SPE-NMR, especially for hydrophobic compounds. Optimizing acetonitrile concentration is crucial for maximizing analyte capture in mass-limited sample analysis.
Area of Science:
- Analytical Chemistry
- Natural Product Chemistry
Background:
- High-Performance Liquid Chromatography-Solid Phase Extraction-Nuclear Magnetic Resonance (HPLC-SPE-NMR) is valuable for structure elucidation.
- Mass-limited samples pose challenges for traditional isolation methods.
Purpose of the Study:
- To evaluate Solid Phase Extraction (SPE) trapping performance for HPLC-SPE-NMR.
- To assess various stationary phases for their suitability in this hyphenated technique.
Main Methods:
- Tested 25 model natural products using six silica-based bonded phases and two polymeric phases.
- Investigated the impact of acetonitrile concentration and flow rate on trapping efficiency.
- Utilized frontal chromatography analysis to determine breakthrough levels.
Main Results:
- Polystyrene/divinylbenzene polymers demonstrated superior trapping efficiency compared to silica-based phases.
- Hydrophobic analytes showed better trapping on silica phases.
- Acetonitrile concentration in the loading solvent critically affected trapping on polymeric phases.
- Multiple trapping simulations indicated high performance for hydrophobic and moderate performance for polar analytes.
Conclusions:
- Polymeric phases, particularly Resin GP, are highly effective for SPE trapping in HPLC-SPE-NMR.
- Optimized loading solvent conditions are essential for maximizing trapping efficiency.
- The HPLC-SPE-NMR technique, with optimized SPE, enables significant analyte accumulation for mass-limited samples.
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