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Chip-based solid-phase extraction pretreatment for direct electrospray mass spectrometry analysis using an array of
Aimin Tan1, Salete Benetton, Jack D Henion
1Analytical Toxicology, New York State College of Veterinary Medicine, Cornell University, 927 Warren Drive, Ithaca, New York 14850, USA.
Analytical Chemistry
|January 9, 2004
Summary
This study developed a novel chip-based solid-phase extraction (SPE) system using porous monolithic columns for biological sample cleanup. The system demonstrates excellent reproducibility and linearity for pharmaceutical analysis, enabling efficient sample preparation for mass spectrometry.
Area of Science:
- Analytical Chemistry
- Materials Science
- Biotechnology
Background:
- Directly coupled electrospray mass spectrometry (ESI-MS) requires efficient sample cleanup for biological matrices.
- Existing solid-phase extraction (SPE) methods can be time-consuming and require significant sample volumes.
- Development of integrated, miniaturized sample preparation systems is crucial for high-throughput analysis.
Purpose of the Study:
- To develop and evaluate a novel chip-based SPE system utilizing an array of porous monolithic columns.
- To assess the performance of the chip-based SPE for cleanup of biological samples prior to ESI-MS.
- To demonstrate the analytical potential of the system for real-world sample analysis.
Main Methods:
- Fabrication of a Zeonor polymeric chip with eight parallel porous monolithic columns via UV-initiated polymerization.
- Characterization of monolithic columns using scanning electron microscopy.
- Evaluation of SPE performance including sample capacity, recovery, reproducibility, and linearity using imipramine as a test compound and ESI-MS.
Main Results:
- The chip-based SPE system demonstrated good reproducibility with a relative standard deviation (RSD) of 2.0% for peak height ratios across eight columns.
- Average recovery was 79.1% with an RSD of 7.9%, and a linear calibration curve (R2 = 0.9995) was achieved for imipramine.
- The system successfully analyzed real-world samples, including human urine and P450 drug metabolism mixtures, detecting metabolites.
Conclusions:
- The developed chip-based porous monolithic SPE system offers a robust and reproducible platform for biological sample cleanup.
- The system is suitable for direct coupling with ESI-MS, enabling sensitive analysis of pharmaceuticals and their metabolites.
- This technology holds significant potential for streamlining analytical workflows in various biological and pharmaceutical applications.