Silicon micropillar array electrospray chip for drug and biomolecule analysis

Rapid Commun Mass Spectrom. 2007;21(22):3677-82. doi: 10.1002/rcm.3266.

Abstract

We have developed a lidless micropillar array electrospray ionization chip (microPESI) combined with mass spectrometry (MS) for analysis of drugs and biomolecules. The microPESI chip, made of silicon, contains a sample introduction spot for a liquid sample, an array of micropillars (diameter, height, and distance between pillars in the range of 15-200, 20-40, and 2-80 microm, respectively), and a sharpened tip for direct electrospray formation. The microchips were fabricated using deep reactive ion etching (DRIE) which results in accurate dimensional control. The chip, providing a reliable open-channel filling structure based on capillary forces and a electrospray emitter tip for ionization, allows an easy operation and reliable, non-clogging liquid transfer. The microPESI chip can be used for a fast analysis using single sampling or for continuous infusion measurements using a syringe pump for sample introduction. The microPESI-MS shows high sensitivity, with limit of detection 30 pmol/L (60 amol or 28 fg) for verapamil measured with tandem mass spectrometry (MS/MS) and using a sample volume of 2.5 microL. The system shows also good quantitative linearity (r2 > 0.99) with linear dynamic range of at least six orders of magnitude and good ion current stability (standard deviation <5%) in 1-h continuous flow measurement. The microPESI-MS is shown to be a very potential method for direct analysis of drugs and biomolecules.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Animals
  • Anti-Arrhythmia Agents / analysis*
  • Microchemistry / instrumentation*
  • Microchemistry / methods
  • Peptides / analysis
  • Pharmaceutical Preparations / analysis
  • Spectrometry, Mass, Electrospray Ionization / instrumentation*
  • Spectrometry, Mass, Electrospray Ionization / methods
  • Tandem Mass Spectrometry / instrumentation
  • Tandem Mass Spectrometry / methods
  • Verapamil / analysis*

Substances

  • Anti-Arrhythmia Agents
  • Peptides
  • Pharmaceutical Preparations
  • Verapamil