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Silicon micropillar array electrospray chip for drug and biomolecule analysis

Teemu NissiläDivision of Pharmaceutical Chemistry, P.O. Box 56, FI-00014 University of Helsinki, FinlandLauri SainiemiHelsinki University of Technology, Micro and Nanosciences Laboratory, P.O. Box 3500, FI-02015 TKK, FinlandTiina SikanenDivision of Pharmaceutical Chemistry, P.O. Box 56, FI-00014 University of Helsinki, FinlandTapio KotiahoDivision of Pharmaceutical Chemistry, P.O. Box 56, FI-00014 University of Helsinki, FinlandSami FranssilaHelsinki University of Technology, Micro and Nanosciences Laboratory, P.O. Box 3500, FI-02015 TKK, FinlandRisto KostiainenDivision of Pharmaceutical Chemistry, P.O. Box 56, FI-00014 University of Helsinki, FinlandRaimo A. KetolaDivision of Pharmaceutical Chemistry, P.O. Box 56, FI-00014 University of Helsinki, Finland

2007en

ABI

Annotatsiya

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.

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DOI: 10.1002/rcm.3266

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