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Improved silica xerogel film processing for MALDI-TOF–MS quantitative analysis of peptides and small molecules

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Abstract

In this work, sol–gel derived silica films were prepared for direct desorption/ionization of organic compounds in MALDI-TOF–MS analysis with the aim of improving method precision and of reducing interfering signals at low m/z values. Two commonly used MALDI matrices, 2,5-dihydroxybenzoic acid (DHB) and α-cyano-4-hydroxycinnamic acid (CHCA), were incorporated into the sol–gel network in order to absorb laser energy and to induce analyte desorption/ionization with low or absent background signals in the mass spectra. To achieve a reproducible xerogel film formation, experimental parameters for its deposition were optimized. The gel matrices were characterized by Fourier Transform Infrared (FT-IR) spectroscopy, X-ray Diffraction (XRD), and Scanning Electron Microscopy (SEM) analysis. The results proved the embedding of the matrix molecules in a disperse form into the homogeneous sol–gel material. The sol–gel matrix was then tested for the qualitative and quantitative analysis of two reference peptides, such as Bradykinin and P14R. In addition, spectral quality and method performance were assessed for quantitation of melamine, a low-molecular weight compound of food safety concern. In all cases, high quality spectra and excellent mass accuracy (between 3.5 and 13 ppm) were observed. Furthermore, the experimental results evidenced a significant improvement of the measurement repeatability on spot and between spots (relative standard deviation <10%), with respect to the traditional dried-droplet sample deposition method. Good sensitivity and linearity in the concentration range explored were obtained for peptides and melamine, demonstrating the suitability of the sol–gel-based matrix to be used for quantitative analysis.

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Acknowledgments

The Project was funded by Laboratorio Regionale SITEIA (PRRIITT Misura 4 “Sviluppo di rete”, Azione A—Laboratori di ricerca e trasferimento tecnologico, DGR n. 1853/07). The facilities of the Centro Interdipartimentale Misure (CIM) “Giuseppe Casnati” (University of Parma) were used to perform MALDI-TOF–MS analysis. Thanks are due to Dr. Marco Rocchetti for helpful discussions and suggestions.

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  1. Dipartimento di Chimica Generale e Inorganica, Chimica Analitica, Chimica Fisica, Università degli Studi di Parma, Parco Area delle Scienze 17/A, I-43124, Parma, Italy

    M. Careri, L. Elviri, A. Lorenzi, A. Mangia, A. Penna & G. Predieri

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  1. M. Careri
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  2. L. Elviri
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  3. A. Lorenzi
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  4. A. Mangia
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  5. A. Penna
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  6. G. Predieri
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Correspondence to L. Elviri.

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Careri, M., Elviri, L., Lorenzi, A. et al. Improved silica xerogel film processing for MALDI-TOF–MS quantitative analysis of peptides and small molecules. J Sol-Gel Sci Technol 60, 359–365 (2011). https://doi.org/10.1007/s10971-011-2555-z

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  • DOI: https://doi.org/10.1007/s10971-011-2555-z

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