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Lowering the concentration limits of detection by on-line solid-phase extraction-capillary electrophoresis-electrospray mass spectrometry.
J Chromatogr A. 2007 Jan 26; 1140(1-2):205-12.JC

Abstract

The use of solid-phase extraction coupled on-line to capillary electrophoresis using electrospray mass spectrometry detection (SPE-CE-ESI-MS) is described for the analysis of peptides in dilute solutions. A SPE microcartridge or analyte concentrator containing C(18) derivatized silica particles as the extraction sorbent was easily constructed near the inlet of the separation capillary using commercially available materials. The reversed-phase sorbent selectively retained the target peptides, enabling large volumes of the sample to be introduced (>100muL). The captured analytes were eluted in a small volume of an appropriate solution (20-50nL). This resulted in sample clean-up and concentration enhancement, with minimum sample handling. As the SPE-CE conditions were compatible with on-line ESI-MS detection, the potential for identifying and characterizing the preconcentrated analytes by SPE-CE-ESI-MS using a sheath-flow CE-ESI-MS interface is also shown. Using separation electrolytes containing N-[carbamoylmethyl]-2-aminoethanesulfonic acid (ACES) at pH 7.4, an elution plug of 80:20 (v/v) (25mM of formic acid in MeCN):H(2)O and a sheath liquid of 20mM of acetic acid in 50:50 (v/v) methanol:H(2)O the concentration limits of detection for the analyzed peptides in the positive ion mode were lowered to nanogram per milliliter levels. The systematic optimization of the operational parameters involved in the development of the SPE-CE method is described in detail, in order to promote robust and quantitative SPE-CE-ESI-MS analysis and facilitate the widespread use of the technique.

Authors+Show Affiliations

Department of Analytical Chemistry, University of Barcelona, Diagonal 647, 08028 Barcelona, Spain. fbenavente@ub.eduNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

17174962

Citation

Benavente, Fernando, et al. "Lowering the Concentration Limits of Detection By On-line Solid-phase Extraction-capillary Electrophoresis-electrospray Mass Spectrometry." Journal of Chromatography. A, vol. 1140, no. 1-2, 2007, pp. 205-12.
Benavente F, Vescina MC, Hernández E, et al. Lowering the concentration limits of detection by on-line solid-phase extraction-capillary electrophoresis-electrospray mass spectrometry. J Chromatogr A. 2007;1140(1-2):205-12.
Benavente, F., Vescina, M. C., Hernández, E., Sanz-Nebot, V., Barbosa, J., & Guzman, N. A. (2007). Lowering the concentration limits of detection by on-line solid-phase extraction-capillary electrophoresis-electrospray mass spectrometry. Journal of Chromatography. A, 1140(1-2), 205-12.
Benavente F, et al. Lowering the Concentration Limits of Detection By On-line Solid-phase Extraction-capillary Electrophoresis-electrospray Mass Spectrometry. J Chromatogr A. 2007 Jan 26;1140(1-2):205-12. PubMed PMID: 17174962.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Lowering the concentration limits of detection by on-line solid-phase extraction-capillary electrophoresis-electrospray mass spectrometry. AU - Benavente,Fernando, AU - Vescina,M Cristina, AU - Hernández,Elena, AU - Sanz-Nebot,Victoria, AU - Barbosa,José, AU - Guzman,Norberto A, Y1 - 2006/12/18/ PY - 2006/07/31/received PY - 2006/11/23/revised PY - 2006/11/29/accepted PY - 2006/12/19/pubmed PY - 2007/3/24/medline PY - 2006/12/19/entrez SP - 205 EP - 12 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1140 IS - 1-2 N2 - The use of solid-phase extraction coupled on-line to capillary electrophoresis using electrospray mass spectrometry detection (SPE-CE-ESI-MS) is described for the analysis of peptides in dilute solutions. A SPE microcartridge or analyte concentrator containing C(18) derivatized silica particles as the extraction sorbent was easily constructed near the inlet of the separation capillary using commercially available materials. The reversed-phase sorbent selectively retained the target peptides, enabling large volumes of the sample to be introduced (>100muL). The captured analytes were eluted in a small volume of an appropriate solution (20-50nL). This resulted in sample clean-up and concentration enhancement, with minimum sample handling. As the SPE-CE conditions were compatible with on-line ESI-MS detection, the potential for identifying and characterizing the preconcentrated analytes by SPE-CE-ESI-MS using a sheath-flow CE-ESI-MS interface is also shown. Using separation electrolytes containing N-[carbamoylmethyl]-2-aminoethanesulfonic acid (ACES) at pH 7.4, an elution plug of 80:20 (v/v) (25mM of formic acid in MeCN):H(2)O and a sheath liquid of 20mM of acetic acid in 50:50 (v/v) methanol:H(2)O the concentration limits of detection for the analyzed peptides in the positive ion mode were lowered to nanogram per milliliter levels. The systematic optimization of the operational parameters involved in the development of the SPE-CE method is described in detail, in order to promote robust and quantitative SPE-CE-ESI-MS analysis and facilitate the widespread use of the technique. SN - 0021-9673 UR - https://www.unboundmedicine.com/medline/citation/17174962/Lowering_the_concentration_limits_of_detection_by_on_line_solid_phase_extraction_capillary_electrophoresis_electrospray_mass_spectrometry_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0021-9673(06)02256-4 DB - PRIME DP - Unbound Medicine ER -