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Evaluation of fritless solid-phase extraction coupled on-line with capillary electrophoresis-mass spectrometry for the analysis of opioid peptides in cerebrospinal fluid.
Electrophoresis. 2014 Oct; 35(20):2996-3002.E

Abstract

Fritless SPE on-line coupled to CE with UV and MS detection (SPE-CE-UV and SPE-CE-MS) was evaluated for the analysis of opioid peptides. A microcartridge of 150 μm id was packed with a C18 sorbent (particle size > 50 μm), which was retained between a short inlet capillary and a separation capillary (50 μm id). Several experimental parameters were optimized by SPE-CE-UV using solutions of dynorphin A (DynA), endomorphin 1 (End1), and methionine-enkephaline (Met). A microcartridge length of 4 mm was selected, sample was loaded for 10 min at 930 mbar and the retained peptides were eluted with 67 nL of an acidic hydro-organic solution. Using SPE-CE-MS, peak area and migration time repeatabilities for the three opioid peptides were 12-27% and 4-5%, respectively. SPE recovery was lower for the less hydrophobic DynA (22%) than for End1 (66%) and Met (78%) and linearity was satisfactory in all cases between 5 and 60 ng/mL. The LODs varied between 0.5 and 1.0 ng/mL which represent an enhancement of two orders of magnitude when compared with CE-MS. Cerebrospinal fluid (CSF) samples spiked with the opioid peptides were analyzed to demonstrate the applicability to biological samples. Peak area and migration time repeatabilities were similar to the standard solutions and the opioid peptides could be detected down to 1.0 ng/mL.

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Publisher Full Text (DOI)

Authors+Show Affiliations

Medina-Casanellas S
Department of Analytical Chemistry, University of Barcelona, Barcelona, Spain.
Tak YH
No affiliation info available
Benavente F
No affiliation info available
Sanz-Nebot V
No affiliation info available
Sastre Toraño J
No affiliation info available
Somsen GW
No affiliation info available
de Jong GJ
No affiliation info available

MeSH

Electrophoresis, CapillaryEquipment DesignHumansLimit of DetectionLinear ModelsMass SpectrometryOpioid PeptidesReproducibility of ResultsSolid Phase Extraction

Pub Type(s)

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

Language

eng

PubMed ID

25074562

Citation

Medina-Casanellas, Silvia, et al. "Evaluation of Fritless Solid-phase Extraction Coupled On-line With Capillary Electrophoresis-mass Spectrometry for the Analysis of Opioid Peptides in Cerebrospinal Fluid." Electrophoresis, vol. 35, no. 20, 2014, pp. 2996-3002.
Medina-Casanellas S, Tak YH, Benavente F, et al. Evaluation of fritless solid-phase extraction coupled on-line with capillary electrophoresis-mass spectrometry for the analysis of opioid peptides in cerebrospinal fluid. Electrophoresis. 2014;35(20):2996-3002.
Medina-Casanellas, S., Tak, Y. H., Benavente, F., Sanz-Nebot, V., Sastre Toraño, J., Somsen, G. W., & de Jong, G. J. (2014). Evaluation of fritless solid-phase extraction coupled on-line with capillary electrophoresis-mass spectrometry for the analysis of opioid peptides in cerebrospinal fluid. Electrophoresis, 35(20), 2996-3002. https://doi.org/10.1002/elps.201400293
Medina-Casanellas S, et al. Evaluation of Fritless Solid-phase Extraction Coupled On-line With Capillary Electrophoresis-mass Spectrometry for the Analysis of Opioid Peptides in Cerebrospinal Fluid. Electrophoresis. 2014;35(20):2996-3002. PubMed PMID: 25074562.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Evaluation of fritless solid-phase extraction coupled on-line with capillary electrophoresis-mass spectrometry for the analysis of opioid peptides in cerebrospinal fluid. AU - Medina-Casanellas,Silvia, AU - Tak,Yvonne H, AU - Benavente,Fernando, AU - Sanz-Nebot,Victoria, AU - Sastre Toraño,Javier, AU - Somsen,Govert W, AU - de Jong,Gerhardus J, PY - 2014/06/16/received PY - 2014/07/18/revised PY - 2014/07/19/accepted PY - 2014/7/31/entrez PY - 2014/7/31/pubmed PY - 2015/6/9/medline KW - CE KW - Cerebrospinal Fluid KW - Neuropeptides KW - On-line preconcentration KW - SPE SP - 2996 EP - 3002 JF - Electrophoresis JO - Electrophoresis VL - 35 IS - 20 N2 - Fritless SPE on-line coupled to CE with UV and MS detection (SPE-CE-UV and SPE-CE-MS) was evaluated for the analysis of opioid peptides. A microcartridge of 150 μm id was packed with a C18 sorbent (particle size > 50 μm), which was retained between a short inlet capillary and a separation capillary (50 μm id). Several experimental parameters were optimized by SPE-CE-UV using solutions of dynorphin A (DynA), endomorphin 1 (End1), and methionine-enkephaline (Met). A microcartridge length of 4 mm was selected, sample was loaded for 10 min at 930 mbar and the retained peptides were eluted with 67 nL of an acidic hydro-organic solution. Using SPE-CE-MS, peak area and migration time repeatabilities for the three opioid peptides were 12-27% and 4-5%, respectively. SPE recovery was lower for the less hydrophobic DynA (22%) than for End1 (66%) and Met (78%) and linearity was satisfactory in all cases between 5 and 60 ng/mL. The LODs varied between 0.5 and 1.0 ng/mL which represent an enhancement of two orders of magnitude when compared with CE-MS. Cerebrospinal fluid (CSF) samples spiked with the opioid peptides were analyzed to demonstrate the applicability to biological samples. Peak area and migration time repeatabilities were similar to the standard solutions and the opioid peptides could be detected down to 1.0 ng/mL. SN - 1522-2683 UR - https://www.unboundmedicine.com/medline/citation/25074562/Evaluation_of_fritless_solid_phase_extraction_coupled_on_line_with_capillary_electrophoresis_mass_spectrometry_for_the_analysis_of_opioid_peptides_in_cerebrospinal_fluid_ DB - PRIME DP - Unbound Medicine ER -