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Chromatographic preconcentration coupled to capillary electrophoresis via an in-line injection valve.
Anal Chem. 2004 Aug 01; 76(15):4432-6.AC

Abstract

A preconcentration-capillary electrophoresis (CE) system using a small precolumn in combination with an in-line injection valve is presented. The advantage of the present design is the ability to perform the sample preconcentration fully independently from the CE separation and to prevent sample matrix and washing solvents from entering the CE capillary. With a micro injection valve, sample could be effectively introduced into the CE system in an in-line fashion without seriously affecting the CE separation efficiency. Breakthrough volume, desorption efficiency, and elution volume for the C18 microcolumn (5 x 0.5 mm i.d.) were established, yielding values of 750 microL, 70%, and 0.9-1.1 microL, respectively, using enkephalin peptides. The time between the start of the desorption of the analytes from the precolumn and the injection into the CE system was also studied in order to achieve optimal sensitivity and separation efficiency. The performance of the complete system was demonstrated by the preconcentration and separation of an enkephalin mixture. Using a sample volume of 250 microL and a CE injection voltage of -15 kV for 12 s, linearity was observed over 2 orders of magnitude, and detection limits (S/N = 3) were in the 5-10 ng/mL range. A 1000-fold sensitivity enhancement is obtained using this setup, as compared to a regular CE setup. For 100 ng/mL samples, repeatabilities (RSDs) of migration time and peak area were 1.2 and 11%, respectively.

Authors+Show Affiliations

Tempels FW
Department of Biomedical Analysis, Faculty of Pharmaceutical Sciences, Utrecht University, Sorbonnelaan 16, NL-3584 CA Utrecht, The Netherlands.
Underberg WJ
No affiliation info available
Somsen GW
No affiliation info available
de Jong GJ
No affiliation info available

MeSH

ChromatographyElectrophoresis, CapillaryEnkephalinsEquipment DesignIndicators and ReagentsPeptide FragmentsSolvents

Pub Type(s)

Journal Article

Language

eng

PubMed ID

15283584

Citation

Tempels, F W Alexander, et al. "Chromatographic Preconcentration Coupled to Capillary Electrophoresis Via an In-line Injection Valve." Analytical Chemistry, vol. 76, no. 15, 2004, pp. 4432-6.
Tempels FW, Underberg WJ, Somsen GW, et al. Chromatographic preconcentration coupled to capillary electrophoresis via an in-line injection valve. Anal Chem. 2004;76(15):4432-6.
Tempels, F. W., Underberg, W. J., Somsen, G. W., & de Jong, G. J. (2004). Chromatographic preconcentration coupled to capillary electrophoresis via an in-line injection valve. Analytical Chemistry, 76(15), 4432-6.
Tempels FW, et al. Chromatographic Preconcentration Coupled to Capillary Electrophoresis Via an In-line Injection Valve. Anal Chem. 2004 Aug 1;76(15):4432-6. PubMed PMID: 15283584.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Chromatographic preconcentration coupled to capillary electrophoresis via an in-line injection valve. AU - Tempels,F W Alexander, AU - Underberg,Willy J M, AU - Somsen,Govert W, AU - de Jong,Gerhardus J, PY - 2004/7/31/pubmed PY - 2006/5/3/medline PY - 2004/7/31/entrez SP - 4432 EP - 6 JF - Analytical chemistry JO - Anal Chem VL - 76 IS - 15 N2 - A preconcentration-capillary electrophoresis (CE) system using a small precolumn in combination with an in-line injection valve is presented. The advantage of the present design is the ability to perform the sample preconcentration fully independently from the CE separation and to prevent sample matrix and washing solvents from entering the CE capillary. With a micro injection valve, sample could be effectively introduced into the CE system in an in-line fashion without seriously affecting the CE separation efficiency. Breakthrough volume, desorption efficiency, and elution volume for the C18 microcolumn (5 x 0.5 mm i.d.) were established, yielding values of 750 microL, 70%, and 0.9-1.1 microL, respectively, using enkephalin peptides. The time between the start of the desorption of the analytes from the precolumn and the injection into the CE system was also studied in order to achieve optimal sensitivity and separation efficiency. The performance of the complete system was demonstrated by the preconcentration and separation of an enkephalin mixture. Using a sample volume of 250 microL and a CE injection voltage of -15 kV for 12 s, linearity was observed over 2 orders of magnitude, and detection limits (S/N = 3) were in the 5-10 ng/mL range. A 1000-fold sensitivity enhancement is obtained using this setup, as compared to a regular CE setup. For 100 ng/mL samples, repeatabilities (RSDs) of migration time and peak area were 1.2 and 11%, respectively. SN - 0003-2700 UR - https://www.unboundmedicine.com/medline/citation/15283584/Chromatographic_preconcentration_coupled_to_capillary_electrophoresis_via_an_in_line_injection_valve_ DB - PRIME DP - Unbound Medicine ER -