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Nonaqueous electrokinetic chromatography-electrospray ionization mass spectrometry using anionic cyclodextrins.
J Chromatogr A. 2007 Aug 03; 1159(1-2):51-7.JC

Abstract

The set-up of an on-line method for coupling nonaqueous electrokinetic chromatography (NAEKC) and electrospray ionization mass spectrometry (ESI-MS) is presented. It allows the use of the single-isomer derivative anionic cyclodextrins heptakis(2,3-di-O-methyl-6-O-sulfo)-beta-cyclodextrin (HDMS-beta-CD) and heptakis(2,3-di-O-acetyl-6-O-sulfo)-beta-cyclodextrin (HDAS-beta-CD) for chiral and achiral separations of positively charged analytes. The effect of the cyclodextrins (CDs) on the MS signal intensities of model compounds was studied. When a voltage is applied over the CE capillary, the overall mobility of the CDs is towards the inlet vial preventing CDs from entering the ion source. However, the sodium counter ions of the CDs still enter the ion source and appeared to cause ionization suppression. Nevertheless, significant analyte signals could still be detected with detection limits in the sub-microg/ml. System parameters such as sheath liquid composition and flow rate, nebulizing gas pressure, capillary position in the sprayer and the drying gas flow and temperature were studied and optimized. The selection of a relatively low nebulizing gas pressure appeared to be important to achieve optimum sensitivity. The chiral selectivity of the NAEKC-ESI-MS system could be improved by addition of camphorsulfonate to the background electrolyte. Using mixtures of drugs and drug-related compounds, the NAEKC-ESI-MS system is shown to offer potential for (chiral) drug profiling.

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Authors+Show Affiliations

Mol R
Department of Biomedical Analysis, Utrecht University, NL-3508 TB Utrecht, The Netherlands.
Servais AC
No affiliation info available
Fillet M
No affiliation info available
Crommen J
No affiliation info available
de Jong GJ
No affiliation info available
Somsen GW
No affiliation info available

MeSH

Air PressureAnionsCapillary ElectrochromatographyCyclodextrinsElectrolytesElectrophoresis, CapillaryOnline SystemsSensitivity and SpecificitySolutionsSpectrometry, Mass, Electrospray IonizationStereoisomerismbeta-Cyclodextrins

Pub Type(s)

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

Language

eng

PubMed ID

17543975

Citation

Mol, Roelof, et al. "Nonaqueous Electrokinetic Chromatography-electrospray Ionization Mass Spectrometry Using Anionic Cyclodextrins." Journal of Chromatography. A, vol. 1159, no. 1-2, 2007, pp. 51-7.
Mol R, Servais AC, Fillet M, et al. Nonaqueous electrokinetic chromatography-electrospray ionization mass spectrometry using anionic cyclodextrins. J Chromatogr A. 2007;1159(1-2):51-7.
Mol, R., Servais, A. C., Fillet, M., Crommen, J., de Jong, G. J., & Somsen, G. W. (2007). Nonaqueous electrokinetic chromatography-electrospray ionization mass spectrometry using anionic cyclodextrins. Journal of Chromatography. A, 1159(1-2), 51-7.
Mol R, et al. Nonaqueous Electrokinetic Chromatography-electrospray Ionization Mass Spectrometry Using Anionic Cyclodextrins. J Chromatogr A. 2007 Aug 3;1159(1-2):51-7. PubMed PMID: 17543975.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Nonaqueous electrokinetic chromatography-electrospray ionization mass spectrometry using anionic cyclodextrins. AU - Mol,Roelof, AU - Servais,Anne-Catherine, AU - Fillet,Marianne, AU - Crommen,Jacques, AU - de Jong,Gerhardus J, AU - Somsen,Govert W, Y1 - 2007/05/18/ PY - 2007/03/01/received PY - 2007/05/11/revised PY - 2007/05/15/accepted PY - 2007/6/5/pubmed PY - 2007/10/4/medline PY - 2007/6/5/entrez SP - 51 EP - 7 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1159 IS - 1-2 N2 - The set-up of an on-line method for coupling nonaqueous electrokinetic chromatography (NAEKC) and electrospray ionization mass spectrometry (ESI-MS) is presented. It allows the use of the single-isomer derivative anionic cyclodextrins heptakis(2,3-di-O-methyl-6-O-sulfo)-beta-cyclodextrin (HDMS-beta-CD) and heptakis(2,3-di-O-acetyl-6-O-sulfo)-beta-cyclodextrin (HDAS-beta-CD) for chiral and achiral separations of positively charged analytes. The effect of the cyclodextrins (CDs) on the MS signal intensities of model compounds was studied. When a voltage is applied over the CE capillary, the overall mobility of the CDs is towards the inlet vial preventing CDs from entering the ion source. However, the sodium counter ions of the CDs still enter the ion source and appeared to cause ionization suppression. Nevertheless, significant analyte signals could still be detected with detection limits in the sub-microg/ml. System parameters such as sheath liquid composition and flow rate, nebulizing gas pressure, capillary position in the sprayer and the drying gas flow and temperature were studied and optimized. The selection of a relatively low nebulizing gas pressure appeared to be important to achieve optimum sensitivity. The chiral selectivity of the NAEKC-ESI-MS system could be improved by addition of camphorsulfonate to the background electrolyte. Using mixtures of drugs and drug-related compounds, the NAEKC-ESI-MS system is shown to offer potential for (chiral) drug profiling. SN - 0021-9673 UR - https://www.unboundmedicine.com/medline/citation/17543975/Nonaqueous_electrokinetic_chromatography_electrospray_ionization_mass_spectrometry_using_anionic_cyclodextrins_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0021-9673(07)00908-9 DB - PRIME DP - Unbound Medicine ER -