Ion chromatography (IC) has been used extensively to separate and determine ionic and charged small molecules. When coupled with high resolution accurate mass (HRAM) spectrometry, the combined techniques provide confirmatory identification, structural interpretation, and higher sensitivity in complex matrices. With its unique selectivity and high retention and peak area stability, IC has been successfully applied to the identification and quantification of targeted charged metabolites in biological samples. Capillary IC-HRAM (Cap IC-HRAM) at �L/min flow rates furthers the capability of IC with respect to metabolite identification and quantification by improving the system sensitivity and stability as well as reducing the amount of sample required.Here we demonstrate the targeted analysis of metabolites. The analytes were separated on a capillary (0.4 mm i.d.) anion-exchange packed-resin column optimized for organic acid separations using an electrolytically generated hydroxide gradient by a Reagent-Free IC (RFIC) instrument. The IC-MS interface was optimized by continuous online desalting of the mobile phase and the introduction of an acetic acid-methanol desolvation solution. The analytes were detected by HRAM in full scan negative mode for selective and sensitive quantification. Using this configuration, targeted metabolites can be quantified at fmol levels, requiring only �Ls of sample, and linearity can be maintained over three to four orders of magnitude.

Determinations of targeted metabolites using capillary ion chromatography high resolution accurate mass spectrometry

247th National Meeting (2014)

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