Isocratic separation of four small monovalent organic acids using a weak hydroxide eluent

Singly charged anions of small organic acids can be challenging to separate due to their low retention on many ion chromatography columns. During method development for their analysis several different columns often need to be compared to find a separation selectivity that is suitable for the set of compounds in question.

The low retentivity and few structural features of small monovalent organic acids typically dictates a weak eluent for their elution. In complex samples that also contains polyvalent organic acids, an initial isocratic section with weak hydroxide eluent can therefore be required before the gradient sets in. This example comes from an ion chromatography screening study at Diduco which tested several columns for analysis of some organic acids that were to be analysed in a pharmaceutical formulation.

 

Ion chromatography of organic acids on a Shodex IC SI-37 4D column (150×4 mm) using an eluent containing 3 mM KOH in water pumped at 0.6 mL/min at 25 °C, continuously mixed online from two different EQAX-B1 eluent bottles (1 L), containing either ultrapure water or 0.1 M KOH eluent concentrate, both protected with EQAX-TC1 trap cartridges for carbon dioxide removal. Background reduced by XAMS suppressor with ASUREX-A200 automatic regenerator. Eluent pumping and conductivity detection by (Thermo) Dionex system with modules GS50, CD25, and LC30, connected to a Spark Holland Triathlon 900 autosampler. Injection of 20 µL of gluconate, pyroglutamate, glycolate, formate (20 mg/L) in water.

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