Multisyringe ion chromatography with chemiluminescence detection for the determination of oxalate in beer and urine samples

The first multisyringe-based low-pressure ion chromatographic method is presented. It is based on the use of short surfactant coated octadecyl-silica monolithic columns. As a first application, we have determined oxalate in beer and human urine via post-column chemiluminescence detection. Oxalate is separated from the sample matrix in the monolithic column by precise programmable fluid handling, and then detected by reaction with on-line generated tris(2,2′-bipyridyl)ruthenium(III). Column coating, un-coating, ion chromatography and chemiluminescence detection are quickly performed by using a simple low-pressure multi-burette. The factors influencing the separation of oxalate and its subsequent detection, including the column coating with surfactants and its stability have been studied. The chromatographic behavior of the oxalate in presence of potentially interfering species also was assessed. The method has limits of detection and quantification of 0.025 and 0.035 mg L⁻¹, respectively, a relative standard deviation of 3.1% (for 10 consecutive measurements without column re-coating) and a throughput of 48 h⁻¹. The results obtained with real samples were validated by using an enzymatic spectrophotometric test. The method is critically compared to recent methods for the determination of oxalate.