Trace determination of glycols by HPLC with UV and electrospray ionizationmass spectrometric detections

A high-performance liquid chromatography/mass spectrometry (HPLC/MS) method is developed for trace determination of glycols (ethylene glycol, 1,2- and 1,3-propylene glycols, and 2,3-butylene glycol) in water after derivatizat ion with benzoyl chloride. Benzoyl esters of glycols are separated by micro column reversed-phase HPLC. Sensitivity and linearity of UV detection at 23 7 nm is compared with electrospray ionization mass spectrometric (ESI-MS) d etection using selected ion monitoring. Limits of detection (LOD) and quant itation (LOQ) for UV detection are 1 and 2 mg/L, respectively. For ESI-MS d etection, LOD and LOQ are in the ranges 10-25 and 20-50 mu g/L, respectivel y. LOD obtained by ESI-MS for the determination of glycols is improved by 2 -3 orders of magnitude in comparison to previously published methods. The e ffect of the structure of isomeric glycols on their electrospray mass spect ra is discussed. The method has been applied for the determination of glyco ls in aqueous matrixes containing high concentrations of salts occurring in nuclear waste disposal treatment.