Determination of glycols in biological specimens by gas chromatography-mass spectrometry

A simple extraction and derivatization procedure for the analysis of eight glycols (ethylene glycol, EG; diethylene glycol, DEG; triethylene glycol, TEG; 1,2-propanediol, 1,2-PD; 1,3-propanediol, 1,3-PD; 1,2-butanediol, 1,2-BD; 2,3-butanediol, 2,3-BD; and hexylene glycol, HXG) using a 2-μL serum or blood sample is described. Following deproteinisation with acetonitrile, derivatization to its mono or di TMS derivative, glycols were detected using gas chromatography-electron impact mass spectrometry equipped with a split-spitless inlet and a DB-5MS column in the scan mode from 40 to 500 amu. Gamma-hydroxybutyrate-d6(GHB-d6) was used as the internal standard. The limits of detection and quantitation in 2 μL of serum ranged, respectively, from 0.7 mg/L for EG to 8.5 mg/L for TEG and from 1.3 mg/L for EG to 18.2 mg/L for 1,2-PD. A linear response was observed over the concentration range from 1 to 800 mg/L for EG and 18 from 800 for TEG and 1,2-PD for serum and blood. Coefficients of variation for both intra-assay precision and interassay reproductibility ranged respectively between 1.9% for TEG to 4.9% for 1,2-PD (11.8% for HXG) and 3.5% for DEG to 9% for 2,3-BD (20.4 for HXG) at the 400 mg/L serum level. The method was applied to plasma and whole blood.