Synthesis and application of a novel solid-phase microextraction adsorbent: hollow fiber supported carbon nanotube reinforced sol-gel for determination of phenobarbital

The present study reports the development, validation and application of a new green liquid chromatographic method for the determination of glutathione (GSH) in vegetable samples. In this work we introduce—for the first time—ethyl propiolate (EP) as an advantageous post-column derivatization reagent for thiolic compounds. GSH (t_R = 6.60 min) and N-acetylcysteine (NAC, internal standard) (t_R = 11.80 min) were separated efficiently from matrix endogenous compounds by using a 100% aqueous mobile phase (0.1%, v/v CH₃COOH in 1 mmol L⁻¹ EDTA, Q_V = 0.5 mL min⁻¹) and a Prevail^® reversed phase column that offers the advantage of stable packing material in aqueous mobile phases. The parameters of the post-column reaction (pH, amount concentration of the reagent, flow rates, length of the reaction coil and temperature) were studied. The linear determination range for GSH was 1–200 μmol L⁻¹ and the LOD was 0.1 μmol L⁻¹ (S/N = 3). Total endogenous GSH was determined in broccoli, potato, asparagus and Brussels sprouts using the standards addition approach. The accuracy was evaluated by both recovery experiments (R = 91–110%) and comparison to an o-phthalaldehyde/glycine corroborative post-column derivatization fluorimetric method.