RT Journal Article T1 Volatile organo-selenium speciation in biological matter by solid phase microextraction–moderate temperature multicapillary gas chromatography with microwave induced plasma atomic emission spectrometry detection A1 Dietz, Christian A1 Sanz Landaluce, Jon A1 Ximenez Embun, Pilar A1 Madrid Albarrán, María Yolanda A1 Cámara, Carmen AB Microwave induced plasma atomic emission spectrometry (MIP-AES) in combination with multicapillary (MC) gas chromatography couldbe proven to be useful for element specific detection of volatile species. Solid phase microextraction (SPME) was used for preconcentration andsample-matrix separation. The fiber desorption unit as well as the heating control for the MCcolumn were in-house developed and multicapillarycolumn was operated at moderate temperatures (30–100 ◦C). The method was optimized for organo-selenium species (dimethylselenide(DMSe), diethylselenide (DEtSe) and dimethyldiselenide (DMDSe)), using a chemometric approach. Stationary phases for the separationcolumn were optimized using a conventional GC and contrasted with the results obtained with the MC. Application was focussed on seleniumaccumulating biological matter, such as lupine, yeast, Indian mustard and garlic. These samples were grown in hydroponic solution containinginorganic selenium (Na2SeO3 and Na2SeO4). SPME sampling was carried out in fixed volume flow boxes in headspace above the living plantsand in vials using treated samples. Results demonstrate inorganic selenium transformation into volatile organic species during metabolism.Separation is fast, a chromatogram can be obtained in less than 3 min and detection limits were at sub-ppb level for all investigated species.The system is independent from the use of a conventional gas chromatographic oven and can be used as a versatile alternative to highly costintensive methods such as GC–ICP-MS. SN 0003-2670 YR 2004 FD 2004 LK https://hdl.handle.net/20.500.14352/52239 UL https://hdl.handle.net/20.500.14352/52239 LA eng DS Docta Complutense RD 24 abr 2025