An analytical method for determining seleno-methionine (SeMet), methyl-seleno-cysteine and seleno-cystine in extra-virgin olive oil (EVOO) was developed and validated. EVOO sample (15 g) was diluted with hexane, extracted with methanol/water 80:20 (v/v), and cleaned up by a reversed phase/strong cation exchange solid phase extraction. Analysis was performed by chiral hydrophilic interaction liquid chromatography-tandem mass spectrometry. Process efficiency ranged between 49 and 97% and trueness between 87 and 126%, with intermediate precision, expressed as standard deviation, lower than 10%. Method detection limits (MDLs) and method quantification limits (MQLs) were lower than 1 μg kg −1 . Thirty-two EVOO samples from different Italian regions were analyzed for both total Se and single seleno-amino acids determination. Only L-SeMet was found at level MQL (0.2 μg kg −1 )-1.42 μg kg −1 in ten samples, while total Se was in the range of MDL-9.1 μg kg −1 . Concentration of L-SeMet (5–6% of total Se) and total Se correlated very well to each other (R 2 = 0.995). © 2018 Elsevier Ltd
Investigation of free seleno-amino acids in extra-virgin olive oil by mixed mode solid phase extraction cleanup and enantioselective hydrophilic interaction liquid chromatography-tandem mass spectrometry / Piovesana, Susy; Montone, Carmela Maria; Antonelli, Michela; Cavaliere, Chiara; La Barbera, Giorgia; Canepari, Silvia; Samperi, Roberto; Laganà, Aldo; Capriotti, Anna Laura. - In: FOOD CHEMISTRY. - ISSN 0308-8146. - 278:(2019), pp. 17-25. [10.1016/j.foodchem.2018.11.053]
Investigation of free seleno-amino acids in extra-virgin olive oil by mixed mode solid phase extraction cleanup and enantioselective hydrophilic interaction liquid chromatography-tandem mass spectrometry
Piovesana, Susy;Montone, Carmela Maria;Antonelli, Michela;Cavaliere, Chiara
;La Barbera, Giorgia;Canepari, Silvia;Samperi, Roberto;Laganà, Aldo;Capriotti, Anna Laura
2019
Abstract
An analytical method for determining seleno-methionine (SeMet), methyl-seleno-cysteine and seleno-cystine in extra-virgin olive oil (EVOO) was developed and validated. EVOO sample (15 g) was diluted with hexane, extracted with methanol/water 80:20 (v/v), and cleaned up by a reversed phase/strong cation exchange solid phase extraction. Analysis was performed by chiral hydrophilic interaction liquid chromatography-tandem mass spectrometry. Process efficiency ranged between 49 and 97% and trueness between 87 and 126%, with intermediate precision, expressed as standard deviation, lower than 10%. Method detection limits (MDLs) and method quantification limits (MQLs) were lower than 1 μg kg −1 . Thirty-two EVOO samples from different Italian regions were analyzed for both total Se and single seleno-amino acids determination. Only L-SeMet was found at level MQL (0.2 μg kg −1 )-1.42 μg kg −1 in ten samples, while total Se was in the range of MDL-9.1 μg kg −1 . Concentration of L-SeMet (5–6% of total Se) and total Se correlated very well to each other (R 2 = 0.995). © 2018 Elsevier LtdFile | Dimensione | Formato | |
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