title: Optimization of comprehensive two dimensional gas chromatography-flame ionization detection-quadrupole mass spectrometry for the separation of octyl- and nonylphenol isomers.
abstract: In the present work, the separation of complex nonylphenol technical mixtures has been optimized using comprehensive two-dimensional gas chromatography coupled with a flame ionization detector and quadrupole mass spectrometer (GC×GC-qMS), using valve-based modulator. The optimization of GC×GC-qMS has been carried out using experimental designs and the optimal separation was obtained at the following conditions: 1st column flow: 1mL/min; 2nd column flow: 17.75 mL/min, oven temperature ramp: 1°C/min, modulation period: 1.5s and discharge time: 0.12s. These values have been used to determinate the previously synthesized 22OP, 33OP, 363NP and 22NP isomers in two different nonylphenol technical mixtures. Percentages obtained were as follows: 4.86% and 0.59% for 22OP, 4.91% and 2.82% for 33OP, 11.79% and 7.71% for 363NP and 2.28% and 1.98% for 22NP, in Fluka and Aldrich mixtures, respectively. The values obtained for NP isomers are in good agreement with the literature.
authors.affiliation: Kimika Analitikoa Saila, Euskal Herriko Unibertsitatea, Bilbao, Spain. asier.vallejo@ehu.es
authors.forename: A
authors.initials: A
authors.lastname: Vallejo
authors.forename: M
authors.initials: M
authors.lastname: Olivares
authors.forename: L A
authors.initials: LA
authors.lastname: Fernández
authors.forename: N
authors.initials: N
authors.lastname: Etxebarria
authors.forename: S
authors.initials: S
authors.lastname: Arrasate
authors.forename: E
authors.initials: E
authors.lastname: Anakabe
authors.forename: A
authors.initials: A
authors.lastname: Usobiaga
authors.forename: O
authors.initials: O
authors.lastname: Zuloaga
mesh_terms: D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D007536:Isomerism; D010636:Phenols / Q000737:chemistry / Q000302:isolation & purification*; D015203:Reproducibility of Results; D014874:Water Pollutants, Chemical / Q000737:chemistry / Q000302:isolation & purification*
chemical_list: D010636:Phenols; D014874:Water Pollutants, Chemical; C474055:octylphenol; C025256:nonylphenol