title: On-line analysis of carbonyl compounds with derivatization in aqueous extracts of atmospheric particulate PM10 by in-tube solid-phase microextraction coupled to capillary liquid chromatography.
abstract: A new device for carbonyl compounds based on coupling on-line and miniaturizing both, sample pretreatment and chromatographic separation, is reported. Two capillary columns, a GC capillary column (95% methyl-5% phenyl substituted backbone, 70 cm × 0.32 mm i.d., 3 μm film thickness) in the injection valve for in-tube solid-phase microextraction (IT-SPME) and a Zorbax SB C18 (150 mm × 0.5 mm i.d., 5 μm particle diameter) LC capillary column were employed. Different combinations of IT-SPME and derivatization using 2,4-dinitrophenylhydrazine (DNPH) were examined for mixtures containing 15 carbonyl compounds (aliphatic, aromatic and unsaturated aldehydes and ketones). A screening analysis of aqueous extracts of atmospheric particulate PM(10) was carried out. Moreover, the possibility of coupling IT-SPME and conventional liquid chromatography is also tested. Derivatization solution and IT-SPME coupled to capillary liquid chromatography provided the best results for achieving the highest sensitivity for carbonyl compounds in atmospheric particulate analysis. Detection limits (LODs) using a photodiode array detector (DAD) were ranged from 30 to 198 ng L(-1), improving markedly those LODs reported by conventional SPME-LC-DAD.
authors.affiliation: Departamento de Química Analítica, Facultade de Ciencias, Universidade da Coruña, Campus da Zapateira, Coruña, Spain.
authors.forename: M C
authors.initials: MC
authors.lastname: Prieto-Blanco
authors.forename: P
authors.initials: P
authors.lastname: López-Mahía
authors.forename: P
authors.initials: P
authors.lastname: Campíns-Falcó
mesh_terms: D000096:Acetone / Q000032:analysis*; D000447:Aldehydes / Q000032:analysis*; D002853:Chromatography, Liquid / Q000379:methods*; D010316:Particle Size; D052638:Particulate Matter / Q000737:chemistry*; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D052617:Solid Phase Microextraction / Q000379:methods*
chemical_list: D000447:Aldehydes; D052638:Particulate Matter; D000096:Acetone