Microscale extraction combined with gas chromatography/mass spectrometry for the simultaneous determination of polycyclic aromatic hydrocarbons and polycyclic aromatic sulfur heterocycles in marine sediments.
J Chromatogr A
; 1653: 462414, 2021 Sep 13.
Article
en En
| MEDLINE
| ID: mdl-34320434
ABSTRACT
This paper describes a novel method based on an ultrasound-assisted extraction microscale device (UAE-MSD) for the rapid and simultaneous determination of polycyclic aromatic hydrocarbons (PAH) and polycyclic aromatic sulfur heterocycles (PASH) in marine sediments. Solvent extraction conditions were optimized by applying a simplex-centroid mixture design. Optimum conditions were used to validate and determine the concentrations of 17 PAH and 7 PASH. The best conditions were obtained by extracting sediments with 500 µL of DCMMeOH (6535, vv) over 23 min of sonication. Analytes were determined by gas chromatography/mass spectrometry in selective ion monitoring (GC-MS/SIM). Matrix effects were evaluated, and matrix-matched calibration was used for quantitation. Analytical method validation was carried out using the certified reference material NIST SRM 1941b, as well as sediment spiked with PASH at three concentration levels. Recoveries ranged between 70.0 ± 3.5% and 119 ± 9.1% for PAH and 80.6 ± 10.4% and 120 ± 10% for PASH. Linearity (R2) was ≥0.99 for all compounds. Method detection limits ranged from 8.8 to 30.2 ng g-1, while limits of quantification ranged from 29.4 to 1011 ng g-1. UAE-MSD was applied to marine sediments exposed to different anthropogenic impacts collected in Todos os Santos Bay, Brazil. PAH concentrations ranged from Palabras clave
Texto completo:
1
Colección:
01-internacional
Base de datos:
MEDLINE
Asunto principal:
Hidrocarburos Policíclicos Aromáticos
/
Monitoreo del Ambiente
/
Sedimentos Geológicos
/
Cromatografía de Gases y Espectrometría de Masas
País/Región como asunto:
America do sul
/
Brasil
Idioma:
En
Revista:
J Chromatogr A
Año:
2021
Tipo del documento:
Article
País de afiliación:
Brasil