An Ultrasound-Vortex-Assisted Dispersive Liquid-Liquid Micro-Extraction (USVADLLME) procedure (Figure 1) coupled with a gas chromatography-ion trap mass spectrometry (GC-IT/MS) [1] is proposed for fast analysis of nine PolyAromatic Hydrocarbons, PAHs, (fluorene, phenanthrene, anthracene, fluoranthene, pyrene, crysene, benzo(b)fluoranthene, 3,4-benzopyrene and benzoperylene) in beer (alcohol by volume, alc vol-1, ≤ 7 %). Among 5 possible extraction solvents tested, dichloromethane, density 1.325 g mL-1 at 25°C, was selected for further method development. Parameters such as extraction solvent type and volume, extraction time and pH, and NaCl concentration were optimized. Under optimal conditions, the enrichment factor of the nine analytes ranges from 100 to 1000 fold and the recoveries from 93% to 103% and correlation coefficients range from 0.9982 to 0.9999. The limit of detection (LOD) and limit of quantification (LOQ) are ≥ 3.8 pg μL-1 and ≥ 9.8 pg μL-1, respectively. The precisions expressed as relative standard deviation (RSD), are ≤ 4.0 %. The whole proposed methodology has demonstrated to be simple, reproducible and sensible for the determination of trace PAHs in beer samples.
Fast analysis of nine PAHs in beer by ultrasound-vortex-assisted dispersive liquid-liquid micro-extraction coupled with gas chromatography-ion trap mass spectrometry
RUSSO, Mario Vincenzo;P. Avino;
2014-01-01
Abstract
An Ultrasound-Vortex-Assisted Dispersive Liquid-Liquid Micro-Extraction (USVADLLME) procedure (Figure 1) coupled with a gas chromatography-ion trap mass spectrometry (GC-IT/MS) [1] is proposed for fast analysis of nine PolyAromatic Hydrocarbons, PAHs, (fluorene, phenanthrene, anthracene, fluoranthene, pyrene, crysene, benzo(b)fluoranthene, 3,4-benzopyrene and benzoperylene) in beer (alcohol by volume, alc vol-1, ≤ 7 %). Among 5 possible extraction solvents tested, dichloromethane, density 1.325 g mL-1 at 25°C, was selected for further method development. Parameters such as extraction solvent type and volume, extraction time and pH, and NaCl concentration were optimized. Under optimal conditions, the enrichment factor of the nine analytes ranges from 100 to 1000 fold and the recoveries from 93% to 103% and correlation coefficients range from 0.9982 to 0.9999. The limit of detection (LOD) and limit of quantification (LOQ) are ≥ 3.8 pg μL-1 and ≥ 9.8 pg μL-1, respectively. The precisions expressed as relative standard deviation (RSD), are ≤ 4.0 %. The whole proposed methodology has demonstrated to be simple, reproducible and sensible for the determination of trace PAHs in beer samples.I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.
