title: Ultrasound-assisted dispersive liquid-liquid microextraction for the determination of synthetic musk fragrances in aqueous matrices by gas chromatography-mass spectrometry.
abstract: A rapid and simple method for the simultaneous determination of twelve synthetic musks in water samples, using ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) coupled with gas chromatography-mass spectrometry (GC-MS) was successfully developed. The influence of seven factors (volume of the extraction solvent and disperser solvent, sample volume, extraction time, ionic strength, type of extraction and disperser solvent) affecting the UA-DLLME extraction efficiency was investigated using a screening design. The significant factors were selected and optimised employing a central composite design: 80 μL of chloroform, 880 μL of acetonitrile, 6 mL of sample volume, 3.5% (wt) of NaCl and 2 min of extraction time. Under the optimised conditions, this methodology was successfully validated for the analysis of 12 synthetic musk compounds in different aqueous samples (tap, sea and river water, effluent and influent wastewater). The proposed method showed enrichment factors between 101 and 115 depending on the analyte, limits of detection in the range of 0.004-54 ng L(-1) and good repeatability (most relative standard deviation values below 10%). No significant matrix effects were found, since recoveries ranged between 71% and 118%. Finally, the method was satisfactorily applied to the analysis of five different aqueous samples. Results demonstrated the existence of a larger amount of synthetic musks in wastewaters than in other water samples (average concentrations of 2800 ng L(-1) in influent and 850 ng L(-1) in effluent). Galaxolide, tonalide and exaltolide were the compounds most detected.
authors.affiliation: LEPABE - Laboratory for Process Engineering, Environment, Biotechnology and Energy, Faculty of Engineering, University of Porto, Rua Dr. Roberto Frias, 4200-465 Porto, Portugal. Electronic address: vhomem@fe.up.pt.
authors.forename: Vera
authors.initials: V
authors.lastname: Homem
authors.affiliation: LEPABE - Laboratory for Process Engineering, Environment, Biotechnology and Energy, Faculty of Engineering, University of Porto, Rua Dr. Roberto Frias, 4200-465 Porto, Portugal. Electronic address: alice.a.alves.13@gmail.com.
authors.forename: Alice
authors.initials: A
authors.lastname: Alves
authors.affiliation: LEPABE - Laboratory for Process Engineering, Environment, Biotechnology and Energy, Faculty of Engineering, University of Porto, Rua Dr. Roberto Frias, 4200-465 Porto, Portugal. Electronic address: aalves@fe.up.pt.
authors.forename: Arminda
authors.initials: A
authors.lastname: Alves
authors.affiliation: LEPABE - Laboratory for Process Engineering, Environment, Biotechnology and Energy, Faculty of Engineering, University of Porto, Rua Dr. Roberto Frias, 4200-465 Porto, Portugal. Electronic address: lsantos@fe.up.pt.
authors.forename: Lúcia
authors.initials: L
authors.lastname: Santos
mesh_terms: D005229:Fatty Acids, Monounsaturated / Q000032:analysis* / Q000138:chemical synthesis; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D059627:Liquid Phase Microextraction / Q000379:methods*; D010476:Perfume / Q000032:analysis* / Q000138:chemical synthesis; D000069453:Ultrasonic Waves; D014867:Water / Q000032:analysis*; D014874:Water Pollutants, Chemical / Q000032:analysis
chemical_list: D005229:Fatty Acids, Monounsaturated; D010476:Perfume; D014874:Water Pollutants, Chemical; D014867:Water; C008563:musk
keywords: Design of experiments; Gas chromatography–mass spectrometry; Synthetic musks; Ultrasound-assisted dispersive liquid–liquid microextraction; Water samples