Determination of endocrine-disrupting compounds in water samples by magnetic nanoparticle-assisted dispersive liquid-liquid microextraction combined with gas chromatography-tandem mass spectrometry.
A rapid extraction procedure is presented for the determination of five endocrine-disrupting compounds, estrone, ethinylestradiol, bisphenol A, triclosan, and 2-ethylhexylsalicylate, in water samples. The analysis involves a two-step extraction procedure that combines dispersive liquid-liquid microextraction (DLLME) with dispersive micro-solid phase extraction (D-μ-SPE), using magnetic nanoparticles, followed by in situ derivatization in the injection port of a gas chromatograph coupled to triple quadrupole mass spectrometry. The use of uncoated or oleate-coated Fe3O4nanoparticles as sorbent in the extraction process was evaluated and compared. The main parameters involved in the extraction process were optimized applying experimental designs. Uncoated Fe3O4nanoparticles were selected in order to simplify and make more cost-effective the procedure. DLLME was carried out at pH 3, during 2 min, followed by the addition of the nanoparticles for D-μ-SPE employing 1 min in the extraction. Analysis of spiked water samples of different sources gave satisfactory recovery results for all the compounds with detection limits ranging from 7 to 180 ng l-1. Finally, the procedure was applied in tap, well, and river water. Graphical abstract Diagram of the extraction method using magnetic nanoparticles (MNPs).
Departamento de Medio Ambiente, Instituto Nacional de Investigación y Tecnología Agraria y Alimentaria (INIA), Carretera de la Coruña 7, 28040, Madrid, Spain. perez.rosana@inia.es.
Rosa Ana
RA
Pérez
Departamento de Medio Ambiente, Instituto Nacional de Investigación y Tecnología Agraria y Alimentaria (INIA), Carretera de la Coruña 7, 28040, Madrid, Spain.
Beatriz
B
Albero
Departamento de Medio Ambiente, Instituto Nacional de Investigación y Tecnología Agraria y Alimentaria (INIA), Carretera de la Coruña 7, 28040, Madrid, Spain.
José Luis
JL
Tadeo
Departamento de Medio Ambiente, Instituto Nacional de Investigación y Tecnología Agraria y Alimentaria (INIA), Carretera de la Coruña 7, 28040, Madrid, Spain.
Consuelo
C
Sánchez-Brunete
D052244:Endocrine Disruptors / Q000032:analysis*; D004784:Environmental Monitoring / Q000295:instrumentation / Q000379:methods*; D005618:Fresh Water / Q000737:chemistry*; D008401:Gas Chromatography-Mass Spectrometry; D059627:Liquid Phase Microextraction; D058185:Magnetite Nanoparticles / Q000737:chemistry*; D053719:Tandem Mass Spectrometry; D014874:Water Pollutants, Chemical / Q000032:analysis*
D052244:Endocrine Disruptors; D058185:Magnetite Nanoparticles; D014874:Water Pollutants, Chemical
Dispersive liquid–liquid microextraction; Endocrine-disrupting compounds; Gas chromatography–tandem mass spectrometry; Magnetic nanoparticles; Waters