Determination of endocrine-disrupting compounds in water samples by magnetic nanoparticle-assisted dispersive liquid-liquid microextraction combined with gas chromatography-tandem mass spectrometry. 2016

Rosa Ana Pérez, and Beatriz Albero, and José Luis Tadeo, and Consuelo Sánchez-Brunete
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.

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 Fe3O4 nanoparticles as sorbent in the extraction process was evaluated and compared. The main parameters involved in the extraction process were optimized applying experimental designs. Uncoated Fe3O4 nanoparticles 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).

UI MeSH Term Description Entries
D008401 Gas Chromatography-Mass Spectrometry A microanalytical technique combining mass spectrometry and gas chromatography for the qualitative as well as quantitative determinations of compounds. Chromatography, Gas-Liquid-Mass Spectrometry,Chromatography, Gas-Mass Spectrometry,GCMS,Spectrometry, Mass-Gas Chromatography,Spectrum Analysis, Mass-Gas Chromatography,Gas-Liquid Chromatography-Mass Spectrometry,Mass Spectrometry-Gas Chromatography,Chromatography, Gas Liquid Mass Spectrometry,Chromatography, Gas Mass Spectrometry,Chromatography, Mass Spectrometry-Gas,Chromatography-Mass Spectrometry, Gas,Chromatography-Mass Spectrometry, Gas-Liquid,Gas Chromatography Mass Spectrometry,Gas Liquid Chromatography Mass Spectrometry,Mass Spectrometry Gas Chromatography,Spectrometries, Mass-Gas Chromatography,Spectrometry, Gas Chromatography-Mass,Spectrometry, Gas-Liquid Chromatography-Mass,Spectrometry, Mass Gas Chromatography,Spectrometry-Gas Chromatography, Mass,Spectrum Analysis, Mass Gas Chromatography
D004784 Environmental Monitoring The monitoring of the level of toxins, chemical pollutants, microbial contaminants, or other harmful substances in the environment (soil, air, and water), workplace, or in the bodies of people and animals present in that environment. Monitoring, Environmental,Environmental Surveillance,Surveillance, Environmental
D005618 Fresh Water Water containing no significant amounts of salts, such as water from RIVERS and LAKES. Freshwater,Fresh Waters,Freshwaters,Water, Fresh,Waters, Fresh
D014874 Water Pollutants, Chemical Chemical compounds which pollute the water of rivers, streams, lakes, the sea, reservoirs, or other bodies of water. Chemical Water Pollutants,Landfill Leachate,Leachate, Landfill,Pollutants, Chemical Water
D052244 Endocrine Disruptors Exogenous agents, synthetic and naturally occurring, which are capable of disrupting the functions of the ENDOCRINE SYSTEM including the maintenance of HOMEOSTASIS and the regulation of developmental processes. Endocrine disruptors are compounds that can mimic HORMONES, or enhance or block the binding of hormones to their receptors, or otherwise lead to activating or inhibiting the endocrine signaling pathways and hormone metabolism. Endocrine Disrupting Chemical,Endocrine Disrupting Chemicals,Endocrine Disruptor,Endocrine Disruptor Effect,Endocrine Disruptor Effects,Chemical, Endocrine Disrupting,Chemicals, Endocrine Disrupting,Disrupting Chemical, Endocrine,Disruptor Effect, Endocrine,Disruptor Effects, Endocrine,Disruptor, Endocrine,Disruptors, Endocrine,Effect, Endocrine Disruptor,Effects, Endocrine Disruptor
D053719 Tandem Mass Spectrometry A mass spectrometry technique using two (MS/MS) or more mass analyzers. With two in tandem, the precursor ions are mass-selected by a first mass analyzer, and focused into a collision region where they are then fragmented into product ions which are then characterized by a second mass analyzer. A variety of techniques are used to separate the compounds, ionize them, and introduce them to the first mass analyzer. For example, for in GC-MS/MS, GAS CHROMATOGRAPHY-MASS SPECTROMETRY is involved in separating relatively small compounds by GAS CHROMATOGRAPHY prior to injecting them into an ionization chamber for the mass selection. Mass Spectrometry-Mass Spectrometry,Mass Spectrometry Mass Spectrometry,Mass Spectrometry, Tandem
D058185 Magnetite Nanoparticles Synthesized magnetic particles under 100 nanometers used in many biomedical applications including DRUG DELIVERY SYSTEMS and CONTRAST AGENTS. The particles are usually coated with a variety of polymeric compounds. Magnetite SPIONs,Magnetite Superparamagnetic Iron Oxide Nanoparticles,Superparamagnetic Magnetite Nanoparticles,Magnetite Nanoparticle,Magnetite Nanoparticle, Superparamagnetic,Magnetite Nanoparticles, Superparamagnetic,Magnetite SPION,Nanoparticle, Magnetite,Nanoparticle, Superparamagnetic Magnetite,Nanoparticles, Magnetite,Nanoparticles, Superparamagnetic Magnetite,SPION, Magnetite,SPIONs, Magnetite,Superparamagnetic Magnetite Nanoparticle
D059627 Liquid Phase Microextraction Miniaturized methods of liquid-liquid extraction. Liquid-Liquid Microextraction,Micro Liquid Phase Extraction,Micro Liquid-Liquid Extraction,Extraction, Micro Liquid-Liquid,Extractions, Micro Liquid-Liquid,Liquid Liquid Microextraction,Liquid Phase Microextractions,Liquid-Liquid Extraction, Micro,Liquid-Liquid Extractions, Micro,Liquid-Liquid Microextractions,Micro Liquid Liquid Extraction,Micro Liquid-Liquid Extractions,Microextraction, Liquid Phase,Microextraction, Liquid-Liquid,Microextractions, Liquid Phase,Microextractions, Liquid-Liquid,Phase Microextraction, Liquid,Phase Microextractions, Liquid

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