title: Application of a fast and cost-effective in situ derivatization method prior to gas chromatography with mass spectrometry to monitor endocrine disruptors in water matrices.
abstract: This work deals with the optimization of a rapid, cost-effective, and eco-friendly gas chromatography with mass spectrometry method for the simultaneous determination of four endocrine disruptor compounds in water matrices: estrone, 17β-estradiol, 17α-ethinylestradiol, and bisphenol A, that are currently considered to be of main concern in the field of water policy and that could became candidates for future regulations. The method involves simultaneous derivatization and extraction of compounds by dispersive liquid-liquid microextraction followed by gas chromatography with mass spectrometry analysis. Derivatization and extraction parameters were optimized with the aid of experimental design approach. An excellent linear response was achieved for all analytes (r(2) ≥ 0.999). Limits of detection and quantification are 0.003-0.005 and 0.0094-0.0164 μg/L, respectively. Intraday precision ranged between 1.1 and 12.6%, whereas interday precision ranged between 0.5 and 14.7%. For accuracy, bias values varied between -15.0 and 13.7%. Recoveries at three concentration levels ranged from 86.4 to 118.2%. The proposed method can be applied to the routine analysis of groundwater, river, sea, tap, and mineral water samples with excellent sensitivity, precision, and accuracy.
authors.affiliation: REQUIMTE/Departamento de Ciências Químicas, Laboratório de Bromatologia e Hidrologia, Faculdade de Farmácia-Universidade do Porto, Portugal.|Departamento de Saúde Ambiental, Instituto Nacional de Saúde Doutor Ricardo Jorge, Porto, Portugal.
authors.forename: Armindo
authors.initials: A
authors.lastname: Melo
authors.affiliation: REQUIMTE/Departamento de Ciências Químicas, Laboratório de Bromatologia e Hidrologia, Faculdade de Farmácia-Universidade do Porto, Portugal.
authors.forename: Isabel M P L V O
authors.initials: IM
authors.lastname: Ferreira
authors.affiliation: Departamento de Saúde Ambiental, Instituto Nacional de Saúde Doutor Ricardo Jorge, Porto, Portugal.|REQUIMTE, Universidade do Porto, Porto, Portugal.
authors.forename: Catarina
authors.initials: C
authors.lastname: Mansilha
mesh_terms: D003362:Cost-Benefit Analysis; D052244:Endocrine Disruptors / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D011786:Quality Control; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D052244:Endocrine Disruptors; D014874:Water Pollutants, Chemical
keywords: Derivatization; Dispersive liquid-liquid microextraction; Endocrine disruptors; Experimental design; Water