title: Gas chromatography and ultra high performance liquid chromatography tandem mass spectrometry methods for the determination of selected endocrine disrupting chemicals in human breast milk after stir-bar sorptive extraction.
abstract: In the present work, two specific, accurate and sensitive methods for the determination of endocrine disrupting chemicals (EDCs) in human breast milk are developed and validated. Bisphenol A and its main chlorinated derivatives, five benzophenone-UV filters and four parabens were selected as target analytes. The method involves a stir-bar sorptive extraction (SBSE) procedure followed by a solvent desorption prior to GC-MS/MS or UHPLC-MS/MS analysis. A derivatization step is also necessary when GC analysis is performed. The GC column used was a capillary HP-5MS with a run time of 26min. For UHPLC analysis, the stationary phase was a non-polar Acquity UPLC(®) BEH C18 column and the run time was 10min. In both cases, the analytes were detected and quantified using a triple quadrupole mass spectrometer (QqQ). Quality parameters such as linearity, accuracy (trueness and precision), sensitivity and selectivity were examined and yielded good results. The limits of quantification (LOQs) ranged from 0.3 to 5.0ngmL(-1) for GC and from 0.2 to 1.0ngmL(-1) for LC. The relative standard deviation (RSD) was lower than 15% and the recoveries ranged from 92 to 114% in all cases, being slightly unfavorable the results obtained with LC. The methods were satisfactorily applied for the determination of target compounds in human milk samples from 10 randomly selected women.
authors.affiliation: Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, University of Granada, Campus of Fuentenueva, E-18071 Granada, Spain.
authors.forename: R
authors.initials: R
authors.lastname: Rodríguez-Gómez
authors.affiliation: Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, University of Granada, Campus of Fuentenueva, E-18071 Granada, Spain. Electronic address: azafra@ugr.es.
authors.forename: A
authors.initials: A
authors.lastname: Zafra-Gómez
authors.affiliation: Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, University of Granada, Campus of Fuentenueva, E-18071 Granada, Spain.
authors.forename: F J
authors.initials: FJ
authors.lastname: Camino-Sánchez
authors.affiliation: Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, University of Granada, Campus of Fuentenueva, E-18071 Granada, Spain.
authors.forename: O
authors.initials: O
authors.lastname: Ballesteros
authors.affiliation: Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, University of Granada, Campus of Fuentenueva, E-18071 Granada, Spain.
authors.forename: A
authors.initials: A
authors.lastname: Navalón
mesh_terms: D001559:Benzhydryl Compounds / Q000032:analysis; D001577:Benzophenones / Q000032:analysis; D002623:Chemistry Techniques, Analytical / Q000379:methods* / Q000592:standards; D052244:Endocrine Disruptors / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry; D006801:Humans; D008895:Milk, Human / Q000737:chemistry*; D010226:Parabens / Q000032:analysis; D010636:Phenols / Q000032:analysis; D015203:Reproducibility of Results; D000098826:Bisphenol A Compounds
chemical_list: D001559:Benzhydryl Compounds; D001577:Benzophenones; D052244:Endocrine Disruptors; D010226:Parabens; D010636:Phenols; C006780:bisphenol A; D000098826:Bisphenol A Compounds
keywords: Endocrine disrupting chemicals; GC–MS/MS; Human breast milk; Stir-bar sorptive extraction; UHPLC–MS/MS