title: Determination of benzophenone-UV filters in human milk samples using ultrasound-assisted extraction and clean-up with dispersive sorbents followed by UHPLC-MS/MS analysis.
abstract: A new sample preparation method for the determination of five benzophenone UV-filters in human breast milk has been developed. The procedure involves the lyophilization of the sample, and its subsequent extraction by ultrasound sonication using acetonitrile. In order to reduce matrix effects produced by milk components that are coextracted, mainly proteins, sugars and lipids, a further clean-up step with a mixture of dispersive-SPE sorbents, C18 and PSA, was applied. Extraction parameters were optimized using experimental design, and the compounds were detected and quantified by ultrahigh performance liquid-chromatography tandem mass spectrometry (UHPLC-MS/MS) in positive ESI mode. Analytes were separated in 10 min. BP-d10 was used as internal standard. The limits of detection (LODs) were between 0.1 and 0.2 ng mL(-1), and the limits of quantification (LOQs) were between 0.3 and 0.6 ng mL(-1) for the target analytes. The inter- and intra-day variability was <12%. The method was validated using matrix-matched calibration and recovery assays with spiked samples. Recovery rates were between 90.9 and 109.5%. The method was successfully applied for the determination of these compounds in human milk samples collected from volunteers lactating mothers with no known occupational exposure to these compounds who live in the province of Granada (Spain). The analytical method developed here may be useful for the development of more in-depth studies on the prenatal exposure and biomonitoring of these commonly used UV-filters.
authors.affiliation: Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, Campus of Fuentenueva, University of Granada, 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, Campus of Fuentenueva, University of Granada, 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, Campus of Fuentenueva, University of Granada, E-18071 Granada, Spain.
authors.forename: N
authors.initials: N
authors.lastname: Dorival-García
authors.affiliation: Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, Campus of Fuentenueva, University of Granada, 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, Campus of Fuentenueva, University of Granada, E-18071 Granada, Spain.
authors.forename: A
authors.initials: A
authors.lastname: Navalón
mesh_terms: D000327:Adsorption; D001577:Benzophenones / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D005260:Female; D006801:Humans; D008895:Milk, Human / Q000737:chemistry*; D021241:Spectrometry, Mass, Electrospray Ionization; D013473:Sunscreening Agents / Q000032:analysis*; D053719:Tandem Mass Spectrometry; D014465:Ultrasonics
chemical_list: D001577:Benzophenones; D013473:Sunscreening Agents; C047723:benzophenone
keywords: Benzophenone-UV filters; Human breast milk analysis; Sorbent materials; UHPLC–MS/MS; Ultrasound-assisted extraction