Bioaccumulation assessment of the sunscreen agent 2-ethylhexyl 4-(N,N-dimethylamino)benzoate in human semen by automated online SPE-LC-MS/MS

• Published in: Analytical and bioanalytical chemistry Vol. 401; no. 3; pp. 1003 - 1011
• Main Authors: León-González, Zacarías, Ferreiro-Vera, Carlos, Priego-Capote, Feliciano, Luque de Castro, María Dolores
• Format: Journal Article
• Language: English
• Published: Berlin/Heidelberg Springer-Verlag 01.08.2011; Springer
• Subjects: 4-Aminobenzoic Acid - analysis; 4-Aminobenzoic Acid - metabolism; Analysis; Analytical Chemistry; Assessments; Bioaccumulation; Biochemistry; Characterization and Evaluation of Materials; Chemistry; Chemistry and Materials Science; Chromatographic methods and physical methods associated with chromatography; Chromatography, Liquid; Cytokinins; Exact sciences and technology; Food Science; Human; Humans; Laboratory Medicine; Male; Mathematical analysis; Metabolites; Molecular Structure; Monitoring/Environmental Analysis; On-line systems; Online; Original Paper; Other chromatographic methods; Reproducibility of Results; Semen; Semen - chemistry; Semen - metabolism; Solid Phase Extraction; Spectrometric and optical methods; Sunscreening Agents - analysis; Sunscreening Agents - metabolism; Sunscreens (Cosmetics); Tandem Mass Spectrometry; LC-MS/MS; Online solid-phase extraction; dimethylamino)benzoate; Sunscreen; Semen; Bioaccumulation; 2-Ethylhexyl 4-; ,; Solid phase extraction; Standard addition method; Chemical analysis; On line; Metabolite; Product; Calibration standards; Chemical enrichment; Detection limit; Standard deviation; Quantitative analysis; Human; Automation; 2-Ethylhexyl 4-(N,N-dimethylamino)benzoate; Sample; Use; Liquid chromatography; Matrix effect; Concentration; Automatic processing; Benzoate; Repeatability; Mass spectrometry MS/MS; Distribution; Analytical method; Application
• ISSN: 1618-2642; 1618-2650
• DOI: 10.1007/s00216-011-5141-x

The proven endocrine disruption nature of the sunscreen ingredient 2-ethylhexyl 4-( N , N -dimethylamino)benzoate (EDP) calls for research to understand its distribution and bioaccumulation in the human body. A sensitive analytical method to determine EDP and its metabolites in human semen based on online SPE-LC-MS/MS is described. The method has been fully validated and a standard addition calibration has been used for quantification to correct the observed matrix effects. The on-column detection limits of the analytes are between 0.2 and 0.6 ng, depending on the analyte and the sample. The repeatability of the method, expressed as relative standard deviation, was in the range 4.6–9.4%. The method was satisfactorily applied to semen samples from male volunteers who were subjected to single and repeated whole-body applications of an EDP-containing sunscreen product. EDP metabolites were found at different concentrations in semen samples from the repeated application study, thus showing evidences of bioaccumulation in humans.