Fast and simultaneous determination of endocrine disrupting compounds by ultra-high performance liquid chromatography–tandem mass spectrometry

A rapid and sensitive analytical method for the simultaneous determination of thirteen endocrine disruptors (five phthalates, seven parabens, and bisphenol A) in a single chromatographic run has been developed for the first time. The separation method, based on ultra-high performance liquid chromato...

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Bibliographic Details
Published in:Talanta (Oxford) 2016-01, Vol.146, p.326-334
Main Authors: Esteve, C., Herrero, L., Gómara, B., Quintanilla-López, J.E.
Format: Article
Language:English
Subjects:
Bisphenol A
Chromatography, High Pressure Liquid - methods
Cosmetics - chemistry
Endocrine Disruptors - analysis
Endocrine Disruptors - chemistry
Experimental design
Multicomponent method
Parabens
Phthalates
Tandem Mass Spectrometry - methods
Time Factors
Triple quadrupole tandem mass spectrometry
Ultra-high performance liquid chromatography
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Summary:A rapid and sensitive analytical method for the simultaneous determination of thirteen endocrine disruptors (five phthalates, seven parabens, and bisphenol A) in a single chromatographic run has been developed for the first time. The separation method, based on ultra-high performance liquid chromatography (UHPLC), allows the separation of all compounds (including isobaric pairs) in less than 4.1min. The fast polarity switching mode of the triple quadrupole mass spectrometer used enables the registration of positive (phthalates) and negative (parabens and BPA) ions in the same acquisition run. A Response Surface Methodology was used for the optimization of the method. The optimum elution program starts with 0.2min in isocratic conditions (79.8% water; 20% acetonitrile, 0.2% ammonium formate 5mM at pH 10.2), then the content of acetonitrile is linearly increased in 2min up to 42%, and later up to 98% in 1.1min. The analytical characteristics of the developed method were satisfactory. The method is robust and showed a linear response with determination coefficients (R2) higher than 0.991 in the range 5.0–2000pg on column (or higher) for all the compounds investigated. Instrumental intra- and inter-day precision (expressed as relative standard deviation) were lower than 12% for parabens and bisphenol A, and between 5.9% and 27% for phthalates. Instrumental detection and quantification limits (iLODs and iLOQs) were in the range of medium-high femtograms (270–1300pg on column for iLODs). Finally, the suitability of the developed method was demonstrated through its application to the analysis of commercial personal care products (shower gels) without any sample treatment, only a simple dilution, being possible to determine the simultaneous presence of phthalates, parabens, and bisphenol A in almost all the gels analyzed. [Display omitted] •Thirteen endocrine disruptors have been simultaneously determined by LC–MS/MS.•A Box–Wilson Central Composite Design was used for method optimization.•The developed LC–MS/MS method is fast (less than 4.1min) and sensitive.•Chromatographic separation for isobaric compounds was achieved.•Different commercial personal care products have been tested.
ISSN:0039-9140
1873-3573
DOI:10.1016/j.talanta.2015.08.064