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

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

Talanta (2015-12-24)
C Esteve, L Herrero, B Gómara, J E Quintanilla-López
ABSTRACT

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 4.1 min. 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 0.2 min 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 2 min up to 42%, and later up to 98% in 1.1 min. The analytical characteristics of the developed method were satisfactory. The method is robust and showed a linear response with determination coefficients (R(2)) higher than 0.991 in the range 5.0-2000 pg 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 (270-1300 pg 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.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Methanol, suitable for NMR (reference standard)
Sigma-Aldrich
Acetone, ≥99%, meets FCC analytical specifications
Sigma-Aldrich
Acetone, natural, ≥97%
Sigma-Aldrich
Ammonium formate, ≥99.995% trace metals basis
Sigma-Aldrich
Benzyl 4-hydroxybenzoate, 99%
Sigma-Aldrich
Methanol, anhydrous, 99.8%
Sigma-Aldrich
Ammonia-14N, 99.99 atom % 14N
Sigma-Aldrich
Methanol, purification grade, 99.8%
Sigma-Aldrich
Acetone, ACS reagent, ≥99.5%
Sigma-Aldrich
Acetone, Laboratory Reagent, ≥99.5%
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Ammonium formate, reagent grade, 97%
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, ACS spectrophotometric grade, ≥99.9%
Sigma-Aldrich
Acetone, ACS reagent, ≥99.5%
Sigma-Aldrich
Methanol, Laboratory Reagent, ≥99.6%
Sigma-Aldrich
Acetone, puriss., meets analytical specification of Ph. Eur., BP, NF, ≥99% (GC)
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.8% (GC)
Sigma-Aldrich
Acetone, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.5% (GC)
Sigma-Aldrich
Methanol, puriss., meets analytical specification of Ph Eur, ≥99.7% (GC)
Sigma-Aldrich
Methanol, BioReagent, ≥99.93%
Sigma-Aldrich
Acetone, histological grade, ≥99.5%
Sigma-Aldrich
Ammonium formate solution, BioUltra, 10 M in H2O
Sigma-Aldrich
Dichloromethane, anhydrous, ≥99.8%, contains 40-150 ppm amylene as stabilizer
Supelco
Bisphenol A, ≥99%
Sigma-Aldrich
Bisphenol A, 97%
Sigma-Aldrich
Formic acid, ≥95%, FCC, FG
Sigma-Aldrich
Hexane, anhydrous, 95%
Sigma-Aldrich
Dichloromethane, suitable for HPLC, ≥99.9%, contains 40-150 ppm amylene as stabilizer