The determination of perfluoroalkyl substances, brominated flame retardants and their metabolites in human breast milk and infant formula

Talanta. 2013 Dec 15:117:318-25. doi: 10.1016/j.talanta.2013.08.040. Epub 2013 Aug 30.

Abstract

In the present study, a novel analytical approach for the simultaneous determination of 18 perfluoroalkyl substances (PFASs) and 11 brominated flame retardants (BFRs) including their hydroxylated metabolites and brominated phenols has been developed and validated for breast milk and infant formula. The sample preparation procedure based on extraction using acetonitrile and subsequent purification by dispersive solid-phase extraction (d-SPE) employing C18 sorbent is rapid, simple and high-throughput. Ultra-high performance liquid chromatography (UHPLC) interfaced with a tandem mass spectrometry (MS/MS) was employed for the identification/quantification of these compounds. The method recoveries of target compounds for both matrices ranged from 80% to 117% with relative standard deviations lower than 28% and quantification limits in the range of 3-200 pg/mL for milk and 5-450 pg/g for infant formula. Within the pilot study, the new method was used for the analysis of PFASs and BFRs in 50 human breast milks and six infant formulas. In the breast milk samples the total contents of PFASs and BFRs were in the range of 38-279 and 45-16,200 pg/mL, respectively. The most abundant PFASs detected in all tested breast milk samples were perfluorooctanoic acid (PFOA) and perfluorooctanesulfonate (PFOS), the latter contaminant was present not only as a linear form but also as a branched isomers. The incidence of BFRs was lower, the only representatives of this group, tetrabromobiphenol A (TBBPA) and α-hexabromocyclododecane (α-HBCD), were detected in less than 30% of breast milk samples. None of the infant formulas contained BFRs, traces of either PFOS, PFOA or PFNA were found in three samples.

Keywords: BFRs; HBCDs; Human milk; LC–MS/MS; PFASs; TBBPA.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Acetonitriles / chemistry
  • Alkanesulfonic Acids / analysis*
  • Caprylates / analysis*
  • Chromatography, High Pressure Liquid
  • Female
  • Flame Retardants / analysis*
  • Fluorocarbons / analysis*
  • Humans
  • Hydrocarbons, Brominated / analysis*
  • Infant
  • Infant Formula / chemistry*
  • Limit of Detection
  • Milk, Human / chemistry*
  • Polybrominated Biphenyls / analysis*
  • Solid Phase Extraction
  • Tandem Mass Spectrometry

Substances

  • Acetonitriles
  • Alkanesulfonic Acids
  • Caprylates
  • Flame Retardants
  • Fluorocarbons
  • Hydrocarbons, Brominated
  • Polybrominated Biphenyls
  • hexabromocyclododecane
  • perfluorooctanoic acid
  • perfluorooctane sulfonic acid
  • tetrabromobisphenol A
  • acetonitrile