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Determination of Human Metabolites of Chlorinated Phosphorous Flame Retardants in Wastewater by N-tert-butyldimethylsilyl-N-methyltrifluoroacetamide-derivatization and Gas Chromatography-High Resolution Mass Spectrometry

Determination of Human Metabolites of Chlorinated Phosphorous Flame Retardants in Wastewater by N-tert-butyldimethylsilyl-N-methyltrifluoroacetamide-derivatization and Gas Chromatography-High Resolution Mass Spectrometry

Verónica Castro, Rosario Rodil, José Benito Quintana, Rafael Cela, Laura Sánchez-Fernández, Iria González-Mariño

J Chromatogr A. 2019 Sep 27;1602:450-457.

PMID: 31208794

Abstract:

The analysis of wastewater for the determination of human biomarkers of exposure (human metabolites) is a non-intrusive, economic and complementary alternative to the analysis of urine in the monitoring of human exposure to chemicals of concern. This study provides the first gas chromatography-based method for the determination of three metabolites of chlorinated organophosphorous flame retardants (OPFRs: bis(2-chloroethyl) phosphate, bis(chloropropyl) phosphate and bis(1,3-dichloro-2-propyl) phosphate) in wastewater. A solid-phase extraction procedure based on the use of mixed-mode reversed-phase weak anion exchange sorbents was optimized including a fractionated elution of OPFRs and their metabolites. Analytes derivatization was investigated by comparing two silylating reagents, N-tert-butyldimethylsilyl-N-methyltrifluoroacetamide and N-methyl-N-(trimethylsilyl)trifluoroacetamide, the first one providing better results. Determination was performed by gas chromatography-high resolution mass spectrometry with a quadrupole-time-of-flight system (GC-QTOF) in order to improve selectivity. Furthermore, the use of GC-QTOF combined with the specific ion obtained from silylated metabolites (m/z 154.9924) can be exploited to screen for other phosphate ester metabolites. Under final conditions, the overall method performance was satisfactory, affording method detection limits ranging from 1.1 to 4.6 ng/L, percentages of recovery from 90% to 110%, and relative standard deviations below 13%. The analysis of composite raw wastewater samples collected over 24 h in the NW of Spain allowed to quantify, for the first time in this matrix, the metabolite bis(chloropropyl) phosphate at levels over 60 ng/L.

Chemicals Related in the Paper:

Catalog Number	Product Name	Structure	CAS Number	Price
AP77377527-B	N-tert-Butyldimethylsilyl-N-methyltrifluoroacetamide		77377-52-7	Price

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