Measurement of selected polybrominated diphenyl ethers, polybrominated and polychlorinated biphenyls, and organochlorine pesticides in human serum and milk using comprehensive two-dimensional gas chromatography isotope dilution time-of-flight mass spectrometry

Jean François Focant, Andreas Sjödin, Wayman I. Turner, Donald G. Patterson

Research output: Contribution to journalArticlepeer-review

110 Scopus citations

Abstract

A new method using comprehensive two-dimensional gas chromatography and isotope dilution time-of-flight mass spectrometry (GCxGC-IDTOFMS) for the simultaneous measurement of selected polychlorinated biphenyls (PCBs), organochlorine pesticides (OCPs), and brominated flame retardants is presented. In contrast to the reference methods based on classical GC/MS, a single injection of the extract containing all compounds of interest results in accurate identification and quantification. Using GCxGC ensures the Chromatographic separation of most compounds, and TOFMS allows mass spectral deconvolution of coeluting compounds as well as the use of 13C- labeled internal standards for quantification. Isotope ratio measurements of the most intense ions for both native and labels ensure the required specificity. The use of this new method with an automated sample preparation procedure developed at the Centers for Disease Control and Prevention (CDC) for the analysis of human serum and milk compared favorably to conventional isotope-dilution one-dimensional gas chromatography-high-resolution mass spectrometry (GC-IDHRMS) for the different human serum and milk pools tested. The instrumental detection limits ranged between 0.5 pg/μL and 10 pg/μL and the method detection limits ranged between 1 and 15 pg/μL (N = 59 analytes). The reproducibility of the method was almost as good as with GC-IDHRMS, the relative standard deviations ranging between 1 and 11% for OCPs measured in human serum. OCP, PBDE, and PCB levels measured using the two methods were highly correlated, and the deviations between the two methods were below 20% for most analytes with concentrations above 1 ng/g milk lipids.

Original languageEnglish (US)
Pages (from-to)6313-6320
Number of pages8
JournalAnalytical chemistry
Volume76
Issue number21
DOIs
StatePublished - Nov 1 2004

All Science Journal Classification (ASJC) codes

  • Analytical Chemistry

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