MSACL 2016 US Abstract

Determination of PBDEs in Human Milk by Automated Solid Phase Extraction and Gas Chromatography/High Resolution Mass Spectrometry

Weihong Guo (Presenter)
California Department of Toxic Substances Control

Bio: Weihong Guo is a research scientist at California Department of Toxic Substances Control, CalEPA.

Authorship: Weihong Guo, Arthur Holden, June-Soo Park, F. Reber Brown
California Department of Toxic Substances Control

Short Abstract

Although they have been banned since 2004, PBDEs are still ubiquitous in humans and in wildlife. Due to their possible adverse health effects, biomonitoring programs and research studies require that PBDEs be continuously measured in biological matrices including breast milk, serum, and tissue. We have developed a new method to determine PBDE levels in human milk that improves throughput, precision, and that reduces background contamination. This method has been validated using breast milk samples from an epidemiological study with high, medium, and low PBDE levels measured previously using the traditional method. PBDE levels from the two methods are in agreement.

Long Abstract

Although they have been banned since 2004, PBDEs are still ubiquitous in humans and in wildlife. Due to their possible adverse health effects in humans, biomonitoring programs and research studies require that PBDEs be continuously measured in biological matrices including breast milk, serum, and tissue. These measurements can provide important information such as PBDE body burden in reproductive female age group, assessment of infant PBDE daily exposures via breast milk, and the correlation of PBDE body burdens with various health outcomes in infants and mothers. Our laboratory’s traditional method of measuring PBDEs in freeze-dried breast milk was time consuming, of limited throughput, required extensive extraction equipment (freeze dryer, accelerated solvent extractor, gel permeation chromatograph), large volumes of solvents, and showed high background levels and poor precision.

We have developed a new method to determine PBDE levels in human milk that improves throughput and precision, reduces background contamination, and uses less solvent and less sample. Using automated Biotage® RapidTrace SPE modules (Biotage, Sweden), we achieved a much higher sample throughput. Breast milk samples (2 mL) were fortified with surrogate standards, extracted with Oasis®HLB cartridges (3 cc, Waters, USA), and cleaned up in two stages using manually packed: 1) acidified silica/activated silica/sodium sulfate; and 2) potassium silicate/acidified silica/Florisil cartridges (3cc) on a Biotage® RapidTrace system. PBDE congeners were separated on a DB-5MS column (15 m x 0.25 mm I.D. x 0.1 ìm film thickness, Agilent J&W, USA) and analyzed by high resolution mass spectrometry using isotope dilution (GC–HRMS, ThermoFisher, Bremen, Germany). When compared with our previous method, this method has lower detection limits, reduced background, and higher precision and accuracy. In addition, this method has been validated using breast milk samples from an epidemiological study with high, medium, and low PBDE levels measured previously using the traditional method. PBDE levels from the two methods are in agreement.


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