Optimization and validation of organochlorine compounds in adipose tissue by SPE-gas chromatography

Biomed Chromatogr. 2012 Dec;26(12):1494-501. doi: 10.1002/bmc.2723. Epub 2012 Mar 8.

Abstract

Scientific evidence has shown an association between organochlorine compounds (OCC) exposure and human health hazards. Concerning this, OCC detection in human adipose samples has to be considered a public health priority. This study evaluated the efficacy of various solid-phase extraction (SPE) and cleanup methods for OCC determination in human adipose tissue. Octadecylsilyl endcapped (C₁₈-E), benzenesulfonic acid modified silica cation exchanger (SA), poly(styrene-divinylbenzene (EN) and EN/RP₁₈ SPE sorbents were evaluated. The relative sample cleanup provided by these SPE columns was evaluated using gas chromatography with electron capture detection (GC-ECD). The C₁₈-E columns with strong homogenization were found to provide the most effective cleanup, removing the greatest amount of interfering substance, and simultaneously ensuring good analyte recoveries higher than 70%. Recoveries > 70% with standard deviations (SD) < 15% were obtained for all compounds under the selected conditions. Method detection limits were in the 0.003-0.009 mg/kg range. The positive samples were confirmed by gas chromatography coupled with tandem mass spectrometry (GC-MS/MS). The highest percentage found of the OCC in real samples corresponded to HCB, o,p'-DDT and methoxychlor, which were detected in 80 and 95% of samples analyzed respectively.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Adipose Tissue / chemistry*
  • Aluminum Oxide / chemistry
  • Chromatography, Gas / methods*
  • Humans
  • Hydrocarbons, Chlorinated / analysis*
  • Limit of Detection
  • Pesticide Residues / analysis*
  • Reproducibility of Results
  • Solid Phase Extraction / methods*
  • Tandem Mass Spectrometry

Substances

  • Hydrocarbons, Chlorinated
  • Pesticide Residues
  • Aluminum Oxide