Optimization and validation of organochlorine compounds in adipose tissue by SPE‐gas chromatography |
| |
Authors: | Rosário Monteiro Gil Faria Manuela Meireles Luísa Correia‐Sá Diana Teixeira Ana Faria Conceição Calhau Valentina F. Domingues Cristina Delerue‐Matos |
| |
Affiliation: | 1. Department of Biochemistry (U38‐FCT), Faculty of Medicine, University of Porto, , Portugal;2. General Surgery Department, S. Jo?o Hospital, Faculty of Medicine, University of Porto, , Portugal;3. Requimte, Instituto Superior de Engenharia, Instituto Politécnico do Porto, , 4200‐072 Porto, Portugal;4. Faculty Nutrition and Food Sciences, University of Porto, , Porto, Portugal;5. CIQ – Faculdade de Ciência da Universidade do Porto‐Departamento de Qu?ímica, , 4169‐007 Porto, Portugal |
| |
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. Copyright © 2012 John Wiley & Sons, Ltd. |
| |
Keywords: | organochlorine pesticides TCDD SPE GC‐ECD GC‐MS/MS adipose tissue |
|
|