Multiresidue determination of endosulfan and metabolic derivatives in human adipose tissue using automated liquid chromatographic cleanup and gas chromatographic analysis.
A multiresidue method based on normal-phase liquid chromatography (LC) cleanup and gas chromatography-electron capture detection-mass selective detection (GC-ECD-MSD) analysis has been developed for the determination of endosulfan and its main metabolic derivatives in human adipose tissues. Analytes were extracted by dissolving the fat samples in n-hexane, and the hexanic extracts were directly injected onto the silicagel column of the automated LC cleanup system. Purified LC extracts were analyzed by GC-ECD or GC-MSD, without any solvent exchanges or preconcentration steps. The high efficiency of the high-performance liquid chromatographic cleanup for the elimination of fats allowed to reach detection limits for all analytes at low nanograms-per-gram concentration levels. The optimized overall analytical procedure was applied to 18 selected human mammary adipose and abdominal fat tissue samples. p,p'-DDE, hexachlorobenzene, and beta-HCH were the most frequently detected compounds, and residues of endosulfan-sulfate and -ether were also found in several samples. All findings were confirmed by an additional GC-MS-MS analysis of the LC sample extracts.
Hernández
F
F
Analytical Chemistry, Dept. Experimental Sciences, University Jaume I, Castellón, Spain. hernandf@exp.uji.es
Pitarch
E
E
Serrano
R
R
Gaspar
J V
JV
Olea
N
N
D000273:Adipose Tissue / Q000737:chemistry* / Q000378:metabolism; D000328:Adult; D000368:Aged; D002853:Chromatography, Liquid / Q000295:instrumentation / Q000379:methods*; D004726:Endosulfan / Q000032:analysis* / Q000493:pharmacokinetics; D005260:Female; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D006843:Hydrocarbons, Chlorinated; D007306:Insecticides / Q000032:analysis* / Q000493:pharmacokinetics; D008875:Middle Aged; D015203:Reproducibility of Results
D006843:Hydrocarbons, Chlorinated; D007306:Insecticides; D004726:Endosulfan