Optimization and application of SPME for the gas chromatographic determination of endosulfan and its major metabolites in the ng L-1 range in aqueous solutions

Deger, A. B.; Gremm, T. J.; Frimmel, F. H.; Mendez, L.
May 2003
Analytical & Bioanalytical Chemistry;May2003, Vol. 376 Issue 1, p61
Academic Journal
In the present study an analytical method was optimized for the determination of α-endosulfan, β-endosulfan, endosulfan sulfate, endosulfan ether and endosulfan lactone in small volumes of environmental aqueous samples using solid-phase microextraction (SPME) and gas chromatography–electron capture detection (GC–ECD). A 100 µm polydimethylsiloxane (PDMS) phase was used for the extraction. The limit of detection (LOD) for the analytes varied between 0.01 and 0.03 µg L-1 with a relative standard deviation of 3 to 11%. The influence of the ionic strength on the extraction efficiency was investigated for the individual compounds. α-Endosulfan, β-endosulfan, endosulfan sulfate and endosulfan ether were extracted successfully without salt addition. The extraction efficiency of endosulfan lactone was improved with 30% NaCl content. A general decrease in extraction efficiency for α-endosulfan, β-endosulfan, endosulfan sulfate and endosulfan ether with high NaCl content (20–30%) in the solution was observed due to glass surface adsorption. No effect of dissolved organic material (DOM) on the extraction efficiency was observed. The extraction coefficients changed between Log K=2.17 and 3.33. A sample from the Antarctic region was analyzed using the optimized GC–ECD/SPME method. To confirm the results obtained for the real sample a GC with a mass spectrometer (MS) was used. Endosulfan sulfate, the most toxic metabolite of endosulfan, was found in the sample at a concentration of 0.3 µg L-1.


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