Quantitative solid phase microextraction - gas chromatography mass spectrometry analysis of the pesticides lindane, heptachlor and two heptachlor transformation products in groundwater.

This paper describes the development and validation of a method for the determination of lindane, heptachlor and two heptachlor transformation products (exo- and endo-heptachlor epoxide) in groundwater. Samples were extracted using a simple solid phase microextraction (SPME) method with a polyacrylate fibre prior to detection by gas chromatography mass spectrometry in electron impact ionisation mode (GC-EI-MS). The linearity of the method ranged from 0.015 to 5.0 µg L(-1), with correlation coefficients greater than 0.99. Recoveries ranged from 96 to 101% at several fortification levels with all coefficients of variation (CV%) less than 10.5%. The method was validated to the permitted limits laid down in the European Union drinking water directive (98/83/EC). The limit of quantitation (LOQ) was 0.015 µg L(-1) in groundwater samples. Samples had to be analysed within 24h of collection otherwise degradation occurred and disposable SPME polyacrylate fibres lasted up to 51 injections. Both endo-heptachlor epoxide and lindane were detected in groundwater samples with concentrations ranging between 0.033 and 0.048 µg L(-1).

Liquid chromatographic separation of the enantiomers of trans-chlordane, cis-chlordane, heptachlor, heptachlor epoxide and alpha-hexachlorocyclohexane with application to small-scale preparative separation.

Analytical high-performance liquid chromatographic separations of the individual enantiomers of five polychlorinated compounds were obtained on polysaccharide stereoselective HPLC columns. The enantiomers of the pesticides trans-chlordane, cis-chlordane and heptachlor were separated on CHIRALCEL OD using a hexane mobile phase. The enantiomers of the heptachlor metabolite, heptachlor epoxide, were separated on CHIRALPAK AD using a methanol mobile phase. The enantiomers of alpha-hexachlorocyclohexane (alpha-HCH), were separated on CHIRALCEL OJ using a hexane/2-propanol mobile phase. Similar chromatographic conditions using preparative columns were used to isolate approximately 250 mg of each of the individual enantiomers. The purified individual enantiomers have been submitted for testing of their endocrine disruptor (ED) activity.

Organochlorinated pesticides in the Argentine Antarctic sector and Atlantic coastline waters.

The presence of organochlorinated pesticides in water samples drawn in the Argentine Antarctic Sector and Atlantic coastline has been proved. In general, these samples showed quantities that varied between a few hundredths of a ppmm to slightly more than 1 ppmm, although in some cases and for certain pesticides, depending on the locations, the levels found were definitely higher. With the exception of Dieldrin, which appeared in only one sample/in what would seem to be its course few hundredths of a ppm, to slightly more than 1 ppmm, although in some cases and for certain pesticides found were the same as those reported in previous investigations. The isolated cases of high pesticide contents in water samples drawn at wharves and of snow in the vicinity of Almirante Brown Base show up clearly the influence of human activity on the contamination of the environment.