Multidimensional Gas Chromatographic Analysis of Toxaphene

Abstract

The pesticide toxaphene with a total worldwide production of 1.3 Mt is found in the aquatic environment with a widespread, global distribution. Its analysis is difficult due to its complex character. A technical toxaphene mixture and a number of biological samples were analyzed by multidimensional gas chromatography (MDGC). Four different column combinations were used: DB5/DX4, DB5/FFAP, Ultra 2/DX4, and Ultra 2/Rtx 2330. The technical mixture consists of at least 246 congeners, while only 107 peaks were found in a one-dimensional GC/ECD chromatogram. The major peaks present in the technical mixture and biological samples mostly consist of 2-10 toxaphene congeners. These results show that in most cases single-column chromatography is not suitable for a congener-specific determination of the toxaphene congeners. The Rtx 2330 column is recommended as the best choice as a second column in MDGC of toxaphene, particularly because of its stability at higher temperatures and because of a slightly better separation, although the differences in results obtained with the different column combinations were relatively small. The relatively high concentrations of toxaphene in European fish, which may even lead to exceeding the tolerance levels for human consumption, and in marine mammals demand a proper monitoring of total toxaphene and individual CHBs in relevant samples from European aquatic ecosystems.

Comprehensive Two-Dimensional Gas Chromatography with a Rotating Thermal Desorption Modulator and Independently Temperature-Programmable Columns

“…A second fraction was eluted with 12 mL diethyl ether:iso-octane (20:80, v/v). This fraction contained the bulk of toxaphene (›95%) [9].…”

Environmental Occurrence, Analysis, and Toxicology of Toxaphene Compounds

“…However, this approach can only be used successfully when the indicator compounds do not coelute with other compounds. Coelution of suggested indicator compounds was shown by heart-cut multidimensional gas chromatography (69 …”

Determination of Enantiomer Ratios of Bornane Congeners in Biological Samples Using Heart-Cut Multidimensional Gas Chromatography

“…The samples were extracted and cleaned-up according to de Boer et al [8]. This method included 6.5 h Soxhlet extraction with npentane/dichloromethane (1 : 1, v/v), alumina column chromatography with n-pentane and silica gel column fractionation.…”

“…Relevant parts of the first separation are transferred to a second column for further resolution. This technique offers a higher separation power than single-column GC and has successfully been used to reveal co-elution in toxaphene-contain-ing samples [8]. For the determination of enantiomer ratios an isomer-specific pre-separation on the first column can be combined with an enantioselective separation on the second one.…”