In rural parts of South Africa the organochlorine insecticide DDT (1,1,1-trichloro-2,2-bis(p-chlorophenyl)ethane) is still used for malaria vector control where traditional dwellings are sprayed on the inside with small quantities of technical DDT. Since o,p'-DDT may show enantioselective oestrogenicity and biodegradability, it is important to analyse enantiomers of o,p'-DDT and its chiral degradation product, o,p'-DDD, for both health and environmentalforensic considerations. Generally, chiral analysis is performed using heartcut multidimensional gas chromatography (MDGC) and, more recently, comprehensive two-dimensional gas chromatography (GC x GC). We developed an off-line gas chromatographic fraction collection (heart-cut) procedure for the selective capturing of the appropriate isomers from a first