Abstract

A published method for separation of the 22 tetrachlorodibenzo- p-dioxin (TCDD) isomers by high-performance liquid chromatography (HPLC)—gas chromatography (GC) was modified to improve the recovery and chromatographic resolution of individual isomers. For the first step, reversed-phase HPLC, minor changes were made in column temperature (50 to 40°C, to prolong column life) and in injection solvent (chloroform to benzene, to avoid photodecomposition). For the second step, normal-phase HPLC, the silica gel columns were used in a less active state, and 0.4% toluene was added to the hexane eluent as a polar orgnaic modifier. Resolution of the 22 isomers was significantly improved by this change of solvent system, and recovery of subnanogram quantities of TCDDs from the silica gel columns was increased from 20 to 80%. For the final step a capillary GC column (OV-275) was used in place of a packed column.

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