Abstract

The influence of the freeze-drying process on the recovery of 12 chlorobiphenyl standards spiked in a wet candidate reference material (mussel) was investigated. Losses of spiked amounts tended to reduce with increasing number of chlorine atoms in the molecule. The aqueous phase in wet materials in combination with small volumes of organic solvents introduced by spiking may serve as an intermediate in the loss processes observed during freeze-drying, facilitating differential losses of spiked surrogate standards as well as analytes originally present in the material. Overall losses will be determined both by the amount of polychlorinated biphenyls stored in the aqueous phase (solubility) and by evaporation from the aqueous and tissue phases (vapour pressure) in a kinetic and complex way. Hence, recovery figures for surrogate standards thus obtained may lead to an overestimation of the actual efficiency of the analytical procedure for biologically bound polychlorinated biphenyls.

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