Abstract :
[en] Within the entire complex procedure required to measure dioxins and related compounds in biological matrices, the extraction step is often seen as a well controlled step. Although maybe true for many human and food-related matrices, the situation is very different for animal feed and feed ingredients. Specific European guidelines (e.g. Commission Directive 2006/13/EC, Commission Regulation (EC) No 152/2009) exist for animal feed but only list general requirements for the various stages of the procedure. The liberty is left to laboratories to select, for example, the tools used for the extraction steps. This has the advantage to allow ‘in-house’ methods to be used, as long as they satisfy with all the requirements of the EU Regulation. In that context, it is foreseen that the European Committee for Standardization (CEN) will soon propose a standard for the determination of PCDD/Fs and PCBs in animal feed that would be the reference method to be used to solve potential issues in case of dispute over results reported from different laboratories.
A major point of concern is that it has been reported earlier1 that most commonly accepted extraction procedure can conduct to significantly different results for the extraction of dioxins and related compounds in feed and feed additives such as mineral clays and various oxides. Several non-instrumental and instrumental automated approaches are available for extraction. Soxhlet extractors have long been the most used tools for non-instrumental extraction of solids. They have proven to be very efficient but some limitations encouraged the development of other approaches based on instrumental techniques. For feed extraction, pressurized liquid extraction (PLE) (also branded as accelerated solvent extraction ASE®) is the technique of choice for high sample throughput.
This study reports on the investigation of the use of various solvent mixtures, extraction temperatures, and instruments (parallel PLE, sequential ASE®) for the extraction of 17 PCDD/Fs and 12 dioxin-like PCBs in mineral clay, bovine feed, fish meal, and in-house quality control animal compound feed.