Application of semi-permeable membrane dialysis/ion trap mass spectrometry technique to determine polybrominated diphenyl ethers and polychlorinated biphenyls in milk fat

Polychlorinated biphenyls (PCBs) and polybrominated diphenyl ethers (PBDEs) are hazardous food contaminants, their maximum legally allowable levels in food and environment are in the low pg g−1 range. Therefore some highly selective and sensitive analytical methods must be used to determine them. The 96/23/EC Directive implemented by EC Decision of 12 August 2002 requires recovery rate of an analyte at a concentration below 1 ng g−1 within the 50–120% range at relative standard deviation (RSD) as low as possible.A method to determine low level PCBs and PBDEs in milk fat based on the semi-permeable membrane dialysis/ion trap GC MS technique was developed. Validation experiments proved that the method performance was within bounds set by the currently standing UE regulations. Recovery rates calculated on the basis of labeled internal standards for majority of the studied indicator PCB congeners and PBDE congeners were close to 100% at RSD below 20%. Also, dioxin-like PCBs recovery rates were compatible with the 1883/2006 EC Regulation (80–120%, RSD below 15%).The developed method turned out to be linear within a far broader concentration range than the studied 0.0025–10 pg μL−1 range entirely sufficient for analyses of PCB and PBDE in milk fat. Within that range coefficient of linear correlation (R2) of calibration curves exceeded 0.98.

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► We have investigated the usefulness of SPM dialysis for determination of PCB/PBDE.
► The factors affecting the dialysis process were evaluated.
► The ion trap MS was optimized for determination of PCB/PBDE in milk fat.
► Described extraction/clean up method proves usefulness for the milk fat analysis.