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A method for the isotope dilution-mass spectrometric (ID-MS) determination of butyric acid C4 in butter fat (RM164) was developed in order to support the data gathered from nine experienced European laboratories within the final certification exercise. The ID-MS results (3,46±0,06 g C4/100 g fat) were in very good agreement with those obtained by “classical” GLC and HPLC techniques. (RM164 was finally certified at 3,49±0,06 g C4/100 g fat). This paper reports briefly on a previous preliminary study undertaken to validate a procedure (agreed by the BCR-sterol group) for the isolation of the sterol from fats and oils. By use of labelled sterols and radiometric measurements it was shown that sterol recoveries were superior to 96%.

Application of radiometric and isotope dilution-mass spectrometric techniques to the certification of edible oil and fat reference materials