Comparative Study of Four Analytical Methods for the Routine Determination of Acrylamide in Black Ripe Olives

Reducing acrylamide in foods is an important scientific and regulatory goal. Black ripe olives contain significant levels of acrylamide. However, unlike cereal and potato products, there are no standardized methods or certified reference materials for olives and no harmonization between laboratories performing routine analyses. The industry has observed inconsistencies between laboratories using different analytical methods. To narrow the cause of this variability, acrylamide was extracted from olives using a single protocol and analyzed with the most commonly used routine methods: liquid chromatography with ultraviolet detection (LC-UV) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) without bromination and LC-UV and gas chromatography-mass spectrometry (GC-MS) following bromination. This design specifically evaluated the effects of sample derivatization and detector on acrylamide measurements, which has not been documented for any food. Accuracy, precision, sensitivity, linearity, and reproducibility were assessed, and 10 commercial olive samples were analyzed. LC-MS/MS demonstrated the best overall performance. Although derivatization decreased precision and reproducibility, all detection methods had comparable accuracy and calculated acrylamide values. The results suggest that harmonization of extraction protocols across laboratories is the most important area of future study. This study provides the framework for a standardized method for acrylamide analysis in olives. Reliable measurements are essential for aiding the decision making of the industry and regulatory agencies.