Comparison of Sample Preparation Methods for Multielements Analysis of Olive Oil by ICP-MS

Abstract

Elemental analysis of olive oils by Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is challenging because of the high organic load in olive oil samples and the low analyte concentrations. However, conflicting operating procedures in the preparation of oils prior to analysis by ICP-MS have been reported to overcome these difficulties. This study compared three methods of inorganic elements’ extraction from olive oils: The two commonly used microwave-assisted, acid digestion, and liquid−liquid, ultrasound-assisted extraction methods; and an optimized method: The combined microwave digestion-evaporation. Overall, microwave digestion-based methods did not compare opportunely, and ultrasound-assisted extraction was found to provide the best accord between simplicity of use, detection limits and precision improvement. The detection limits were in the range of 0.3−160 µg·kg-1, 0.012−190 µg·kg−1 and 0.00061−1.5 µg·kg−1, while repeatabilities were in the range of 5−21%, 5.4−99% and 5.1−40% for the microwave digestion, the combined digestion-evaporation and the ultrasound assisted extraction, respectively. The ultrasound-assisted extraction is therefore recommended as a preparation method for olive oils prior to analysis by ICP-MS. The broader range of elements that can be accurately detected is expected to help increase the discriminatory power and performance of geographical traceability models.

Keywords

• multielements
• olive oil
• ICP-MS
• microwave digestion
• evaporation
• ultrasound-assisted extraction