Determination of natural phenols in olive fruits by chitosan assisted matrix solid-phase dispersion microextraction and ultrahigh performance liquid chromatography with quadrupole time-of-flight tandem mass spectrometry

• A novel application of MSPD microextraction using chitosan as sorbent is presented.
• The proposed method involves the use of UHPLC-Q-TOF/MS.
• MSPD microextraction is rapid, low cost, and economic to implement for routine control.
• Highly sensitive and selective analysis of natural phenols in olive fruits was achieved.

A simple, efficient and low-cost method based on matrix solid-phase dispersion (MSPD) microextraction and ultrahigh-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (UHPLC-Q-TOF/MS) was developed for the determination of seven main natural phenols (gallic acid, hydroxytyrosol, methyl gallate, luteolin 7-O-β-d-glucoside, rutin, ellagic acid and oleuropein) and other eleven compounds in olive fruits. The experimental conditions for the MSPD extraction, including the type of adsorbent, the amount of dispersing sorbent, the grinding time, and the type of elution solvent were investigated and optimized. The optimized parameters were determined to be that middle-molecular-weight chitosan was used as adsorbent, the amount of middle-molecular-weight chitosan was selected to be 25 mg, the grinding time was chosen to be 60 s, and methanol: water (6:4, v:v) was used as elution solvent. Compared with reported methods, the proposed method was more simple, rapid, and efficient. Moreover, this method required less extraction time and less amount of sample and solvent. The method showed good linearity (r2 ≥ 0.9909) for the seven analytes, with the limits of detection in the range of 69.6–358.4 ng/g. And recoveries were above 80.06%. The methodology was successfully applied to the extraction and determination of seven phenolic compounds in olive fruits（Canarii fructus）.