Green, simple analytical method for biogenic amines determination in fruit juice samples using salting-out assisted liquid-liquid microextraction andgas chromatography-mass spectrometry

Abstract

Salting-out assisted liquid-liquid microextraction (SALLME) was integrated withthederivatization procedure to establish a one-step sample pre-treatment approach for rapid analysis of14 biogenic amines (BAs) in fruit juices. The methodology consists of salting-out ofanalytes,derivatization with ethyl chloroformate (ECF), extraction with ethyl acetate (EtAc), andtheanalysis of the derivatized BAs using gas chromatography-mass spectrometry (GC-MS). Optimization oftheSALLME parameters, including the amount of sample, NaOH, and ECF was carried out through a Box-Behnken response surface design. The developed method exhibits satisfactory limits ofdetection (from 1.5 to 8.1 µg/L) andquantification (from 5.0 to 26.7 µg/L), and average recoveries between 84% and 108%. The developed procedure was used for BAs determination injuices ofdifferent berries withthe highest determined concentrations found for cadaverine, putrescine, tryptamine, andtyramine. Both GAPI and AGREE tools were used to assess the green character of the SALLME-GC-MS procedure.

Keywords: Biogenic amines; Experimental design; Fruit juices; Gas chromatography-mass spectrometry; Greenness evaluation; Salting-out assisted liquid-liquid extraction.