Development of a capsule phase microextraction methodology for the selective determination of coumarin in foodstuff analyzed by HPLC-DAD

Abstract

• Development of Sol-Gel C18 coated CPME device for food monitoring. • An optimized CPME protocol for the isolation of coumarin from bakery products. • Green selective extraction of coumarin to guarantee food quality and safety. In this work, a novel capsule phase microextraction (CPME) method coupled to high performance liquid chromatography with diode array detection (HPLC-DAD) was developed and validated for the determination of coumarin in bakery products, in accordance with the European Commission Regulation (EC) 1334/2008. The CPME extraction protocol was optimized after examining the following critical parameters: a) selection of the CPME membrane, b) sample loading time c) type of elution solvent, and d) desorption time. The optimum extraction parameters involved the use of a sol-gel CPME capsule (1 cm length), 1 mL of sample loading volume, elution with 3 mL of methanol, the stirring was set at 350 rpm, while the absorption time was 20 min and the desorption time was 15 min. The developed CPME-HPLC-DAD method was validated in terms of selectivity, linearity, accuracy, and precision and showed satisfactory results. The LOD and LOQ were equal to 0.18 µg/g and 0.48 µg/g, respectively. Trueness was assessed by means of relative percentage of recovery and ranged between 83 to 91% for intra-day experiments, and between 81-86% for inter-day experiments, respectively. The green character of the proposed method was examined using complexGAPI index. The method was successfully applied in the analysis of coumarin in bakery products.