Development of a fast and low-cost aqueous based-extraction protocol for the simultaneous extraction and...

The determination of (nano)particulate content from food additives has been a long-standing concern for authorities since it is of vital importance for ensuring food safety, regulatory adherence, and transparent consumer information. Nonetheless, a critical step in these determinations is the refinement of a careful and quantitative extraction process for particles that may be found within complex matrices such as confectionery products. The development of new technologies and analysis methods for nanoparticles is ongoing. Whereas new technologies and analysis methods for nanoparticles are being developed, the extraction of (nano)particles of different nature has not been adequately addressed in the literature.

A simple aqueous extraction procedure was found to be suitable for the simultaneous extraction of TiO₂ and SiO₂ (nano)particles from five confectionery products. Neither the extraction agents (water, lipase, pancreatin and Tris-HCl solutions) nor the methods (manual shaking, ultrasonic bath, ultrasonic probe and ultrafiltration) altered the size, morphology, or aggregation state of either type of particle, as revealed by the micrographs obtained by Transmission Electron Microscopy (TEM). Single-particle ICP-MS (spICP-MS) determined that the optimal conditions for extracting both types of particles involve manual shaking using water as the solvent. Furthermore, the use of enzymes seemed to hinder the determination of both types of particles by spICP-MS. (Nano)particles of TiO₂ and SiO₂ were detected in all the confectionaries, even though the E171 additive was only labeled in one of them. The average percentage of nanoparticulate TiO₂ material in the evaluated products was 30 %, while no nanometer-sized particles of SiO₂ were detected.

Ensuring food safety, regulatory compliance and transparent consumer information relies on getting reliable results that connect with the application of sample treatment procedures for detecting unaltered nanoparticles in food products. The presented research introduces an economical, swift, user-friendly, environmentally responsible, and harmonious extraction method for the concurrent analysis of TiO₂ and SiO₂ particles in confectionery samples. Furthermore, particles from additives not included in the labeling have been detected, characterized, and quantified in the confectionary products.