Multimethod approach for the detection and characterisation of food-grade synthetic amorphous silica nanoparticles

Synthetic amorphous silica (SAS) has been used as food additive under the code E551 for decades and the agrifood sector is considered a main exposure vector for humans and environment. However, there is still a lack of detailed methodologies for the determination of SAS' particle size and concentration. This work presents the detection and characterization of NPs in eleven different food-grade SAS samples, following a reasoned and detailed sequential methodology. Dynamic Light Scattering (DLS), Multiangle Light Scattering (MALS), Asymmetric Flow-Field Flow Fractionation (AF4), Inductively Coupled Plasma Mass Spectrometry (ICPMS) and Transmission Electron Microscopy (TEM) were used. The suitability and limitations, information derived from each type of analytical technique and implications related to current EC Regulation 1169/2011 on the provision of food information to consumers are deeply discussed. In general the z-average, AF4 hydrodynamic diameters and root mean square (rms) radii measured were in good agreement. AF4-ICPMS coupling and pre channel calibration with silica NPs standards allowed the reliable detection of NPs below 100 nm for ten of eleven samples (AF4 diameters between 20.6 and 39.8 nm) and to quantify the mass concentration in seven different samples (at mg L−1 concentration level). TEM characterisation included the determination of the minimum detectable size and subsequent measurement of the equivalent circle diameter (ECD) of primary particles and small aggregates, which were between 10.3 and 20.3 nm. Because of the dynamic size application range is limited by the minimum detectable size, all the techniques in this work can be used only as positive tests.