Challenges in isolating silica particles from organic food matrices with microwave-assisted acidic digestion

Synthetic amorphous silica is widely used in food processing as a food additive (E551) due to its properties as a flavour carrier and anti-caking agent. The direct measurement of E551 suspended or embedded in complex matrices is difficult without prior removal of the matrix components. The isolation of nanoparticles from the matrix is hence the first step towards their comprehensive characterization. Due to its complexity, matrix removal is frequently not trivial and may cause modification of the number-size distribution of the silica particles. The isolation of engineered silica nanoparticles by removal of the matrix with microwave-assisted acidic digestion is demonstrated methodologically using both monodisperse (size standards) and polydisperse (E551) particles spiked into ultrapure water and tomato sauce. For the characterization of the isolated nanoparticles, asymmetric field flow fractionation (AF(4)) coupled to multi-angle laser light scattering (MALS) and inductively coupled plasma mass spectrometry (ICP-MS) were chosen. The combination of ICP-MS and ultracentrifugation allowed for the rapid and reliable measurement of the dissolved fraction of SiO(2). The results show that microwave-assisted acidic digestion partially dissolves silica nanoparticles. Moreover, the digestion conditions, in particular the low pH value, lead to strong agglomeration of the particles. A complete deagglomeration is not achieved, even when exposing the suspension to elevated sonication doses. The consequence of these two findings is a size distribution of particles after acidic digestion that is different from the original distribution before digestion. This result may have an impact on the evaluation of whether the material is a nanomaterial according to the recommended definition of the European Commission. [Figure: see text] ELECTRONIC SUPPLEMENTARY MATERIAL: The online version of this article (10.1007/s00216-019-01964-2) contains supplementary material, which is available to authorized users.