Screening-confirmation strategy for nanomaterials involving spectroscopic analytical techniques and its application...

The full characterization of nanomaterials (NMs), which requires a range of different and expensive equipment, is not always necessary to meet certain demands of information. Qualitative analytical methods are ideal alternatives when only a piece of information is required. In this work, a qualitative method for the screening of NMs has been developed and statistically validated for the first time, with silver nanoparticles (AgNPs) as a proof of concept. It is based on the generation of chemiluminescence of the luminol/Ag⁺ system in alkaline media in the presence of AgNPs. Measurements are obtained in a short time with a simple instrument. Probability of detection (POD) curves were constructed at three cut-off values next to the limit of detection of the chemiluminescent method. The unreliability region (UR) was from 0.50 to 1.82 μg L^-1. Currently, no regulation on AgNPs exists, but the present method was successfully tested for a hypothetical threshold of 2.5 μg L^-1 of 40 nm AgNPs. The method was applied to silver colored pearls, with silver (E-174) or aluminum (E-173) coating, used for decoration of pastry. Performance parameters such as false negative and positive rates as well as specificity, sensitivity and reliability rates were calculated for validation. The results of the screening method were confirmed by asymmetric flow field flow fractionation coupled to inductively coupled plasma mass spectrometry (AF4-ICP-MS). The proposed screening method is simple, fast, economic, and easy to transfer to routine laboratories in the field of food safety.