Development of a combined SEM and ICP-MS approach for the qualitative and quantitative analyses of metal microparticles and sub-microparticles in food products |
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Authors: | D Beltrami D Calestani M Maffini M Suman B Melegari A Zappettini L Zanotti U Casellato M Careri A Mangia |
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Institution: | 1.Dipartimento di Chimica Generale ed Inorganica, Chimica Analitica, Chimica Fisica,Università degli Studi di Parma,Parma,Italy;2.IMEM-CNR,Parma,Italy;3.Barilla Food Research Labs,Parma,Italy;4.ICIS-CNR,Padova,Italy |
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Abstract: | An integrated approach based on the use of inductively coupled plasma mass spectrometry (ICP-MS) and scanning electron microscopy
(SEM) for the qualitative and quantitative analyses of metal particles in foods was devised and validated. Different raw materials
and food products, like wheat, durum wheat, wheat flour, semolina, cookies, and pasta were considered. Attention was paid
to the development of sample treatment protocols for each type of sample to avoid potential artifacts such as aggregation
or agglomeration. The analytical protocols developed followed by ICP-MS and SEM investigations allowed us the quantitative
determination and the morphological and dimensional characterization of metal nano- and microparticles isolated from the raw
materials and finished food products considered. The ICP-MS method was validated in terms of linearity (0.8–80 μg/g and 0.09–9 μg/g
for Fe and Ti, respectively), quantification limits (0.73 μg/g for Fe and 0.09 μg/g for Ti), repeatability (relative standard
deviation (RSD) % equal to 10% for Fe and 20% in a wheat matrix as an example), and extraction recoveries (93 ± 2–101 ± 2%).
Validation of the scanning electron microscopy–energy dispersive X-ray spectroscopy (SEM-EDS) measurements was performed working
in a dimensional range from 1 to 100 μm with an estimated error in the size determination equal to 0.5 μm. ICP-MS data as
well as SEM measurements showed a decrease in the concentration of metal particles from wheat to flour and from durum wheat
to semolina samples, thus indicating an external contamination of grains by metal particles. These findings were confirmed
by environmental SEM analysis, which allowed investigation of particles of lower dimensions. Generally, the largest number
of particles was found in the case of iron and titanium, whereas particles of copper and zinc were only occasionally found
without any possibility of quantifying their number. |
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