Nontargeted 400 MHz (13)C and (1)H nuclear magnetic resonance (NMR) spectroscopy was used in the context of food surveillance to reveal Pinus species whose nuts cause taste disturbance following their consumption, the so-called pine nut syndrome (PNS). Using principal component analysis, three groups of pine nuts were distinguished. PNS-causing products were found in only one of the groups, which however also included some normal products. Sensory analysis was still required to confirm PNS, but NMR allowed the sorting of 53% of 57 samples, which belong to the two groups not containing PNS species. Furthermore, soft independent modeling of class analogy was able to classify the samples between the three groups. NMR spectroscopy was judged as suitable for the screening of pine nuts for PNS. This process may be advantageous as a means of importation control that will allow the identification of samples suitable for direct clearance and those that require further sensory analysis.
Despite official regulations, the illegal use of formaldehyde-containing or releasing hair straightening products has become a popular practice in Europe and high contents of formaldehyde in such products have been reported. In this study, a methodology utilizing (1)H NMR spectroscopy has been developed to measure the concentration of formaldehyde in hair straightening products. For sample preparation, a dilution and alkaline hydrolysis is required. The total formaldehyde content can then be quantified by a distinct peak of the CH2 group of the methanediol molecule in the δ4.84-4.82 ppm range. The developed methodology was applied for the analysis of 10 hair straightening products. Seven of these products contained detectable amounts of formaldehyde that were higher than the maximum allowed concentration of 0.2%. The formaldehyde content of these products was found to be in the range 0.42-5.83% with an average concentration of 1.46%. The accuracy and reliability of the NMR results were confirmed by the EU reference photometric method. The air formaldehyde concentrations after application of hair straightening products were estimated in ranges 20-423 ppm and 1-18 ppm (for 1 and 24 m(3) salon volume). A probabilistic exposure estimation using Monte Carlo simulation found the average formaldehyde concentration to be 6 ppm (standard deviation 15 ppm). All exposure scenarios considerably exceeded the safe level of 0.1 ppm. Our findings confirmed that the risk of cosmetic formulations with formaldehyde above 0.2% is not negligible, as these products may facilitate considerable exposure of formaldehyde for consumers especially for salon workers.
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