RESUMO
Nanoplastics (NPs) have been identified as an emerging concern for the environment and our food chains in recent years. Monitoring the concentration and size of nanoplastics is essential to assess the potential risks that nanoplastic particles may pose. In this study, we presented a multi-technique based analytical platform to identify, characterize and quantify nanoplastics in water samples through a combination of sample pre-concentration, asymmetric flow field-flow fractionation coupled with multi-angle light scattering (AF4-MALS) and pyrolysis-GC/MS (Py-GC/MS). Models for predicting NPs concentration and particle number in unknown samples were established and validated using NPs standards of known size and AF4-MALS response. Py-GC/MS was applied for further identification of polymer type and quantification of mass concentration. Filtration conditions for pre-concentration were optimized to ensure a high recovery rate with minimal effect on original particle size. The addition of 0.05% SDS prior to filtration, using controlled filtration procedures, effectively improved the recovery. Furthermore, this study demonstrates the application of the analytical platform for the characterization and quantification of different nanoparticles (e.g. spiked PMMA and PS NPs) in the size range 60 nm-350 nm with detection limits down to 0.01 ppm in water samples. The established analytical platform can fill an analytical gap by offering a solution for quantifying size-resolved mass concentrations of nanoplastics and providing comprehensive data on size distribution, particle number and mass quantification with high sensitivity for detection.
RESUMO
The current food crisis demands unambiguous determination of mycotoxin contamination in staple foods to achieve safer food for consumption. This paper describes the first accurate LC-MS/MS method developed to analyze tricothecenes in grains by applying multiple reaction monitoring (MRM) transition and MS(3) quantitation strategies in tandem. The tricothecenes are nivalenol, deoxynivalenol, deoxynivalenol-3-glucoside, fusarenon X, 3-acetyl-deoxynivalenol, 15-acetyldeoxynivalenol, diacetoxyscirpenol, and HT-2 and T-2 toxins. Acetic acid and ammonium acetate were used to convert the analytes into their respective acetate adducts and ammonium adducts under negative and positive MS polarity conditions, respectively. The mycotoxins were separated by reversed-phase LC in a 13.5-min run, ionized using electrospray ionization, and detected by tandem mass spectrometry. Analyte-specific mass-to-charge (m/z) ratios were used to perform quantitation under MRM transition and MS(3) (linear ion trap) modes. Three experiments were made for each quantitation mode and matrix in batches over 6 days for recovery studies. The matrix effect was investigated at concentration levels of 20, 40, 80, 120, 160, and 200 µg kg(-1) (n = 3) in 5 g corn flour and rice flour. Extraction with acetonitrile provided a good overall recovery range of 90-108% (n = 3) at three levels of spiking concentration of 40, 80, and 120 µg kg(-1). A quantitation limit of 2-6 µg kg(-1) was achieved by applying an MRM transition quantitation strategy. Under MS(3) mode, a quantitation limit of 4-10 µg kg(-1) was achieved. Relative standard deviations of 2-10% and 2-11% were reported for MRM transition and MS(3) quantitation, respectively. The successful utilization of MS(3) enabled accurate analyte fragmentation pattern matching and its quantitation, leading to the development of analytical methods in fields that demand both analyte specificity and fragmentation fingerprint-matching capabilities that are unavailable under MRM transition.
