A rapid hybrid solid phase extraction (HybridSPE®) protocol tailored to ultra-performance liquid chromatography–electrospray ionization tandem mass spectrometry (UPLC®–ESI–MS/MS) analysis was developed for the determination of 15 per- and polyfluoroalkyl substances (PFAS) in liver tissue from harbour porpoises (Phocoena phocoena). The HybridSPE® technique has been applied in trace concentration bioanalysis, but it was mainly used for liquid biological media until now. In this study, the protocol was applied on tissue matrix, and it demonstrated acceptable absolute recoveries (%) ranging from 44.4 to 89.4%. The chromatographic separation was carried out using a gradient elution program with a total run time of 4 min. The inter-day method precision ranged from 2.15 to 15.4%, and the method limits of detection (LODs) ranged from 0.003 to 0.30 ng/g wet weight (w.w.). A total of 20 liver samples were analyzed to demonstrate the applicability of the developed method in liver tissue from a wildlife species.
In Europe, Northern America, and China a large number of individuals are suffering from peach ( Prunus persica ) allergy caused by the protein Pru p 1. Immunologic reactions against this 17.5 kDa protein result from initial sensitization to the birch ( Betula verrucosa ) pollen allergen Bet v 1 and subsequent immunologic cross-reactivity of Bet v 1 specific antibodies. Allergic symptoms typically include severe itching, scratching of the throat, and rhino conjunctivitis. So far, experimental structural data for the peach allergen Pru p 1 are not available. In a first step towards the elucidation of the structure of this protein we assigned backbone and side chain 1 H, 13 C, and 15 N chemical shifts of the naturally occurring isoform Pru p 1.0101 by solution NMR spectroscopy. Our chemical shift data indicate that this protein fold consists of seven β-strands separated by two short α-helices and a long C-terminal α-helix, which is in accordance with the reported crystal structure of Bet v 1. Our data provide the basis for determining the three-dimensional solution structure of this protein and to characterize its immunologic cross-reactivity on a structural basis.
Seven plant certified reference materials (NIST SRM1515 Apple Leaves, NIST SRM1547 Peach Leaves, BCR-129 Hay Powder, BCR-670 Aquatic Plant, GBW07603 Bush Twigs and Leaves, GBW10015 Spinach Leaves and NCS ZC73036a Green Tea) were analysed for their mass fractions of 48 elements by inductively coupled plasma tandem-mass spectrometry (ICP-MS/MS): Li, Be, Na, Mg, Al, Ca, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, As, Se, Rb, Sr, Y, Nb, Mo, Ag, Cd, Sb, Te, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Ta, Tl, Pb, Bi, Th, U. Special focus was put on the determination of technology-critical elements (TCEs), to which, e.g. Li, Be, Ga, Ge, Nb, Sb, Ta, Tl, Bi, and the rare-earth elements (REEs, lanthanides and Y) are counted. Closed-vessel microwave digestion was performed using HNO3, H2O2 and HBF4. The average bias for certified values is − 1% ± 13% (SD). Limits of detection (xL) in the measured solutions lie between 13 fg g−1 (Tb) and 52 ng g−1 (Ca). This article seeks to provide an optimised measurement procedure for the determination of element mass fractions of emerging importance in environmental samples, which are challenging to analyse with more traditional techniques such as single-quad ICP-MS. In addition, it aims to improve the characterisation of commonly used plant reference materials by providing mass fraction data for rarely studied elements. Graphical abstract
Ambient air pollutants are a global public health problem accounting for millions of annual deaths. A mobile module-based wind tunnel (WT) was developed to investigate the interaction between airborne particulate matter and various surface structures. The external dimensions were 4.33 m × 1.96 m × 1.73 m (lwh). The tunnel provided a cross-section of 0.40 m × 1.10 m (wh) and a total volume of 2.84 m3. An exchangeable test section in the WT offered a vertical area of one square meter to introduce variable installations. Due to the modular design, the WT could be divided into seven segments. This enables flexibility in setting, easy transport and set up at different locations. Atmospheric parameters (temperature, humidity, flow speeds and flow directions) were measured. At the test section, determined flow speeds ranged from 0.3 to 2.6 m s−1, with turbulence intensities detected between 9% and 11% and Reynold numbers from 10,000 to 90,000. Losses of ambient PM within the blank tunnel were less than 10% for particle counts (>0.25 µm), while smaller losses were obtained for PM1 and PM2.5. Thus, the construction, performance, as well as the limitations and various possible applications of the WT are shown in this article.
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