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To generate a given peak capacity, the 1.1 µm particles in 20 cm columns required roughly 75% of the time as 1.7 µm particles in 50 cm columns with both operated at 35 kpsi. The 1.1 µm particle packed columns generated a given peak capacity nearly 3 times faster than 1.7 µm particles in 15 cm columns operated at ~10 kpsi. This latter condition represents commercial state of the art for capillary LC. To consider practical benefits for metabolomics, the effect of different LC-MS variables on mass spectral feature detection was evaluated. Lower flow rates (down to 700 nL/min) and larger injection volumes (up to 1 µL) increased the features detected with modest loss in separation performance. The results demonstrate the potential for fast and high resolution separations for metabolomics using 1.1 µm particles operated at 35 kpsi for capillary LC-MS.Antibody fragments (Fab) are often produced by recombinant methods in Escherichia coli as no glycosylation is needed. Besides the correctly expressed Fab molecule, a multitude of host cell impurities and product related impurities are present in the crude sample. The identification and characterization of the product-related impurities, such as modified Fab-molecules or free light chain, are of utmost importance. The objective of this work was to design a purification strategy to isolate and characterize Fab and related impurities. A three-dimensional chromatography method was established, consisting of two affinity steps (Protein G and Protein L) and subsequent cation exchange chromatography, followed by mass spectrometry analysis of the purified samples. The procedure was automated by collecting the eluted target species in loops and directly loading the samples onto the high-resolution cation exchange chromatography column. As an example, four different Fab molecules are characterized. All four samples contained mainly the correct Fab, while only one showed extensive N-terminal pyroglutamate formation of the Fab. In another case, we found a light chain variant with uncleaved amino acids from the lead molecule, which was not used for the formation of whole Fab as only correct Fab was found in that sample. Impurities with lower molecular weights, which were bound on the Protein L column, were observed in all samples, and identified as fragments of the light chain. In conclusion, we have devised a platform for characterizing Fab and Fab-related impurities, which significantly facilitated strain selection and optimization of cultivation conditions.In this investigation, an efficient sorbent based on Fe3O4@polyphenols magnetic nanoparticles has been prepared using the extract of Mentha piperita leaves for the first time. The main purposes of this study were synthesis of economically affordable and environmentally friendly sorbent using the extract of Mentha piperita leaves and evaluating its application as a sorbent in magnetic solid phase extraction. The functional groups, magnetic property, size, and shape of the synthesized sorbent were characterized. The sorbent was utilized for the extraction and preconcentration of various pesticides (chlorpyrifos, fenazaquin, penconazole, diniconazole, oxadiazon, haloxyfop-methyl, hexaconazole, clodinafop-propargyl, tebuconazole, and fenoxaprop-p-ethyl) from vegetable, fruit, and water samples. After magnetic solid phase extraction, a dispersive liquid-liquid microextraction method was done to achieve low detection limits. The enriched pesticides were monitored by gas chromatography-tandem mass spectrometry. The synthesized sorbent was characterized by Fourier transform infrared, scanning electron microscopy, energy-dispersive x-ray spectroscopy, x-ray diffraction, and vibrating sample magnetometer techniques, which confirmed the successful synthesis of the magnetic nanoparticles. The effective parameters such as the sorbent weight, ionic strength, pH, vortex time, and kind and volume of elution and extraction solvents were studied. Under optimum extraction conditions, the method showed broad linear ranges (0.05-1000 µg L-1) with low limits of detection (0.27-4.13 ng L-1) and quantification (0.91-13.8 ng L-1). Extraction recoveries and enrichment factors were in the ranges of 54-89 % and 491-811, respectively.Understanding the transportation of polycyclic aromatic hydrocarbons (PAHs) across the water-sediment interface can help researchers to partition their sources while being particularly important for managing PAH input. This study fully explored the PAH dynamics between water and sediment in a tide-dominated estuary. The monthly concentration of ΣPAHs in sediments ranged from 325.47 to 1098.49 ng/g (dry weight), while that in water varied from 154.00 to 725.80 ng/L. CW069 Microtubule Associat inhibitor The PAH levels found in the present study were relatively high in comparison with other estuarine systems worldwide. The high-molecular-weight PAHs were more readily redissolved from sediment to water, while the low-molecular-weight PAHs were mostly in an unsaturated state with diffusion occurring from water to sediment. The seasonal differences of ΣPAHs were significant and were largely controlled by the changes in sediment properties, marine currents, and water temperature. The diagnostic ratios revealed that predominant sources of PAHs were pyrogenic processes and petrogenic inputs.A yearlong seasonal survey was carried out during 2016-2017 at 26 stations representing four tidal channels of the north-western part of the Gulf of Gabès (Tunisia). The area studied (characterized by a maximum tidal range of 2.3 m) was subjected to diverse anthropogenic pressures from the phosphate industry and its metallic pollution, unauthorized bottom trawling in shallow water (known locally as 'Kiss'), and organic pollution from the nearby urbanized areas. A total of 23,506 invertebrates representing 311 taxa were collected. Dominant taxa were the polychaetes with 51.4% of the individuals collected and 39.3% of the taxa, the amphipods (18.6% and 15.5%), the tanaids (12.3% and 2.6%), and the molluscs (11.5% and 18.3%). The mean annual abundances varied widely from one channel to another from 300 to 3700 ind·m-2. The stations located in deeper waters exhibited greater variability. Measurements of abundance revealed seasonal changes with maximum values in winter, spring, and lower numbers in summer. Each tidal channel was characterized by specific features in the fauna.
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