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In this study, a method based on direct-immersion single-drop microextraction was developed for the determination of vanadium in water. The detection system uses digital images obtained directly from the solvent drop after the sorption of V(V). The extraction solvent used was the ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate ([C6MIM][PF6]). The images were obtained directly from the solvent drop, with the aid of a camera. The digital images were stored, and the RGB (red, green, and blue) data were obtained. The data collected by the red channel were used to construct the analytical curve since it showed higher sensitivity compared with green and blue channels. Under optimized conditions, the method presented an enrichment factor of 50 and a limit of detection of 0.6 μg L-1 for 3.5 mL sample volume. The limit of quantification and the relative standard deviation (50.0 μg L-1) obtained were 1.8 μg L-1 and 4.8%, respectively. Certified reference material (Plankton) was used to assess the accuracy of the method. The simple, fast, efficient, and low-cost procedure was successfully applied to the determination of V(V) in water samples. The proposed method is also following the principles of green chemistry since it uses minimal volumes of samples, reagents, and solvents and yields a small amount of waste.Introducing a myriad array of chemicals in different industrial fields has made sample preparation inevitable for trace analysis. Classical extraction techniques such as solid phase extraction (SPE) and liquid-liquid extraction (LLE) techniques often suffer from tedious procedures (huge workload) and hazards to personnel and environment (samples and reagents are often user-unfriendly and processed in high amounts). For addressing these problems, microextraction techniques have been introduced. These systems benefit from using a minute amount of sample, reduced consumption of organic solvents, enhanced clean-up, high recovery and high enrichment factors. Moreover, approaches based on the use of natural materials have emerged during the last 10 years. Agarose is a natural biopolymer used as a green material in the form of gel-based separation medium. It has been recently utilized in the microextraction schemes. Easy fabrication, adjustability to get various dimensions and shapes, high inertness and biodegradability are of its main attributes. The present overview is focused on applications of agarose in solid phase microextraction (SPME), micro-solid phase extraction (μ-SPE) and liquid phase microextraction (LPME) - agarose film-liquid phase microextraction (AF-LPME) and gel electromembrane extraction (G-EME) since 2012. Besides, the pros and cons of agarose employment in the mentioned techniques will be described in depth.The occurrence of emerging contaminants is becoming of increasing importance to assess the impact of anthropogenic activities onto the environment. The present study reports for the first time the development and validation of an efficient method for the simultaneous determination of fragrance materials in water samples based on the use of a novel multiwalled carbon nanotubes (MWCNTs)-based solid-phase microextraction coating. Helical MWCNTs were selected as adsorbent material due to their outstanding extraction performance. The multicriteria method of desirability functions allowed the optimization of the experimental conditions in terms of extraction time and extraction temperature. Validation proved the reliability of the method for the determination of the analytes at ultra-trace levels, obtaining detection limits in the 0.2-13 ng/L range, good precision, with relative standard deviations lower than 20% and recovery rates in the 80 ± 12%-111 ± 11%. Superior enrichment factors compared to commercial fibers were also calculated. Finally, applicability to real sample analysis was demonstrated.Nivolumab is a fully human immunoglobulin G4 used for the treatment of several advanced solid cancers as immune checkpoint inhibitors. Silmitasertib in vivo There are some challenges for the quantification of mAb in plasma because IgG are present intrinsically in complex biologic matrices and this determination must be based on reliable, selective, and accurate analytical methods. This study described two validated methods carried out in two separate laboratories, one developed with a triple quadrupole tandem mass spectrometry (LC-MS/MS) and the other with high resolution mass spectrometry with an orbitrap system (LC-MS/HRMS). Both methods used full-length stable isotope-labeled nivolumab-like (Arginine 13C6-15N4 and Lysine 13C6-15N2) as internal standard. The sample preparation was based on IgG immunocapture, then trypsin digestion was performed and one surrogate peptide was quantified in positive mode. Assays showed good linearity over the range of 5-100 μg/mL and 5-150 μg/mL for LC-MS/HRMS and LC-MS/MS, respectively. The limit of quantification was set at 2 and 5 μg/mL for LC-MS/HRMS and LC-MS/MS, respectively. Acceptable accuracy (from - 13.6% to 3.0%) and precision (within 20%) values were also obtained with both methods. The two LC-MS methods showed a very different matrix effect linked to the use of different analytical columns and elution gradients. Nivolumab plasma concentrations from 60 cancer outpatients were compared with the two mass spectrometry methods and also with a home-made ELISA method. The Bland-Altman analysis did not show any significant bias between the three methods. The Passing-Bablock linear regression analysis showed a good agreement between the three methods with a better correlation between the two mass spectrometry methods.In this work, an automated surfactant-assisted dispersive liquid-liquid microextraction approach based on in-a-syringe concept was developed for the first time. The procedure assumed mixing aqueous sample phase and hydrophilic emulsion containing hexanoic acid and sodium hexanoate in a syringe of flow system. Sodium hexanoate acted as an emulsifier in dispersive liquid-liquid microextraction process and it was required for the formation of supramolecular solvent phase. After spontaneous separation of phases in the syringe, the upper supramolecular solvent phase containing target analytes was withdrawn and analyzed. The procedure was applied to the determination of 13 polycyclic aromatic hydrocarbons in tea infusion by high performance liquid chromatography with fluorescence detection. It was shown that the supramolecular solvent provided effective extraction of polycyclic aromatic hydrocarbons and fast phase separation in the syringe without centrifugation. The enrichment factors were in the range of 38-46. The automated microextraction procedure lasted 4 min including syringe cleaning.
Read More: https://www.selleckchem.com/products/cx-4945-silmitasertib.html
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