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Targeted and also semi-untargeted determination of phenolic substances within place matrices through top rated fluid chromatography-tandem muscle size spectrometry.
The glutathione (GSH) trapping assay is commonly utilized for the screening and characterization of reactive metabolites produced by drug metabolism. This study describes a fluorous derivatization method for a more sensitive and selective analysis of reactive metabolites trapped by GSH using liquid chromatography-tandem mass spectrometry (LC-MS/MS). In this study, the GSH-trapped reactive metabolites, which were obtained after incubation of the test compounds with human liver microsome (HLM) in the presence of GSH and NADPH, were derivatized using the perfluoroalkylamine reagent through oxazolone chemistry. Since this reaction enabled the selective modification of the α-carboxyl group in GSH, the structural compositions of the metabolites were not affected by the derivatization. Furthermore, the selective analysis of the resulting derivatives could be performed using perfluoroalkyl-modified stationary phase LC separation via the interaction between the perfluoroalkyl-containing compounds, such as fluorous affinity, followed by detection with the precursor ion and/or enhanced product ion scan modes in MS/MS. Finally, we demonstrated the applicability of this method by analyzing perfluoroalkyl derivatives of some drug metabolites trapped by GSH in HLM incubation.Molecularly imprinted polymers coated magnetic particles (Fe3O4@MIPs) were prepared and used as adsorbents in solid phase extraction for efficient enantioseparation of racemic tryptophan (Trp) in aqueous medium. The amino-modified magnetic particles (Fe3O4-NH2) were first synthesized by one-pot hydrothermal method. Then the template molecules (L-Trp) were assembled on the surface of Fe3O4-NH2. Finally, Fe3O4@MIPs were prepared via a sol-gel method using L-Trp@Fe3O4-NH2 complex as matrix, 3-aminopropyltriethoxylsilane and n-octyltriethoxysilane as functional monomers. The as-prepared Fe3O4@MIPs were spherical with an average diameter about 149 ± 6.0 nm. The thickness of MIPs layer was approximately 3.5 ± 2.3 nm. click here The adsorption isotherms data of Fe3O4@MIPs toward L-Trp and D-Trp were well described by the Langmuir model. The maximum adsorption capacities of Fe3O4@MIPs for L-Trp and D-Trp were calculated to be 17.2 ± 0.34 mg/g and 7.2 ± 0.19 mg/g, respectively. The material exhibited good selectivity toward L-Trp with imprinting factor of 5.6. Excitingly, the enantiomeric excess (ee) of Trp in supernatant after adsorption of racemic Trp by Fe3O4@MIPs was as high as 100%. The result suggests that the imprinted caves in Fe3O4@MIPs are highly matched with L-Trp molecule in space structure and spatial arrangement of active functional groups. The work also demonstrates that sol-gel technology has great potential in preparation of MIPs for chiral separation.A method to thermodynamically model the alkane isovolatility curves of a comprehensive two dimensional gas chromatography (GC × GC) separation is presented. This method omits all instrument modifications, additional chromatogram collection, or method alterations which typical isovolatility curve generation requires. Provided that the thermodynamic indices of reference alkanes are available, chromatographers only need to specify the GC × GC method parameters of their separation to output the isovolatility curves. The curves can then be used alongside reference retention indices to generate two dimensional retention times for each analyte. Agreement between the modeled and experimental retention times provides a secondary mechanism for compound identification, supporting the results of a mass spectral search. The technique was used to model the retention times of a GC × GC separation of aromatic hydrocarbons, achieving an average first dimension retention time modeling error of 11 s and an average second dimension retention time modeling error of 0.09 s. Retention indices modeled retention times provide a simpler analyte identification procedure compared to conventional two dimensional retention indices matching.Poly(diphenylacetylene) having optically active anilide pendants (poly-1) were synthesized by the condensation reaction of an optically active carboxylic acid with a key precursor polymer containing amino (-NH2) groups, which was prepared by the polymerization of a phthalimide-protected diphenylacetylene monomer using WCl6-Ph4Sn as a catalyst, followed by phthalimide deprotection in the resulting polymer using hydrazine monohydrate. Poly-1 formed a preferred-handed helical conformation (h-poly-1) upon thermal annealing in DMF because of chirality of the pendant group. Poly-1 and h-poly-1 showed different chiral recognition abilities from the analogous poly(diphenylacetylene)s, having the corresponding optically active amide pendants, as chiral stationary phases (CSPs) for high-performance liquid chromatography. The resolution results with the h-poly-1-based CSP were much better than those with the poly-1-based CSP owing to the preferred-handed macromolecular helicity. Among the tested racemates, the h-poly-1-based CSP exhibited superior chiral recognition ability, especially toward binaphthyl compounds and chiral metal complexes.Background Modifying the implant surface via enhancing the wettability (hydrophilicity) improves osseointegration, reducing the healing period. In this study, the authors aimed to evaluate the stability and survival rates of implants with a hydrophilic surface compared with those with a sandblasted, acid-etched surface. Types of studies reviewed The included studies (randomized controlled trials) were identified through searches of PubMed, ScienceDirect, and Cochrane Library databases without date of publication restrictions. Quality assessment was performed using the Cochrane Collaboration tool. For primary outcome, confidence intervals were set at 95%; weighted means across the studies were calculated using a fixed-effects model or risk ratios and their 95% confidence intervals for secondary outcome. Results The authors included 5 randomized controlled trials (246 dental implants) in the systematic review, which compared a hydrophilic with conventional sandblasted, acid-etched implant surface. The implant stability (primary outcome) was measured at baseline and 3, 6, and 8 weeks, and implant survival rates were measured as a secondary outcome.
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