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1.
[reaction: see text] A novel approach to alpha,alpha-disubstituted-beta-amino acids (beta(2,2)-amino acids) was employed in the synthesis of a series of 3-(pyrrolidin-1-yl)propionic acids possessing high affinity for the CCR5 receptor and potent anti-HIV activity. The rat pharmacokinetics for these new analogues featured higher bioavailabilities and lower rates of clearance as compared to cyclopentane 1.  相似文献   
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The antipsychotics risperidone, aripiprazole and pipamperone are frequently prescribed for the treatment in children with autism. The aim of this study was to validate an ultra‐high performance liquid chromatography–mass spectrometry method for the quantification of these antipsychotics in plasma. An ultra‐high performance liquid chromatography–mass spectrometry assay was developed for the determination of the drugs and metabolites. Gradient elution was performed on a reversed‐phase column with a mobile phase consisting of ammonium acetate, formic acid in methanol or in Milli‐Q ultrapure water at a flow rate of 0.5 mL/min. The method was validated according to the US Food and Drug Administration guidelines. The analytes were found to be stable enough after reconstitution and injection of only 5 μL improved the accuracy and precision in combination with the internal standard. Calibration curves of all five analytes were linear. All analytes were stable for at least 72 h in the autosampler and the high quality control of 9‐OH‐risperidone was stable for 48 h. The method allows quantification of all analytes. The advantage of this method is the combination of a minimal injection volume, a short run‐time, an easy sample preparation method and the ability to quantify all analytes in one run. Copyright © 2015 John Wiley & Sons, Ltd.  相似文献   
3.
The crossing number CR ( G ) of a graph G = ( V , E ) is the smallest number of edge crossings over all drawings of G in the plane. For any k 1 , the k planar crossing number of G , CR k ( G ) , is defined as the minimum of CR ( G 1 ) + CR ( G 2 ) + ? + CR ( G k ) over all graphs G 1 , G 2 , , G k with i = 1 k G i = G . Pach et al [Comput. Geom.: Theory Appl. 68 (2018), pp. 2–6] showed that for every k 1 , we have CR k ( G ) ( 2 / k 2 ? 1 / k 3 ) CR ( G ) and that this bound does not remain true if we replace the constant 2 / k 2 ? 1 / k 3 by any number smaller than 1 / k 2 . We improve the upper bound to ( 1 / k 2 ) ( 1 + o ( 1 ) ) as k . For the class of bipartite graphs, we show that the best constant is exactly 1 / k 2 for every k . The results extend to the rectilinear variant of the k ‐planar crossing number.  相似文献   
4.
Reaction of iron salts with three tripodal imidazole ligands, H(3)(1), H(3)(2), H(3)(3), formed from the condensation of tris(2-aminoethyl)amine (tren) with 3 equiv of an imidazole carboxaldehyde yielded eight new cationic iron(III) and iron(II), [FeH(3)L](3+or2+), and neutral iron(III), FeL, complexes. All complexes were characterized by EA(CHN), IR, UV, M?ssbauer, mass spectral techniques and cyclic voltammetry. Structures of three of the complexes, Fe(2).3H(2)O (C(18)H(27)FeN(10)O(3), a = b = c = 20.2707(5), cubic, I3d, Z = 16), Fe(3).4.5H(2)O (C(18)H(30)FeN(10)O(4.5), a = 20.9986(10), b = 11.7098(5), c = 19.9405(9), beta = 109.141(1), monoclinic, P2(1)/c), Z = 8), and [FeH(3)(3)](ClO(4))(2).H(2)O (C(18)H(26)Cl(2)FeN(10)O(9), a = 9.4848(4), b = 23.2354(9), c = 12.2048(5), beta = 111.147(1) degrees, monoclinic, P2(1)/n, Z = 4) were determined at 100 K. The structures are similar to one another and feature an octahedral iron with facial coordination of imidazoles and imine nitrogen atoms. The iron(III) complexes of the deprotonated ligands, Fe(1), Fe(2), and Fe(3), are low-spin while the protonated iron(III) cationic complexes, [FeH(3)(1)](ClO(4))(3) and [FeH(3)(2)](ClO(4))(3), are high-spin and spin-crossover, respectively. The iron(II) cationic complexes, [FeH(3)(1)]S(4)O(6), [FeH(3)(2)](ClO(4))(2), [FeH(3)(3)](ClO(4))(2), and [FeH(3)(3)][B(C(6)H(5))(4)](2) exhibit spin-crossover behavior. Cyclic voltammetric measurements on the series of complexes show that complete deprotonation of the ligands produces a negative shift in the Fe(III)/Fe(II) reduction potential of 981 mV on average. Deprotonation in air of either cationic iron(II) or iron(III) complexes, [FeH(3)L](3+or2+), yields the neutral iron(III) complex, FeL. The process is reversible for Fe(3), where protonation of Fe(3) yields [FeH(3)(3)](2+).  相似文献   
5.
Polymer–peptide conjugates (also known as biohybrids) are attracting considerable attention as injectable materials owing to the self‐assembling behavior of the peptide and the ability to control the material properties using the polymer component. To this end, a simple method for preparing poly(ethylene oxide)‐oligophenylalanine polymer–peptide conjugates (mPEOm‐Fn‐OEt) using isobutylchloroformate as the activating reagent has been identified and developed. The synthetic approach reported employs an industrially viable route to produce conjugates with high yield and purity. Moreover, the approach allows judicious selection of the precursor building blocks to produce libraries of polymer–peptide conjugates with complete control over the molecular composition. Control over the molecular make‐up of the conjugates allows fine control of the physicochemical properties, which will be exploited in future studies into the prominent self‐assembling behavior of such materials. © 2013 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2013 , 51, 4853–4859  相似文献   
6.
A novel Raman sensor using a liquid-core optical waveguide is reported, implementing a Teflon-AF 2400 tube filled with water. An aqueous analyte mixture of benzene, toluene and p-xylene was introduced using a 1000 μl sample loop to the liquid-core waveguide (LCW) sensor and the analytes were preconcentrated on the inside surface of the waveguide tubing. The analytes were then eluted from the waveguide using an acetonitrile-water solvent mixture injected via a 30 μl eluting solvent loop. The preconcentration factor was experimentally determined to be 14-fold, in reasonable agreement with the theoretical preconcentration factor of 33 based upon the sample volume to elution volume ratio. Raman spectra of benzene, toluene and p-xylene were obtained during elution. It was found that analytically useful Raman signals for benzene, toluene and p-xylene were obtained at 992, 1004 and 1206 cm−1, respectively. The relative standard deviation of the method was 3% for three replicate measurements. The limit of detection (LOD) was determined to be 730 ppb (parts per billion by volume) for benzene, exceptional for a system that does not resort to surface enhancement or resonance Raman approaches. The Raman spectra of these test analytes were evaluated for qualitative and quantitative analysis utility.  相似文献   
7.
The selectivity of high performance liquid chromatography (HPLC) separations is increased using a parallel column configuration. In this system, an injected sample is first split between two HPLC columns that provide complementary separations. The effluent from the two columns is recombined prior to detection with a single multiwavelength absorbance detector. Complementary stationary phases are used so that each chemical component produces a detected concentration profile consisting of two peaks. A parallel column configuration, when coupled with multivariate detection, provides increased chemical selectivity relative to a single column configuration with the same multivariate detection. This enhanced selectivity is achieved by doubling the number of peaks in the chromatographic dimension while keeping the run time constant. Unlike traditional single column separation methodology, the parallel column system sacrifices chromatographic resolution while actually increasing the chemical selectivity, thus allowing chemometric data analysis methods to mathematically resolve the multivariate chromatographic data. The parallel column system can be used to reduce analysis times for partially resolved peaks and simplify initial method development as well as provide a more robust methodology if and when subsequent changes in the sample matrix occur (such as when new interferences show up in subsequent samples). Here, a mixture of common aromatic compounds were separated with this system and analyzed using the generalized rank annihilation method (GRAM). Analytes that were significantly overlapped on both stationary phases applied, ZirChrom PBD and CARB phases, when used in traditional single column format, were successfully quantified with a R.S.D.% of typically 2% when the same stationary phases were used in the parallel column format. These results indicate that a parallel column system should substantially improve the chemical selectivity and quantitative precision of the analysis relative to a single-column instrument.  相似文献   
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Switchgrass (SG), corn stover (CS), and prairie cordgrass (PCG) pretreated with ammonia fiber expansion (AFEX) were densified using a novel low-temperature, low-pressure densification method. Simultaneous saccharification and fermentation (SSF) and separate hydrolysis and fermentation (SHF) were performed with loose and densified AFEX-treated biomass to determine the effect of post-AFEX densification. Biomass particle size reduction before pretreatment increased 144-h SSF ethanol yields from densified material by 8–9 % although no significant differences were seen in the first 72 h. Grinding material after densification had no impact on final ethanol yields but increased production rates in the first 24–48 h. Low-pressure, post-AFEX densification had no adverse effects on SSF ethanol yields from SG or CS but reduced yields from densified PCG by 16 %. Glucose concentrations after hydrolysis (SHF) showed similar trends. Ethanol yields after SHF, however, showed that densification had no significant impact on CS or PCG but reduced final ethanol yields from SG.  相似文献   
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