Determination of hydroxysafflor yellow A in biological fluids of patients with traumatic brain injury by UPLC‐ESI‐MS/MS after injection of Xuebijing

A simple, novel, specific, rapid and reproducible ultra‐performance liquid chromatography electrospray ionization tandem mass spectrometry method has been developed and validated for the determination of hydroxysafflor yellow A (HSYA) in biological fluids (plasma, urine and cerebrospinal fluid) of patients with traumatic brain injury after intravenous injection of Xuebijing (XBJ). Liquid–liquid extraction was performed, and separation was carried out on an Acquity UPLC? BEH C₁₈ column, with gradient elution using a mobile phase composed of methanol and 0.1% formic acid at a flow rate of 0.3 mL/min. A triple quadrupole tandem mass spectrometer with electrospray ionization was used for the detection of HSYA. The mass transition followed was m/z 611.0 → 491. The retention time was less than 3.0 min. The calibration curve was linear in the concentration range from 2 to 6125 ng/mL for cerebrospinal fluid, plasma and urine. The intra‐ and inter‐day precisions were <10%, and the relative standard deviation of recovery was <15% for HSYA in biological matrices. The method was successfully applied for the first time to quantify HSYA in the biological fluids (especially in cerebrospinal fluid) of patients with traumatic brain injury following intravenous administration of XBJ. Copyright © 2014 John Wiley & Sons, Ltd.     

Asymmetric synthesis of β-fluoroaryl-β-amino acids

The conjugate addition of lithium (R)-N-benzyl-N-(α-methylbenzyl)amide to a range of β-fluoroaryl-α,β-unsaturated esters gave the corresponding β-amino esters with high diastereoselectivity and in good isolated yields. Sequential treatment of the resultant β-fluoroaryl-β-amino esters under optimised hydrogenolysis conditions, followed by ester hydrolysis with 2.0 M aq HCl, provided access to a range of β-fluoroaryl-β-amino acids in good yield.     

(R)-3-乙酸奎宁环基酯的合成

分别以(R)-3-奎宁环醇与乙酸乙酯的酯交换法和(R)-3-奎宁环醇与乙酸酐的乙酸酐法合成了(R)-3-乙酸奎宁环基酯。通过考察原料摩尔比、催化剂用量、反应时间对产品收率的影响探索了合适的合成工艺。结果表明,乙酸酐法得到的产品收率远远高于酯交换法得到的产品收率,收率最高可达86.1%。     

Photocatalytic degradation of trichloroethylene over BiOCl under UV irradiation

In this study, BiOCl samples were synthesized under different pH values and characterized by XRD, SEM, UV‐vis DRS, BET, photoelectrochemical measurement and PL. The photocatalytic performances of the as‐prepared samples were evaluated through the decomposition of trichloroethylene (TCE) under UV irradiation. The influences of several parameters such as solution pH and common inorganic anions on TCE removal were investigated. Results indicated that BiOCl‐0.6 exhibited better photocatalytic performance than BiOCl‐6.0 because of its higher migration ability of photo‐induced carrier. The photocatalytic degradation of TCE over BiOCl‐0.6 followed pseudo first‐order kinetics and appeared to be more efficient in acidic solution than in alkaline. TCE was almost completely dechlorinated in 120 minutes. The inhibiting effect of naturally occurring anions was in the order of HCO₃^‐ >SO₄^2‐ >NO₃^‐, while Cl^‐ exhibited a dual effect. Moreover, BiOCl‐0.6 exhibited superior reusability after three cycles of repetition tests.     

Theoretical and Experimental Study of the Diffraction Intensity of Gradient Refractive-Index Lenses

We develop the wave-optics approach for calculating the diffraction distribution of gradient refractiveindex lenses and observing the diffraction pattern of gradient refractive-index lenses in the experiments. The results of our calculation are in good agreement with the experimental results obtained. We show that the diffraction can be regarded as a method to check the quality of the refractive-index distributions of gradient refractive-index lenses.     

A New Synthesis for Methyl 2-Benzyloxylphenylacetate

A new synthetic method for methyl 2-benzyloxylphenylacetate, a key intermediate of a new type of fungicides, had been found, which has only 3 steps. The 80% yield of the new method is a major improvement over the 30% 6-step-process reported by the literature.     

Numerical investigation on dynamic characteristics of drilling shaft in deep hole drilling influenced by minimal quantity lubrication

The dynamic characteristics of drilling shaft in deep hole drilling influenced by minimal quantity lubrication (MQL) is investigated. According to the features of the compressible fluid Reynolds equation in oil/air feature, a time-dependent mathematical model is established to describe the pressure distribution of cutting fluid with nonlinearity in MQL deep hole drilling. By introducing the differential transformation approach, the time-dependent pressure equation arising from cutting fluid is solved by the use of direct integral method. The influences of the rotational speed, the transverse displacement ratio, and radial clearance on the hydrodynamic pressure distribution of cutting fluid are obtained. The advantage of this method is to overcome much of the computational cost and has its rapid convergence rate. Furthermore, the nonlinear responses of drilling shaft influenced by MQL are analyzed, and the instability rotational speeds of drilling tool are discussed while the design parameters of drilling shaft system changing.     

High Carbon-Resistance Ni@CeO<Subscript>2</Subscript> Core–Shell Catalysts for Dry Reforming of Methane

Ni@CeO₂ core–shell catalysts were synthesized via a facile surfactant-assisted hydrothermal method and their catalytic performance in the dry reforming of methane (DRM) reaction was evaluated. A variety of techniques including XRD, N₂ adsorption–desorption, SEM, TEM, TPO, TGA were employed to characterize the prepared or spent catalysts. The encapsulation by the CeO₂ shell, on one side, can restrict the sintering and growth of Ni nanoparticles under harsh reaction conditions. On the other side, compared to the conventional shell material of SiO₂, CeO₂ can provide more lattice oxygens and vacancies, which is helpful to suppress coke deposition. Consequently, the Ni@CeO₂ core–shell catalysts exhibited better catalytic activity and stability in the DRM reaction with respect to the referenced Ni@SiO₂ core–shell catalysts and Ni/CeO₂ supported catalysts.