Synthesis of Y-shaped poly(solketal acrylate)-containing block copolymers and study on the thermoresponsive behavior for micellar aggregates

One novel type of Y-shaped amphiphilic copolymers with two hydrophobic poly(solketal acrylate) (PSA) branches and one hydrophilic monomethoxy poly(ethylene glycol) (MPEG) block was synthesized by atom transfer radical polymerization (ATRP). These Y-shaped polymers can disperse in aqueous media to self-assemble into micellar aggregates with a spherical core-shell structure. The aqueous copolymer solutions exhibited transmittancy transition in the temperature range of 30-60 °C via optical transmittance measurements. An interesting thermo-dependent size of the micellar aggregates was observed by dynamic light scattering techniques and transmission electron microscopy, which showed that the micelle diameters were decreased with temperature increasing. The nile red release from the micelles at 25 °C and 37 °C under various pHs showed that temperature has great influence on release behavior. With good biocompatibility, the micellar aggregates formed from MPEG-block-(PSA)(2) may serve as one promising thermosensitive nanovehicle for targeted drug delivery.     

Diastereoselective silver-catalyzed 1,3-dipolar cycloaddition of azomethine ylides with fluorinated imine

We described hereby an instance of diastereoselective silver-catalyzed 1,3-dipolar cycloaddition of azomethine ylides with imine compounds. This new method provided synthetically useful, highly substituted tetrahydroimidazole derivatives with efficiency and high diastereoselectivity. We can conveniently obtain fluorinated dihydroimidazole, imidazole, and diamino esters through simple modification.     

软岩力学特性研究

本文讨论了软岩的基本特性。根据软岩的膨胀崩解耐久性、冻融作用、力学性质试验结果、, 分析软岩力学特性与赋存环境(含水量、地应力、温度)和时间的关系。总结了软岩的力学性质变化特征。并提出软岩强度取值原则。     

Sensitive and Simple Electrochemical Detection of Lead(II) with Carbon Ionic Liquid Electrode

In this paper a carbon ionic liquid electrode (CILE) was fabricated by using ionic liquid 1‐ethyl‐3‐methylimidazolium ethylsulphate ([EMIM]EtOSO₃) as the modifier and further used as the working electrode for the sensitive anodic stripping voltammetric detection of Pb²⁺. The characteristics of the CILE were investigated by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). In pH 4.5 NaAc‐HAc buffer Pb²⁺ was accumulated on the surface of CILE due to the extraction effect of IL and reduced at a negative potential (‐1.20 V). Then the reduced Pb was oxidized by differential pulse anodic stripping voltammetry with an obvious stripping peak appeared at ?0.67 V. Under the optimal conditions Pb²⁺ could be detected in the concentration range from 1.0 × 10^?8 mol/L to 1.0 × 10^?6 mol/L with the linear regression equation as I_p(μA) = ?0.103 C (μmol/L) + 0.0376 (γ = 0.999) and the detection limit as 3.0 × l0^?9 mol/L (3σ). Interferences from other metal ions were investigated and Cd²⁺ could be simultaneously detected in the mixture solution. The proposed method was further applied to the trace levels of Pb²⁺ detection in water samples with satisfactory results.     

Application of SPE Using Multi-Walled Carbon Nanotubes as Adsorbent and Rapid Resolution LC-MS-MS for the Simultaneous Determination of 11 Triazine Herbicides Residues in River Water

A method for the simultaneous determination of 11 triazine herbicides residues in river water has been developed. It involves solid-phase extraction (SPE) pretreatment step and rapid resolution liquid chromatography-tandem mass spectrometry (RRLC-MS-MS). In the SPE pretreatment step, the adsorptive performance of MWCNTs material as SPE adsorbent and the elution capability of five kinds of solvents were investigated; in the LC separation step, a rapid resolution high throughput LC column, was used and the gradient elution mode adopted. The linear correlation coefficients (r ²) of the method for 11 target analytes varied between 0.9930 and 0.9980, the mean recoveries were in the range of 73.0 and 98.0% with relative standard deviations (RSD) 2.6 ~ 4.2%, the method detection limits (MDL) were all below 0.1 ng L^?1. An expanded uncertainty of not more than 20% was estimated for each analyte at the spiked concentration of 4.0 μg L^?1. The proposed method was applied to the determination of the residue concentrations of 11 pollutants in Songhuajiang River water.     

LC–MS–MS Quantitative Determination of Ursolic Acid in Human Plasma and Its Application to Pharmacokinetic Studies

A sensitive and specific liquid chromatography–electrospray ionization-tandem mass spectrometry method has been developed and validated for the identification and quantification of ursolic acid in human plasma using glycyrrhetic acid as an internal standard. The method involves extraction with methyl tert-butyl ether. The analyte was separated on a C₁₈ column and analyzed in multiple reaction monitoring mode with a negative electrospray ionization interface using the [M–H]? ions, m/z 455.4 for ursolic acid and m/z 469.5 → m/z 425.5 for glycyrrhetic acid. The method was validated over the concentration range of 0.86–110.0 μg L^?1. The intra- and inter-day precisions were less than 13.53% relative standard deviation (RSD) and the accuracy was within ?4.76% in terms of relative error (RE). The lower limit of quantification was 0.86 μg L^?1 with acceptable precision and accuracy. There were almost no matrix effects. Recovery of ursolic acid from spiked drug-free plasma was higher than 68%. The method was used to study the pharmacokinetic profile of ursolic acid in human plasma after oral administration of Jieyu capsules.     

碳酸二甲酯在固体碱上吸附和活化的原位红外光谱研究

采用原位红外技术研究了碳酸二甲酯在氧化镁、氟化镁、镁铝复合氧化物和氟改性的镁铝复合氧化物4种固体碱表面上的吸附和活化行为。结果表明:碳酸二甲酯以单、双齿两种形态吸附于固体碱的表面,双齿吸附的比单齿吸附的更易活化。碳酸二甲酯吸附于氧化镁和镁铝复合氧化物上活化生成甲氧基,吸附于氟化镁上活化生成甲氟基;而吸附于氟改性的镁铝复合氧化物上优先活化生成甲氟基,随着吸附表面温度的升高,逐渐有甲氧基生成,说明氟改性的镁铝复合氧化物是一种优良的甲基化反应催化剂。     

Eu~(3+)离子掺杂纳米TiO_2的制备及其光催化降解甲基兰溶液的研究

采用溶胶-凝胶法制备了系列不同原子摩尔比的Eu3+离子掺杂纳米TiO2光催化剂,通过XRD,SEM和UV-V is等测试手段对纳米TiO2晶型、颗粒度大小、形貌以及光学性能进行了表征;并以甲基兰溶液为目标物,对所制备样品的光催化活性进行了研究。结果表明,稀土Eu3+离子的掺杂能有效抑制纳米TiO2的晶型的转变进而减小晶粒尺寸、提高分散度;稀土Eu3+离子的掺杂使TiO2光催化剂紫外-可见吸收有一定的蓝移,并在可见区有一定的吸收峰;稀土Eu3+离子的掺杂有效提高了TiO2光催化剂的活性,并在本实验条件下,当掺杂原子摩尔比为1%、退火温度500℃时,对甲基兰溶液的光催化活性最强。     

超重力场电沉积NiW合金及其耐碱腐蚀性能

在超重力条件下电沉积NiW合金镀层,考察了超重力对NiW合金电沉积过程(各元素分电流、W含量和槽电压等)的影响规律;并利用扫描电子显微镜(SEM)、Tafel技术和电化学阻抗谱(EIS)技术研究了电沉积NiW合金镀层的表面形貌和在NaOH溶液中的抗腐蚀性能,同时通过浸泡实验考察了镀层的稳定性.结果发现,与常重力条件电沉积的NiW合金相比,超重力场电沉积的NiW合金中W含量增加,镀层表面无微裂纹产生;在10%(w)NaOH溶液中镀层自腐蚀电位正移,自腐蚀电流密度减小,腐蚀电阻也由常重力(重力系数G=1)时的865Ω·cm2增大至超重力(G=256)时的2305Ω·cm2;在10%NaOH溶液中浸泡144h后,超重力场电沉积的NiW合金表面无破碎和起皮现象发生.超重力技术在NiW合金电沉积过程中的应用,使镀层的耐碱腐蚀性能得到改善.