两种测定果汁中钾磷含量方法的比较与分析

采用微波消解-等离子体发射光谱法同时测定果汁中K、P含量,优化了实验所需的各种条件。与国家标准方法湿法消解-分光光度法的测定结果作了实验比较,结果表明本实验方法更简单、高效,节省了样品的前处理时间,减小了最终结果的误差。该法灵敏度高、线性范围宽、加标回收率高,结果令人满意。     

HL-2M 真空室保温层设计及安装

基于 HL-2M 真空室烘烤保温要求，通过有限元分析和原型件实验确定采用陶瓷纤维与纳米级微孔材 料组合作为 HL-2M 真空室保温材料。在 30℃时，保温层的导热系数小于 0.027W⋅m⁻¹·℃⁻¹；300℃时，导热系数 小于 0.038W⋅m⁻¹·℃⁻¹。在保温层厚度 25mm、热面温度 300℃且达到稳态时，冷面可控制在 85℃以下，线圈侧的 温度低于 60℃，整体热损失小于 12kW，满足 HL-2M 真空室烘烤需求。      

Polymer chain diffusion in polymer blends: A theoretical interpretation based on a memory function formalism

The diffusion of polymer chains in miscible polymer blends with large dynamic asymmetry—those where the two blend components display very different segmental mobility—is not well understood yet. In the extreme case of the blend system of poly(ethylene oxide) (PEO) and poly(methyl methacrylate)(PMMA), the diffusion coefficient of PEO chains in the blend can change by more than five orders of magnitude while the segmental time scale hardly changes with respect to that of pure PEO. This behavior is not observed in blend systems with small or moderate dynamic asymmetry as, for instance, polyisoprene/poly(vinyl ethylene) blends. These two very different behaviors can be understood and quantitatively explained in a unified way in the framework of a memory function formalism, which takes into account the effect of the collective dynamics on the chain dynamics of a tagged chain. © 2019 Wiley Periodicals, Inc. J. Polym. Sci., Part B: Polym. Phys. 2019 , 57, 1239–1245     

Development of a high‐performance liquid chromatography method with fluorescence detection for the routine quantification of tamoxifen,endoxifen and 4‐hydroxytamoxifen in plasma from breast cancer patients

To date, several methods for the quantification of tamoxifen and its metabolites have been developed, most of which employ liquid chromatography tandem–mass spectrometry (LC–MS/MS). These methods are highly sensitive and reproducible, but are also time‐consuming and require expensive equipment; one of their main disadvantages is matrix ionization effects. A more viable option, particularly in developing countries, is high‐performance liquid chromatography coupled with UV or fluorescence detection. We developed and validated a method for simultaneous quantification of tamoxifen, endoxifen and 4‐hydroxytamoxifen based on high‐performance liquid chromatography with fluorescence detection in a reverse‐phase column. The method is rapid (16 min plus 5 min of column re‐equilibrium), accurate (80–100%) and precise (0.23–6.00%), and does not require any additional irradiation process. Sample pretreatment consists of protein precipitation with acetonitrile under alkaline conditions, employing only 200 μL plasma. The validated method's wide range allowed quantification of steady‐state levels in patients under standard tamoxifen treatment (20 mg/day). This assay is ready for application in clinical studies and routine quantification of tamoxifen, endoxifen and 4‐hydroxytamoxifen in healthcare institutions.     

Recent Progress on Manganese-Based Nanostructures as Responsive MRI Contrast Agents

Manganese-based nanostructured contrast agents (CAs) entered the field of medical diagnosis through magnetic resonance imaging (MRI) some years ago. Although some of these Mn-based CAs behave as classic T₁ contrast enhancers in the same way as clinical Gd-based molecules do, a new type of Mn nanomaterials have been developed to improve MRI sensitivity and potentially gather new functional information from tissues by using traditional T₁ contrast enhanced MRI. These nanomaterials have been designed to respond to biological environments, mainly to pH and redox potential variations. In many cases, the differences in signal generation in these responsive Mn-based nanostructures come from intrinsic changes in the magnetic properties of Mn cations depending on their oxidation state. In other cases, no changes in the nature of Mn take place, but rather the nanomaterial as a whole responds to the change in the environment through different mechanisms, including changes in integrity and hydration state. This review focusses on the chemistry and MR performance of these responsive Mn-based nanomaterials.     

Molecular QTAIM Topology Is Sensitive to Relativistic Corrections

The topology of the molecular electron density of benzene dithiol gold cluster complex Au₄−S−C₆H₄−S′−Au′₄ changed when relativistic corrections were made and the structure was close to a minimum of the Born–Oppenheimer energy surface. Specifically, new bond paths between hydrogen atoms on the benzene ring and gold atoms appeared, indicating that there is a favorable interaction between these atoms at the relativistic level. This is consistent with the observation that gold becomes a better electron acceptor when relativistic corrections are applied. In addition to relativistic effects, here, we establish the sensitivity of molecular topology to basis sets and convergence thresholds for geometry optimization.     

新型川芎嗪衍生物的合成

以川芎嗪为原料，经氧化、Boekelheide重排、水解和氧化反应合成了中间体3,5,6-三甲基吡嗪-2-甲醛（4）; 4与取代N-4-哌啶酮发生缩合反应合成了9个新型的川芎嗪衍生物，其结构经¹H NMR, ¹³C NMR和MS（ESI）表征。     

In Situ Generation of ArCu from CuF2 Makes Coupling of Bulky Aryl Silanes Feasible and Highly Efficient

A bimetallic system of Pd/CuF₂, catalytic in Pd and stoichiometric in Cu, is very efficient and selective for the coupling of fairly hindered aryl silanes with aryl, anisyl, phenylaldehyde, p‐cyanophenyl, p‐nitrophenyl, or pyridyl iodides of conventional size. The reaction involves the activation of the silane by Cu^II, followed by disproportionation and transmetalation from the Cu^I(aryl) to Pd^II, upon which coupling takes place. Cu^III formed during disproportionation is reduced to Cu^I(aryl) by excess aryl silane, so that the CuF₂ system is fully converted into Cu^I(aryl) and used in the coupling. Moreover, no extra source of fluoride is needed. Interesting size selectivity towards coupling is found in competitive reactions of hindered aryl silanes. Easily accessible [PdCl₂(IDM)(AsPh₃)] (IDM = 1,3‐dimethylimidazol‐2‐ylidene) is by far the best catalyst, and the isolated products are essentially free from As or Pd (<1 ppm). The mechanistic aspects of the process have been experimentally examined and discussed.     

基于非线性梁理论的有限质点法

有限质点法是以向量式力学为基础,用有限数量的质点来模拟结构的变形行为,质点的运动由牛顿运动定律来计算。在有限质点法中,质点通过构件相连,构件约束着质点的运动,并且其内力由质点的运动变量来描述。基于向量式力学的基本思想和非线性梁理论,提出了一种新的有限质点法,该方法在共旋单元坐标系中描述梁的非线性变形。以空间梁系结构为例,推导了计算构件内力的非线性公式,并考虑了弯扭耦合变形。通过两个连续欧拉角的变换公式得到共旋坐标系的旋转矩阵。与传统的有限质点法相比,本文提出的方法避免了刚体虚转动分析。通过四个结构的数值求解,验证了本文方法在计算结构大变形响应时具有较高的精度。     

非金属掺杂改性g-C3N4光催化降解水中有机污染物的研究进展

近年来，石墨相氮化碳(g-C₃N₄)以其合适的带隙宽度、丰富的活性位点和成本低廉等优点，成为新兴的可见光响应非金属光催化剂，被广泛应用于光催化降解有机污染物领域。然而，纯g-C₃N₄对可见光的吸收效率较低且光生电子和空穴复合速率快，导致其光催化活性处于较低水平。基于g-C₃N₄的非金属特性，通过非金属掺杂可以有效提高g-C₃N₄的光催化性能，引起了学者们的广泛关注。本文介绍了目前非金属掺杂g-C₃N₄复合材料常见的制备方法，着重归纳了不同类型的非金属掺杂g-C₃N₄光催化降解水中有机污染物的相关研究进展，探讨其作为光催化剂在可见光条件下降解有机污染物的相关机理。最后，提出目前g-C₃N₄基复合材料在光催化降解水中有机污染物中所面临的挑战，旨在为非金属掺杂g-C₃...