人教版高中化学教科书“研究与实践”栏目分析与实施策略*

对人教版高中化学教科书新设计的“研究与实践”栏目的主题内容、功能价值进行分析,就如何充分发挥该栏目的教学功能和价值,发展学生的化学学科核心素养,提出了创设教学情境线索、开发为研究性学习课题、开发为校本选修课程、开发为STEM课程等实施策略。     

组合式十字形钢管混凝土柱偏压力学性能试验研究

设计了一种由槽钢和方形钢管拼焊形成的组合式十字形钢管混凝土柱,将其灵活地布置在框架结构的中节点,可使柱肢与填充墙等厚,有效地提高建筑使用面积。共制作了6根组合式十字形钢管混凝土柱试件,考虑了偏心距和长细比两种变化参数。通过对其进行偏心受压试验研究,考察了试件的破坏形态和荷载-挠度曲线,并分析了其在不同偏心距和长细比下的荷载-应变曲线发展规律。结果表明:组合式十字形钢管混凝土柱中钢管和槽钢对混凝土的约束作用强,表现为较高的延性系数;偏心距或长细比越大,试件的极限承载力及弹性刚度越小,且偏心距越大延性越好,长细比对延性影响不显著;在受拉侧纵向应变基本上符合平截面假定,在受压侧纵向应变不符合平截面假定。     

高速气体与椭圆柱云相互作用的数值研究

高速颗粒流在天文、自然灾害、工业安全、医疗工业和国防等领域有着重要应用。采用基于分层流模型的直接数值模拟方法,对平面激波与椭圆柱云的相互作用进行数值研究,重点关注椭圆柱横截面的不同长短轴之比和椭圆柱横截面长轴与来流方向所成角度对流场的影响,从气体来流方向上的速度、x轴和y轴方向上的均方根速度、动能、内能和湍动能的分布上进行分析,对能量在计算域的上游区域、椭圆柱云区域和下游区域进行定量分析。同时针对椭圆柱改进了一维体积平均模型,利用该模型拟合了由直接数值模拟得到的反射激波和透射激波位置,获得了最适配的一维体积平均模型中的人工有效阻力系数,并探讨此系数的分布规律。     

基于捕集柱阵列的制备型二维液相色谱纯化烟草中的4个组分

二维液相色谱(2D-LC)因具有较高的峰容量,在复杂样品的分离分析中获得了广泛的关注。然而,制备型2D-LC以纯化高纯单体为目标,在方法开发和设备构成等方面与分析型2D-LC有较大的不同,目前尚未得到充分的开发,在大规模的制备纯化中应用较少。本文以一套制备液相色谱模块为分离系统,以稀释泵、切换阀和捕集柱阵列为接口,构建了新型的制备型2D-LC系统,旨在规模化纯化多个活性成分。以烟叶中可以用作医药原料的烟碱、绿原酸、芦丁和茄尼醇等组分为目标物,考察了不同类型填料对样品的捕集效率、过载条件下的色谱保留行为等,优化了制备色谱条件。进而利用在线2D-LC系统实现了烟叶提取物的纯化,通过一次运行获得了4个高纯化合物。该系统具有中压色谱纯化成本低、系统在线运行自动化程度高、稳定性好及容易放大等优点。烟叶中活性化学成分的回收利用对促进烟草行业的发展及带动地方农业经济开发具有重大的意义。     

Preparation of open tubular capillary column covalently coated with polystyrene sulfonate with 4,4′-Azobis(4-cyanopentanoyl chloride) as polymerization initiator for electrochromatographic separation of alkaloids,sulfonamides, and peptides

An open tubular capillary electrochromatography column covalently bonded with polystyrene sulfonate was prepared via in situ polymerization using functionalized Azo-initiator 4,4′-Azobis(4-cyanopentanoyl chloride). Scanning electron, fluorescence, and atomic force microscopy techniques showed the formation of a relatively rough layer of polymer. In addition, –CN and C = O stretching vibrations from infrared spectroscopy proved the successful immobilization of the azo-initiator through covalent bonding and X-ray photoelectron spectroscopy confirmed the elemental composition of the formed polymer layer. The prepared column was found to be appropriate for small and medium-sized molecules separation. Compared to bare fused silica capillary column higher selectivity and resolution were obtained for the separation of alkaloids, sulfonamides, and peptides as a result of the electrostatic and pi-pi stacking interactions between the small organic molecules and the coated column without compromising the electroosmotic flow mobility. Separation efficiency was also increased compared to the bare capillary for the separation of alkaloids (about 1.5 times). Moreover, intraday, inter-day, intra-batch, and inter-batch relative standard deviation values of retention time and peak area of peptides were within 2% and 10%, respectively, indicating good repeatability of the column preparation procedure. The developed method for the covalent bonding of polymers through a functionalized azo-initiator could represent a promising stable method for the preparation of an open tubular column.     

超高效液相色谱-串联质谱法测定烟用水基胶中邻苯二甲酸酯类化合物

建立了一种测定烟用水基胶中17种邻苯二甲酸酯类(PAEs)化合物的超高效液相色谱-串联质谱(UPLC-MS/MS)法。样品经水分散,以甲醇定容,涡旋振荡萃取。萃取液离心后,过有机相滤膜进行UPLC-MS/MS分析。通过增加延时柱的方法,排除色谱系统带入的PAEs干扰。结果表明:在0~5μg/m L范围内,方法的线性关系良好,相关系数均大于0.994,定量下限为0.010~0.479μg/g。该方法的回收率为87.6%~106.0%,相对标准偏差(RSD,n=6)为0.8%~6.2%。将该方法与YC/T 333-2010标准方法进行对比,结果显示两种方法的检测数据不存在显著性差异。方法用于烟用水基胶中17种PAEs的测定,操作简单,稳定性好。     

整体柱富集技术在微流控芯片系统中的应用

样品预处理技术是微流控芯片技术发展的瓶颈之一。整体材料是近几年在色谱领域发展起来的一种新型色谱填料,具有结构均匀、传质速度快、通透性好、制备过程简单等优点,被广泛用于微流控芯片系统中。该文综述了整体柱富集技术在微流控芯片系统中的应用进展,引用文献80篇。     

HPLC柱效对检测水中磺胺二甲基嘧啶色谱条件的影响

研究色谱柱的柱效降低后对高效液相色谱测定水中磺胺二甲基嘧啶色谱条件的影响。比较了新旧色谱柱的分离效果、色谱峰的对称性和峰面积,结果表明,旧色谱柱的柱效降低,对目标物的分离效果变差,目标物的吸收峰面积变小,峰形不对称。对色谱条件进行了优化试验,结果表明,对流动相水相添加0.125%的冰乙酸调节p H值为4.5后色谱峰的峰形对称性和分离效果得到改善。     

罗丹明B分子印迹固相萃取小柱的研制及应用

研制一种对罗丹明B具有特异性识别性能的分子印迹固相萃取小柱。用沉淀聚合法制备罗丹明B分子印迹聚合物,通过静态平衡吸附实验及固相萃取实验表征其性能,并对市售辣椒样品中的罗丹明B进行测量。罗丹明B模板聚合物的吸附能力明显优于空白聚合物;印迹固相萃取小柱对罗丹明B标准溶液(0.05 mmol/L)一次性萃取率为98.24%,实际样品测量的回收率为90.0%~95.0%,测定结果的相对标准偏差为0.9%~1.7%(n=3)。罗丹明B分子印迹固相萃取小柱选择性好、萃取率高,可应用于食品、化妆品检测等相关领域。     

Stage-frit: A straightforward sub-2 μm nano-liquid chromatography column fabrication for proteomic analysis

In this work we demonstrated a facile method for the fabrication of C18 coordination polymer gel in a capillary, called stage-frit, which was efficiently applied to pack sub-2 μm C18 beads into the capillary by a high pressure bomb for the online separation of proteolytic peptides. The back pressure of the column with 10 cm × 75 μm i.d. is regularly lower than 170 bar at a flow rate of 300 nl/min, which could be operated on a common nanoLC system instead of nanoUPLC system due to the good permeability, low back pressure and high mechanical stress of the frit that will totally reduce the cost for the purchase of instrument. The stage-frit allows long-term continuous flow of the solvent and no significant beads loss or pressure instability was observed during the period. The repeatability of retention time for fifteen BSA tryptic peaks was found to be less than 1.08% (RSD) in six time nanoLC-ESI-MS/MS experiments. The average full width at half maximum (FWHM) of peptide peaks is 5.87 s. The sub-2 μm stage-frit nanoLC column showed better sensitivity than the commercial available for large scale proteomic analysis of total tissue proteins from human spleen. The number of identified peptides is approximately 0.4-fold and 0.2-fold higher than that obtained by utilizing commercial columns packed with 3 μm and 1.8 μm C18 materials, respectively. In the field of analytical chemistry, particularly the use of nanoLC systems, stage-frit nanoLC column offers a great potential for the separation of complex mixtures.