生附子中C19型二萜生物碱的高速逆流色谱分离及其结构鉴定

应用高速逆流色谱法分离制备了生附子中的3个C19型二萜生物碱类化合物。以正己烷-乙酸乙酯-甲醇-水(3:5:4:5, v/v/v/v)为两相溶剂系统,上相为固定相,下相为流动相,在主机转速850 r/min、流动相流速2.0 mL/min、检测波长235 nm条件下进行分离制备;一次性从90 mg附子总碱粗提物中分离制备得到15.3 mg北草乌碱,35.1 mg中乌头碱和22.7 mg次乌头碱,经高效液相色谱分析,测得它们的纯度分别为97.9%、96.2%和99.2%。并应用波谱(电喷雾离子质谱、核磁共振氢谱和核磁共振13C谱)解析法确定了它们的结构。利用该方法可以对生附子中的二萜类生物碱成分进行快速的分离和纯化     

逆流色谱法分离纯化蒲公英中多酚类化合物

采用pH区带逆流色谱(pH-zone-refining counter-current chromatography,pH-ZRCCC)与高速逆流色谱(high-speed counter-current chromatography,HSCCC)相结合的方式,从蒲公英中分离得到6个多酚类化合物。在pH-ZRCCC分离中,选择溶剂体系为乙酸乙酯-乙腈-水(体积比4:1:5),上相加入三氟乙酸(10 mmol/L)作为固定相,下相加入氨水(10 mmol/L)作为流动相。从1.6 g蒲公英乙酸乙酯粗提物中分离得到咖啡酸(60.2 mg,纯度98.1%)和对羟基肉桂酸(6.3 mg,纯度98.8%)及混合物A(590 mg)。之后进一步利用HSCCC,选择溶剂体系为石油醚-乙酸乙酯-甲醇-水(体积比1:4:1:4)。从400 mg混合物A中分离得到1-O-咖啡酰基甘油(7.7 mg,纯度82.2%)、3,4-二羟基苯乙酸(5.4 mg,纯度24.8%)、原儿茶酸(6.2 mg,纯度95.3%)以及对羟基苯乙酸(3.4 mg,纯度89.0%)。该方法制备量大,重现性好,适合蒲公英多酚类化合物的分离纯化。     

A material design of a new high-performance ferroelectric. I. SrTiO2C perovskite

At room temperature, cubic SrTiO₃ perovskite exhibits only paraelectric property, although ferroeletric properties appear in tetragonal BaTiO₃ and PbTiO₃. In this study, the new high-performance ferroelectric such as SrTiO₂C perovskite was theoretically designed. Cluster model calculations based on hybrid density functional theory were performed to clarify a ferroelectric mechanism of SrTiO₂C. It has been concluded that SrTiO₂C can be utilised for a ferroelectric material of a high-speed memory, due to the extremely small polarisation-inversion energy.     

高速电主轴的结构设计与发展

根据电主轴的结构特点和设计要求,通过分析其结构、电机技术、冷却、润滑等直接影响电主轴性能的各项指标,进行性能的分析和比较,提出了提高电主轴性能的主轴设计方案,为高速电主轴的快速发展提供参考.     

CRH3型动车组ATP车载设备安全性分析及故障处理研究

文章分析了CRH3型动车组车载设备ATP在运行过程中存在诸如物理打击、电磁干扰等潜在的安全隐患,并提出了相应的防护措施.讨论了机车一体化设计与设备维护的问题.在总结CRH3型动车组维护工作的基础上,分析了目前在ATP设备维护方面面临的问题及其针对性的解决方案.     

高速履带车辆转向载荷比分析与试验验证

为研究履带车辆稳态转向载荷比的变化规律,根据履带车辆转向过程中履带与地面之间的相互作用关系,建立了履带车辆稳态转向模型和履带车辆转向载荷比模型。分析了转向机构、接地压力分布形式、转向速度对转向载荷比影响。最后对某安装差速式转向机构的履带车辆开展了稳态转向试验,进行数据处理和结果对比。结果表明:车辆转向载荷比试验数据与理论计算结果有很好的一致性,验证了转向载荷比模型的准确性,为下一步履带车辆转向机构动力源的设计奠定了一定的基础。     

An efficient strategy for large-scale preparation of low polarity gingerols directly from ginger crude extract by high-speed countercurrent chromatography with different rotation mode

This study presents an efficient strategy for large-scale preparation of low polarity gingerols directly from ginger crude extract by high-speed countercurrent chromatography with different rotation mode. The ultrasonic-assisted extraction conditions were optimized by response surface methodology and the results showed the major low polarity gingerols could be well enriched under the optimized extraction conditions. Then the crude extract without any pretreatment was directly separated by high-speed countercurrent chromatography with different rotation mode using n-hexane/ethyl acetate/methanol/water (6:4:6:4, v/v/v/v) as the solvent system. In about 400 min, five major gingerols including 150 mg of [6]-gingerol, 50 mg of [8]-gingerol, 20 mg of [6]-shogaol, 43 mg of [6]-dehydrogingerdione, and 40 mg of [10]-gingerol were obtained from 1.2 g of crude extract in a single run with repeated injection. Their structures were identified by ¹H-NMR spectroscopy.     

High-speed counter-current chromatography assisted preparative isolation of phenolic compounds from the flowers of Chrysanthemum morifolium cv. Fubaiju

Chrysanthemum morifolium cv. Fubaiju is rich in phenolic compounds with various benefits such as anti-inflammatory, antioxidant, and cardiovascular protection. In this study, 12 phenolic compounds, including five flavonoid glycosides and seven quinic acid derivatives, were successfully separated from the flowers of Chrysanthemum morifolium cv. Fubaiju by high-speed counter-current chromatography and preparative high-performance liquid chromatography. Ethyl acetate-n-butanol–acetonitrile–water–acetic acid (5:0.5:2.5:5:0.25, v/v/v/v/v) was selected as solvent system to separate six fractions from the flowers of Chrysanthemum morifolium cv. Fubaiju, and 20% aqueous acetonitrile (containing 0.1% formic acid) was chosen to be the elution solvent in preparative high-performance liquid chromatography for purifying the fractions above. Luteolin-7-O-β-D-glucoside ( 1 ), luteolin-7-O-β-D-glucuronide ( 2 ), apigenin-7-O-β-D-glucoside ( 3 ), luteolin-7-O-β-D-rutinoside ( 4 ), diosmetin-7-O-β-D-glucoside ( 5 ), chlorogenic acid ( 6 ), 1,5-dicaffeoylquinic acid ( 7 ), 1,4-dicaffeoylquinic acid ( 8 ), 3,4-dicaffeoylquinic acid ( 9 ), 3,4-dicaffeoyl-epi-quinic acid ( 10 ), 3,5-dicaffeoylquinic acid ( 11 ), and 4,5-dicaffeoylquinic acid ( 12 ) were isolated with purities all above 95%, respectively. In addition, all isolates were evaluated for their protective effects on H₂O₂-induced oxidative damage in adult retinal pigment epithelial cells.     

基于MVB总线的网络控制实验平台的设计与实现

在对电动车组网络控制应用现状进行分析的基础上,介绍了基于MVB总线通信技术的列车网络模拟控制实验平台的设计方案,并对该实验平台的组成结构、主要功能、技术特点、软件实现和上位机监控界面的设计等方面进行了阐述。