A Simple and Efficient Two-Dimensional High-Speed Counter-Current Chromatography Linear Gradient and Isocratic Elution Modes for the Preparative Separation of Coumarins from Roots of Toddalia asiatica (Linn.) Lam.

Toddalia asiatica (L.) Lam. (Rutaceae) has shown a broad spectrum of biological properties, such as anti-inflammatory, antioxidant, antimicrobial, anti-HIV, and anticancer properties. The present study is concerned with the separation of the main components with broad partition coefficients (K_D values) from T. asiatica, using linear gradient high-speed counter-current chromatography (LGCCC) combined with an off-line two-dimensional (2D) mode. Similar to the binary gradient HPLC, the LGCCC mode is operated by the adjustment of the proportion between the mobile phase of 5:5:1:9 (v/v) (pump A) and 5:5:4.5:5.5 (v/v) (pump B) in an n-hexane/ethyl acetate/methanol/water solvent system. The off-line 2D-CCC mode was used in this study for the secondary separation of two similar K_D value compounds with n-hexane/ethyl acetate/methanol/water (5:5:4:6, v/v). Notably, six coumarins, namely, tomentin (1), toddalolactone (2), 5,7,8-trimethoxycoumarin (3), mexoticin (4), isopimpinellin (5), and toddanone (6), were efficiently separated. The structures of the pure compounds were elucidated by spectral techniques and compared with the literature.     

离子色谱法测定乳粉中的高氯酸盐

建立了乳粉中痕量高氯酸盐的固相萃取离子色谱分析方法。在碱性条件下,乙腈提取、浓缩,0.22μm尼龙滤膜+RP柱净化,AS20阴离子分析柱(150mm×4.0mm)分离,流动相为氢氧化钠溶液(30~70mmol/L),流速1.0mL/min。结果表明,高氯酸盐在0.4~20μg/L内具有良好的线性关系,相关系数0.999 8,样品检出限20μg/kg,加标回收率在77.2%~108%。测定了41个乳粉中的高氯酸盐含量,高氯酸盐检出率为31.7%。对质监部门用来检测乳粉中高氯酸盐的方法是一个补充,为食品安全提供了参考数据。     

用于空间激光通信的InGaAsP 激光二极管辐射损伤研究(英文)

对1:55 μm波长DFB 结构的InGaAsP 多量子阱激光二极管开展电子和60Co- 射线辐照试验。试验结果表明,激光二极管的斜度效率主要受带电粒子沉积的电离总剂量影响,而阈值电流和光功率主要受位移损伤剂量的影响。利用位移损伤剂量方法评价激光二极管的辐射损伤特征,并且预测其在空间辐射环境中的光功率衰退情况。模拟计算结果表明,MEO轨道辐射环境对激光二极管光功率辐射损伤远大于GEO轨道的影响,这主要是由于MEO轨道辐射环境的高能电子通量密度远大于GEO轨道的通量密度。The 1.55 μm InGaAsP multi-quantum-well laser diodes with distributed feedback structures were irradiated by electrons and 60Co- rays. The experimental results show the slope efficiency of laser diode is mostly affected by the total ionizing dose produced by charging particles, and the threshold current and the optical power mainly by displacement damage dose. The displacement damage dose methodology was employed to evaluate radiation damage of the laser diodes, and to predict the power degradations of these diodes in space. The calculated results indicate that the optical powers of the diodes will have more serious degradation for medium Earth orbit than for geosynchronous Earth orbit,due to higher fluence density of high energy electrons in GEO orbits.     

β-硝基苯乙烯衍生物与二溴海因高度区域选择性氨溴加成反应

以β-硝基苯乙烯衍生物为底物, 二溴海因为氮源/卤素源, 乙腈作溶剂, 建立了碳碳双键上高度区域选择性氨溴加成反应新体系. β-硝基苯乙烯衍生物与二溴海因在室温无水碳酸钠催化下反应, 可高收率获得邻位氨溴加成产物, 最高收率达97%; β-甲基-β-硝基苯乙烯衍生物在氢氧化钾催化下回流反应, 也可高收率得到邻位氨溴加成产物, 最高收率达95%. 实验结果表明, 对于硝基苯乙烯衍生物, 当苯环4-位具有强供电子基团如CH₃O时, 可以得到单一的α-氨基-β-溴加成产物, 但其收率相对较低; 当硝基苯乙烯衍生物的苯环4-位有强吸电子基团如NO₂时, 反应收率则很高. 这一实验结果证明β-硝基苯乙烯衍生物(缺电子烯烃)与二溴海因的氨溴加成反应具有亲核加成的特征. 本文共考察了20种不同结构的β-硝基苯乙烯衍生物的氨溴加成反应情况, 其产物结构经核磁共振波谱及质谱分析确证, 并提出了可能的反应机理.     

F-P半导体激光器实现多波长注入锁定

F-P半导体激光器中对于TE模比TM模有更大的束缚系数,并且在其反射面上有更高的反射率.当TE模和TM模同时注入F-P半导体激光器的谐振腔时,TE模方向的信号得到增长,TM模方向的信号受到抑制.F-P半导体激光器的这种特性使得它类似于一个偏振器,但是其优越之处在于经过F-P半导体激光器注入锁定之后的光信号没有功率损耗.采用F-P半导体激光器的注入锁定原理,使入射光信号没有功率损耗地由偏振光转换为部分偏振光,降低了通信系统中传输信号的偏振敏感性,使传输信号的质量得到提高,实现了F-P半导体激光器三波长和四波长注入锁定.     

二肽衍生物的电喷雾质谱研究

基于HIV整合酶核心结构域,合成了以HIV整合酶为靶标的二肽衍生物,采用多级质谱技术（二级、三级）研究二肽衍生物在质谱条件下的化学键断裂途径,发现主要的断裂方式为：氨基与羰基间的NH-CO键的断裂以及N-(苯并噻唑-2-基)甲酰氨基与亚甲基间的CO-C间的断裂。     

Determination of dextrin based on its self-aggregation by resonance light scattering technique

A novel free-probe assay of dextrin was established based on the resonance light scattering (RLS) enhancement in aqueous solution due to the self-aggregation of dextrin. The RLS intensity was well proportional to the concentration of dextrin over the wide range 0.2-14 μg mL⁻¹ and a detection limit 0.02 μg mL⁻¹ was obtained in the optimum conditions. The effect factors such as pH, buffer medium, holding time, ionic strength and temperature were studied in detail. Little or no interference was presented in the detection when adding coexisting substances including various metal ions and some saccharine in the solution. The assay proposed owns the advantages of easy operation, rapidity, sensitivity and practicability. Three synthetic samples and three kinds of medicine samples were analyzed with satisfactory results.     

Optimizing the integrated pulsed amperometric multicycle step waveform for the determination of tetracyclines

A method of modified integrated pulsed amperometric detection with multicycle step waveform (Multi-IPAD) following high-performance liquid chromatography (HPLC) was applied for the determination of tetracyclines (TCs) including dimethyltetracycline (DMTC), oxytetracycline (OTC) and tetracycline (TC). The key advantages of the Multi-IPAD are the abilities to enhance sensitivity and reproducibility and the ability to keep working electrode clean through the use of a high-frequent waveform alteration in integration step and the use of a cleaning potential, which is quite different from conventional three-step potential waveform. The analyses were carried out using the mobile phase of acetonitrile-water mixture solution (10:90, v/v) containing 1% perchloric acid on a C(18) column at a flow rate of 0.21 mL/min. The IPAD waveform parameters were optimized to maximize the signal-to-noise ratio (S/N) and successfully applied for the sensitive detection of TCs. The detection limits (S/N=3, 20 microL injected) were 0.07 mg/L for DMTC, 0.08 mg/L for OTC and 0.05 mg/L for TC. The peak height relative standard deviations (RSDs) of every compound for replicate injection (n=15) determined were below 4.6%.     

生物法与化学法制备硫酸软骨素

硫酸软骨素（ChS）是一种天然的酸性黏多糖,生物活性多样,在医学、生物、制药、食品、化妆品和材料等领域均有广泛应用,特别是在治愈骨关节病上具有颇为理想的效果。本文系统地总结了有关硫酸软骨素及其类似物的生物与化学制备方法的研究进展,如高产微生物菌株筛选与改良,培养条件优化与调控,汇聚式合成策略构建,经济易得的起始物原料等,并指出制备硫酸软骨素中存在的问题以及发展方向。     

Variation of gamma radiation shielding properties with incident photon energy and penetration depth for WC/Al composites

In this work, we examined the usefulness of the WC_x/Al_100?x composites (x?=?10, 20, 50, 80 wt. %) for gamma-ray shielding materials. The mass attenuation coefficient (μ/ρ), effective atomic number (Z_eff), electron density (N_e) and energy absorption buildup factor (EABF) and exposure buildup factor (EBF) for WC_x/Al_100?x composites have been calculated by theoretical approach using XCOM program within the energy range 1?keV–100?GeV, 10 keV–1?GeV, 10 keV–1?GeV and 0.015?MeV–15?MeV, respectively. The results showed that both the values of mass attenuation coefficient and Z_eff of the WC_x/Al_100?x composites tend to increase with the increase of the WC concentration. For the energy region below 3?MeV, the WC₈₀/Al₂₀ composite was found to possess superior gamma-ray shielding effectiveness due to its higher values of both mass attenuation coefficient and effective atomic number, and lower values of both EABF and EBF values. However, for the energy region above 3?MeV, the EBF and EABF values of the WC/Al composites are directly proportional to their Z_eff values, leading to the lowest EBF and EABF values of the WC₁₀/Al₉₀ composites.