Preparative isolation and purification of anti‐tumor agent ansamitocin P‐3 from fermentation broth of Actinosynnema pretiosum using high‐performance counter‐current chromatography

Ansamitocin P‐3 is a potent anti‐tumor maytansinoid found in Actinosynnema pretiosum. However, due to the complexity of the fermentation broth of Actinomycete, how to effectively separate ansamitocin P‐3 is still a challenge. In this study, both analytical and preparative high‐performance counter‐current chromatography were successfully used to separate and purify ansamitocin P‐3 from fermentation broth. A total of 28.8 mg ansamitocin P‐3 with purity of 98.4% was separated from 160 mg crude sample of fermentation broth in less than 80 min with the two‐phase solvent system of hexane–ethyl acetate–methanol–water (0.6:1:0.6:1, v/v/v/v). The purity and structural identification were determined by HPLC, ¹H NMR, ¹³C NMR and mass spectroscopy.     

(4R)-5,5-二甲基-4-苄硫甲基-2-噁唑烷酮的合成

以价廉易得的天然L-半胱氨酸为原料,经巯基保护、酯化、氨基保护、格氏反应及环化等5步反应,合成了一个新的手性助剂(4R)-5,5-二甲基-4-苄硫甲基-2-噁唑烷酮,总收率31%.产物结构经IR,~1H NMR,~(13)C NMR及MS表征.     

Ultrasonic-Assisted Drop-to-Drop Solvent Microextraction in a Capillary Tube for Analyzing Trace Benzene, Toluene, Xylene in One Drop of a Water Sample

A novel analytical technique termed ultrasonic-assisted drop-to-drop solvent microextraction (USA-DDSME) in a capillary tube was developed to determine trace benzene, toluene, xylene in one drop of a water sample, which was combined with gas chromatography–flame ionization detection (GC–FID). The advantages of this method are rapidity, convenience, ease of operation, simplicity of the device, and extremely little solvent and sample consumption. Extraction conditions including the type of extraction solvent, the volume of extraction solvent, the volume of sample, extraction time and effect of salt concentration were optimized. The best optimum parameters for extraction were achieved with 3 μL of extraction solvent. Chloroform was divided into four equal divisions in 20 μL water sample (without salt addition) in a capillary tube and ultrasonicated for 10 min, centrifugated at 2,500 rpm for 5 min to let the extraction solvent settle at the bottom of the capillary tube, then 1 μL of the separated extraction solvent was injected into the GC–FID for analysis. Linearity of the method was determined by analyzing spiked water samples over a concentration range of 0.1–50 μg mL^?1. Correspondingly, the LOD values were 0.01 μg mL^?1. All calibration curves were found to have good linearity with correlation coefficients (r ²) > 0.995. The precision (RSD) of the system, measured by six repeated determinations of the analytes at 1 μg mL^?1 were in the range of 1.6–3.5%.     

Fe-Ni 共掺杂 ZnO 的制备及其光催化降解甲基橙活性

 采用溶液法制备了 Fe-Ni 共掺杂 ZnO 光催化剂, 并运用 X 射线衍射、扫描电镜和原子发射光谱等对催化剂进行了表征. 以甲基橙 (MO) 为模型污染物, 评价了样品的光催化活性, 考察了甲基橙初始浓度及其 pH 值, 以及催化剂用量等对光催化反应性能的影响. 结果表明, Fe-Ni 共掺杂降低了 ZnO 的结晶度, 并促进了晶粒的长大. 光催化降解反应表明, Fe-Ni 共掺杂显著提高了 ZnO 光催化降解甲基橙的活性, 当催化剂用量为 0.6 g/L, 经 120 min 紫外光照射时, 可使甲基橙溶液 (10 mg/L) 降解率达到 93.5%. 关键词：铁; 镍; 共掺杂; 氧化锌; 光催化; 甲基橙; 降解     

PLA制备Tb-Si纳米颗粒及室温光致发光性能研究

采用脉冲激光烧蚀技术(PLA)在n型Si(100)单晶衬底上制备Tb-Si纳米颗粒。原子力显微镜(AFM)观察样品的表面形貌,发现样品表面是均匀分布的纳米颗粒,颗粒尺寸在10~20 nm之间,分布密度大约为6×1010/cm2。光电子能谱(XPS)及高分辨透射电镜(HRTEM)分析表明,纳米尺度的单晶硅化物颗粒的主要成分为Tb-Si及少量Tb-Si-O结构。室温下以荧光为激发光对样品的光致发光(photoluminescence)性能进行测试,结果表明样品在可见光区具有较强的发光现象,主要有4个发光峰,分别位于485,545,585和620 nm附近,这些发光峰主要由Tb3+中电子在不同能级之间的跃迁造成。     

利用非接触式电磁感应线圈探头测液体电导率

采用交流电源激励,自制传感器探头,利用标准电阻定标,得到电导率与输出电压的关系,通过定标曲线,得到不同浓度NaCl溶液的电导率.通过测量探头的频率特性,得到输出电压随频率变化的曲线,选出最佳测量频率.     

Graphene-based passively Q-switched diode-side-pumped Nd:YAG solid laser

In this paper, a desirably simple, convenient and inexpensive saturable absorber mirror has been fabricated based on graphene, which has no wavelength selectivity. Moreover, there are no changes in the structure and characteristics of graphene. By inserting the graphene-PMMA SA mirror to the Nd: YAG laser, the shortest pulse width of 260 ns can be obtained with the single-pulse energy of about 8.32 μJ. The experimental results prove that our graphene-PMMA SA mirror is feasible and suitable for Q-switched lasers.     

碳化铝与水反应合成甲烷水合物的实验研究

 利用自行设计的高压气水合物实验装置,通过碳化铝与水反应成功合成了甲烷水合物。实验结果表明,碳化铝与水反应合成甲烷水合物的方法有效地解决了传统甲烷水合物模拟实验中甲烷气体引入问题;同时,碳化铝与水反应产生的甲烷及沉淀物能较好地模拟海洋环境中水合物形成的自然条件,为实验模拟甲烷水合物研究提供了一种新方法。利用此方法,对甲烷水合物合成与分解温度、压力条件及动力学过程进行了初步研究。     

Large-aperture double-focus laser collimator for PAT performance testing of inter-satellite laser communication terminal

A laser collimator is necessary for testing and verification of the pointing, acquisition and tracking (PAT) performance of inter-satellite laser communication terminals on the ground. The laser collimator must have a large clear aperture to fit the PAT performance testing system. The PAT subsystem has a large field of view for the acquisition and a high angular accuracy for the fine tracking. To resolve the conflict between large field of view and fine angular resolution, a large-aperture double-focus laser collimator is proposed and its optical design and mechanical structure are described. The collimator mainly consists of a primary lens, a reflector, a beam-splitting plate, a secondary lens, two compensating lenses, two imaging sensors and a laser. The primary lens directly forms the long focal length arm of the collimator. The combination of the primary lens and the secondary lens form the short focal length arm of the collimator. The collimator has an angular resolution <0.75 μrad and a 10 mrad field of view. For the collimator, the incident beam is focused on the two imaging sensors by its two arms, and the beam emitted from the laser is collimated and transmitted. The collimator is combined with an optical scanner and a fine beam deflector to test and verify the PAT performance of the inter-satellite laser communication terminal in a full physical manner.     

Modification of nano-fibriform silica by dimethyldichlorosilane

The modification of nano-fibriform silica by dimethyldichlorosilane was studied by transmission electron microscopy, X-ray powder diffraction, infrared spectroscopy, Raman spectroscopy, physical N₂ adsorption techniques, differential thermal and thermogravimetric analysis, scanning electron microscopy, and elemental analyzer.The results show that dimethyl silane derivatives have been successfully covalently grafted on nano-fibriform silica. The polarity of the modified product decreases with the substitution of -OH groups by siloxyl groups. Therefore, the modified product can be easily dispersed in organic solvent and its compatibility with organic molecules is improved. After modification the pore volume decreases and the ductility greatly increases, indicating that the modified product is of a higher strength than before. The study demonstrates that the modified product can be used as an ideal additive to reinforce the strength of organic materials.