吉非替尼的合成新工艺研究

以6-羟基-7-甲氧基喹唑啉-4-酮(1)为起始原料,在离子液体催化下与N-(3-氯丙基)吗啉(2)醚化,然后经氯代再与3-氯-4-氟苯胺进行亲核取代反应,得到目标产物吉非替尼,三步反应总收率为68.7%。通过改变反应物配比、离子液体用量和反应温度,得到了关键中间体3的优化制备工艺条件:n(1)∶n(2)=1.0∶1.2;离子液体四氟硼酸1-甲基-4-丁基咪唑鎓用量为原料1的质量的5%;95℃下反应5h。在此条件下,醚化收率约93.6%。该路线具有反应条件温和、分离简单、路线短和总收率较高的特点,为吉非替尼的工业化生产提供了实验依据。     

The characterization of column heating effect in nanoflow liquid chromatography mass spectrometry (nanoLC‐MS)–based proteomics

Column heating strategy is often applied in nano–high‐performance liquid chromatography–mass spectrometer (nanoHPLC‐MS) platform for enhancing the analytical efficiency of peptides or proteins. Nonetheless, the influence effects of column heating in peptides or proteins identification still lack of deep understanding. In this study, a systematic comparison of room temperature (RT) and column heating of nanoHPLC was done. Based on the data, under column heating condition, the backpressure of nanoHPLC can be decreased. Due to the increase of resolution, the peak widths of precursor ion were narrowed. As a result, in MS/MS data acquisition part, more time was spared for MS1 detecting and MS2 fragmenting, which eventually resulted in increased identification of peptides and proteins. Moreover, we also proposed the application scope of column heating by evaluating its influence on sample detection. On one hand, column heating significantly increased the identification of membrane proteins due to more efficient elution of highly hydrophobic peptides compared with RT. On the other hand, heating was not suitable for analyzing short or/and hydrophilic peptides with low retention time, which would be eluted out during sample loading process under high temperature and missed by mass spectrometric detection. In conclusion, our study provides a reference for rational application of column heating in proteomics research.     

超声抗早孕

控制人口是全球进入２１世纪时所面临的重大问题，我国科研人员率先提出了超声抗早孕的新概念，几年来，从超声工程设备开发到对小鼠，香猪及猴子超声抗早孕的动物实验，做了大量系统的研究工作，所获的研究成果，为超声抗早孕的临床应用展示出令工鼓舞的广阔前景。     

Mössbauer study of the methane oxidative coupling catalysts with K2NiF4 layer structure

Six complex oxide catalysts with K₂NiF₄-type structure were prepared by solid state reaction for methane oxidative coupling (MOC). Mössbauer spectroscopy and other methods were used to identify the structure of the samples and the electronic configuration of iron atoms, and the results were correlated with the MOC reactivity. It is found that the partial substitution of iron in the lattice by Li, Zn or Mg results in the formation of high spin Fe(IV) and surface oxygen species O^?, which are assumed to be responsible for the high activity and C2 selectivity for MOC.     

A novel coupled quantum well structure with large field-induced refractive index change and low absorption loss at 1.55 μm

A novel coupled quantum well structure - quasi-symmetric coupled quantum well (QSCQW) is proposed.In the case of low applied electric field (F = 25 kV/cm) and low absorption loss (α≈ 100 cm-1), a large field-induced refractive index change (for TE mode, △n = 0.0106; for TM mode, △n ＝ 0.0115) is obtained in QSCQW structure at operating wavelength λ =1550 nm. The value is larger by over one to two order of magnitude compared to that in a rectangular quantum well (RQW) and about 50% larger than that of five-step asymmetric coupled quantum well (FACQW) structure under the above work conditions.     

GaAs1×4Mach－Zehnder型光开关列阵研究

采用非对称Ｘ结耦合器设计并研制了ＧａＡｓ１×４Ｍａｃｈ－Ｚｅｈｎｄｅｒ型光开关列阵。简述了非对称Ｘ结和相应的光开关列阵的工作原理及器件的设计和制作过程。在波长为１．１５μｍ的光波下测量单元器件，得到了小于－２０ｄＢ的串音和小于１２Ｖ的开关电压，器件的光波导传输损耗约为７ｄＢ／ｃｍ。文中最后分析了导致器件中串音和损耗的各因素，并提出了可能的改进方法     

肌氨酸的二硫代甲酰化及其电位滴定分析

报道了二硫化碳对肌氨酸（ＳＡ）中仲胺基的二硫代甲酰化（ＤＴＦ）反应及其在ＳＡ定量分析中的应用。上述反应中生成的二硫代甲酰胺（ＤＴＦＡ）基团可以通过电位滴定确定含量，从而求得ＳＡ含量。加入回收试验表明该法对ＳＡ的适宜检测浓度范围为１￣１５ｇ／Ｌ；相对标准偏差〈１．０％。该法用于化学合成ＳＡ的含量测定，简便、快捷，准确。     

A study on the reduction behayior of Fe_2(MoO_4)_3 with a combined in-situ temperature-programmed reduction- Mossbauer spectroscopic technique

In H2/N2 atmosphere, the reduction behavior of the stoichiometric compound, Fe2(MoO4)3, was studied by in-situ Mossbauer spectroscopy (in-situ MBS), temperature-programmed reduction (TPR) and X-ray diffraction (XRD). The results showed that the reduction products, β-FeMoO4, Mo4O11, MoO2, Fe3O4, Fe2Mo3O8, Fe and Mo, as well as iron-molybdenum alloys, were formed subsequently when the reduction temperature was raised. It was found that when Mo6+ were reduced to Mo4+, Fe2+ were oxidized to Fe3+. Due to the interactions among the metal ions and the electron transfers, the reduction processes of the metal ions in Fe2(MoO4)3 are very complex. According to the results of XRD and MBS obtained at various TPR stages, the reaction equations for the reduction stages were proposed. The Mossbauer spectrum of an intermediate species, Fe2Mo3O8, was found to exhibit two doublets, with I.S.=0.90mm/s and Q.S. =0.58 mm/s, and I.S. = 1.02mm/s and Q.S. = 1.04mm/s, respectively.     

石墨炉原子吸收光谱中GdCl3,Gd（NO3）3基体的背景吸收

研究了石墨炉原子吸收光谱中ＧｄＣｌ３、Ｇｄ（ＮＯ３）３基体的背影吸收影响。背景吸收波长特性的研究表明，ＧｄＣｌ３和Ｇｄ（ＮＯ３）３的背景吸收都具有明显的波长特性。蒸发行为研究表明ＧｄＣｌ３的背景吸收主要来自ＧｄＣｌ３的分子蒸气，Ｇｄ（ＮＯ３）３的背景吸收主要来自ＮＯ。钆基体的背景吸收峰高与灰化有关，ＧｄＣｌ３背上曲线轮廓与原子化温度和原子化方式有关。Ｇｄ（ＮＯ３）３的背景吸收远小于ＧｄＣｌ３。本文     

恒温洗浴热水添加策略研究

用户和商家都期望有自动化程度高的浴缸加水系统出现,既能使浴缸中的水长时间保持恒定的舒适温度,又尽可能节约热水。综合考虑影响浴缸水温的各种因素,建立了浴缸加水的2个数学模型:热传输模型和微分方程模型。通过分析求解2个模型,分别给出包含加水时间和流速等信息的最优加水方案。最后对2个模型进行比较,推荐最优加水方案,从而为生产厂家制定智能加水系统提供理论支持。