密胺-脲甲醛树脂合成工艺放大研究

以密胺－脲甲醛树脂合成的小试工艺条件为依据，完成了放大试验过程的工艺研究。研究结果与小试研究的工艺条件相吻合。     

Comparisons of NMR spectral quality and success in crystallization demonstrate that NMR and X-ray crystallography are complementary methods for small protein structure determination

X-ray crystallography and NMR spectroscopy provide the only sources of experimental data from which protein structures can be analyzed at high or even atomic resolution. The degree to which these methods complement each other as sources of structural knowledge is a matter of debate; it is often proposed that small proteins yielding high quality, readily analyzed NMR spectra are a subset of those that readily yield strongly diffracting crystals. We have examined the correlation between NMR spectral quality and success in structure determination by X-ray crystallography for 159 prokaryotic and eukaryotic proteins, prescreened to avoid proteins providing polydisperse and/or aggregated samples. This study demonstrates that, across this protein sample set, the quality of a protein's [15N-1H]-heteronuclear correlation (HSQC) spectrum recorded under conditions generally suitable for 3D structure determination by NMR, a key predictor of the ability to determine a structure by NMR, is not correlated with successful crystallization and structure determination by X-ray crystallography. These results, together with similar results of an independent study presented in the accompanying paper (Yee, et al., J. Am. Chem. Soc., accompanying paper), demonstrate that X-ray crystallography and NMR often provide complementary sources of structural data and that both methods are required in order to optimize success for as many targets as possible in large-scale structural proteomics efforts.     

四磺化酞菁钴在微乳液、醇-水体系中的二聚现象研究

采用分光光度法研究了四磺化酞菁钴（ＣｏＴＳＰｃ），在微乳液（ＴｒｉｔｏｎＸ－１００－壬烷－正戊醇－水）、醇－水（甲醇、乙醇、丙醇）体系中的二聚现象，计算了ＣｏＴＳＰｃ的二聚常数ＫＤ。结果表明，ＣｏＴＳＰｃ的二聚常数ＫＤ值随着微乳液中表面活性的浓度及醇－水溶液的介电常数的增加而减小。     

无液接裸露式Ag/AgCl参比电极的研制及应用

提出了一种无液接裸露式Ag/AgC l参比电极制备方法,测试了该参比电极的稳定性、重现性、可逆性、响应时间、温度影响等因素。实验结果表明,该电极电位稳定在49 mV,响应时间在30 s以内时,具有重现性、可逆性好,使用寿命长,温度影响小等特点,可替代饱和甘汞和Ag/AgC l参比电极。     

双8-羟基喹啉端开链冠醚金属络合物的光物理性质

设计合成了双8-羟基喹啉端的开链冠醚QP3Q,研究了金属离子铝或锌与其形成络合物的组成和发光性质,并测定了络合物的激发态寿命.这些络合物在溶液中有较高的荧光量子产率,所得到的络合物固体具有较强的蓝光发光性能.结果表明,有可能通过QP3Q与不同离子形成的络合物得到不同发光波长的发光材料.     

同步辐射白光全反射XRF在痕量元素检测的初步应用研究

叙述了同步辐射白光全反射Ｘ射线荧光分析的实验装置，给出了几种标准物质ＴＸＲＦ实验的检出限，并对实验结果进行了讨论。     

An Efficient and Green Synthesis of 5-Oxo-5, 6, 7, 8-tetrahydro- 4H-benzo-[b]-pyran Derivatives Promoted by InCl_3·4H_2O Under Microwave Irradiation

Construction of tetrahydropyran rings has attracted a great deal of interests in organic synthesis in recent years1, since tetrahydropyran moiety constitutes a structural unit in a number of natural products2. In addition, tetrahydropyran derivatives possess wide range of biological activities and pharmacological properties, such as anticancer activity3 and antihypersensitivity4. Many methods for the preparation of such compounds have already been developed5. Among them, condensation of α, β…     

六(乙氧基吡咯烷酮)三聚磷腈的合成与表征

以N-羟乙基吡咯烷酮与氢化钠作用生成相应的钠盐,再将此钠盐与六氯三聚磷腈(HCCP)发生亲核取代反应,合成了六(乙氧基吡咯烷酮)三聚磷腈,用IR、31P NMR、1H NMR、13C NMR、DEPT、FABMS等现代谱学技术对其结构进行了表征。生物活性试验表明,此化合物1mg/mL时对腐生线虫Panagrellus redivivus的72h致死率为52·7%。     

丙酮在XeCl准分子激光辐射下的多光子电离和碎裂研究

我们用扩散分子束多光子电离光谱技术研究了丙酮在XeCl准分子激光辐射下的多光子电离和碎裂行为。实验表明丙酮没有产生母体离子峰(m/e=58), 只给出m/e=43和15两个峰, 分别对应于丙酮光解所产生的两个碎片CH_3 CO和CH_3。其离子信号(1)分别与激光强度(Ⅰ)的3和3.6次方成正比。分析表明离子是由中性碎片电离产生的。     

纳米多孔双金属氧化物在镍钛合金纤维上的原位生长及其对多环芳烃的选择性固相微萃取

采用阳极氧化法在镍钛合金(NiTi)纤维上原位生长了双金属氧化物纳米孔(NiTiONPs)涂层,通过扫描电镜(SEM)和能谱(EDS)考察了电解质组成和电压对形貌的影响。将NiTiONPs涂层的NiTi纤维与高效液相色谱-紫外检测器联用,研究了4种典型芳香分析物的萃取性能。结果表明,富含TiO2的NiTiONPs涂层对多环芳烃(PAHs)具有良好的萃取效率,尤其对苯并[a]芘的萃取选择性优于市售聚二甲基硅氧烷纤维和聚丙烯酸酯纤维。在优化条件下,PAHs的线性范围为0.05~200μg/L,相关系数均大于0.999,检出限为0.012~0.134μg/L。对单支纤维日内和日间分析的相对标准偏差(RSDs)分别为4.0%~5.5%和6.0%~6.8%,使用分批组装的5支纤维分析的RSDs为6.4%~7.6%。实际水样分析的加标回收率为84.5%~111.5%。所制备NiTi纤维至少可重复使用250次以上,重现性好。