Synthesis, Crystal Structure and Antiproliferative Activity of 2,2-Dimethyl-4-oxochroman-3-ylmorpholine-4-carbodithioate

The crystal structure of the new title compound 2,2-dimethyl-4-oxochroman-3-ylmorpholine-4-carbodithioate(C16H19NO3S2,Mr = 337.44) has been prepared and determined by single-crystal X-ray diffraction.The crystal is of triclinic,space group P1 with a = 9.5518(7),b = 9.7172(7),c = 11.0220(8),α = 67.08(1),β = 74.66(1),= 61.31(1)°,V = 822.72(10)3,Z = 2,Dc = 1.362 g/cm3,F(000) = 356,μ = 0.092 mm-1,MoKa radiation(λ = 0.71073),R = 0.0515 and wR = 0.1389 for 2623 observed reflections with I > 2(I).X-ray diffraction analysis reveals that the chroman ring adopts a half-chair conformation while the morpholine ring shows a chair conformation.Intramolecular and intermolecular C-H···S and C-H···O hydrogen bonds together with π-π interations are found in the structure.The result of MTT assay shows the title compound displays good antiproliferative activity against two human cancer cell lines.     

酸性功能化离子液体催化“一锅法”合成酰胺烷基萘酚

用磺酸型离子液体1-甲基-3-磺酸丙基咪唑硫酸氢盐([MIMPS][HSO₄])催化β-萘酚、芳香醛和酰胺（或脲）3组分“一锅法” 类Ritter反应合成了酰胺烷基萘酚。 投料比为n(β-萘酚)∶n(芳香醛)∶n(酰胺或脲)∶n([MIMPS][HSO₄])=1∶1∶1.3∶0.1,无需溶剂,恒温125 ℃反应5～40 min,通过简单水洗抽滤即可分离产物,酰胺烷基萘酚产率为85%～97%。 离子液体[MIMPS][HSO₄]可回收重复使用4次,其催化活性无明显降低。 探讨了醛、酰胺或脲结构对反应的影响及可能的反应机理。     

纳米氧化锌的微乳液法制备

纳米ZnO颗粒尺寸较小,比表面积较大,其粉体具有非常高的化学活性,表现出表面与界面效应、小尺寸效应、量子尺寸效应和宏观量子隧道效应.纳米ZnO在电、磁、光、热等方面具有一般ZnO所无法比拟的性能,广泛用于气体敏感材料、涂料和高效催化剂等许多领域.因而,制备高质量的纳米ZnO是非常重要的.     

活性炭自水溶液中吸附酚的热力学与机理研究

研究了水溶液中活性炭分别吸附苯酚、邻甲酚过程热力学与机理, 测定了不同温度下的吸附等温线。结果表明, 常温下稀溶液中, 苯酚以垂直与平伏混杂取向被吸附, 高浓度时则以垂直取向为主。邻甲酚以平伏聚向被吸附且取向几乎不受浓度变化的影响, 但受温度的影响, 55~60℃时, 吸附情况与苯酚相似。体系的热力学与吸附机理关系密切。垂直吸附的熵变较小, 平伏吸附的熵较大。对产生上述现象的原因, 本文进行了分析讨论, 并由此阐明了其它固-液吸附体系中的一些问题。     

A High Yield Method of Extracting Alkaloid from Aconitum coreanum by Pulsed Electric Field

A high yield method to extract alkaloids from Aconitum coreanum using pulsed electric field (PEF) was developed, and the optimized extraction method compared to the other four extraction methods, consisting of cold maceration extraction, percolation extraction, heat reflux extraction (HRE), and ultrasonic-assisted extraction (UE). The experimental factors of the extraction methods such as electric field intensity, pulse frequency and solid-to-solvent ratio were evaluated. The content of Guanfu base A (GFA) was quantified by liquid chromatography coupled with electrospray ionization tandem mass spectrometry. The results indicated that the highest yield of GFA was 3.94 mg g^?1 by PEF with conditions of 20 kV cm^?1 electric field intensity, 8 pulse, 1:12 solid-to-solvent ratio, and 90 % ethanol–water solution. Meanwhile, the extraction time of PEF was <1 min, which is much less than the HRE of 10 h and even the newly used technique UE of 40 min. Moreover, the results of PEF extraction method showed obvious advantages, with the highest efficiency (120 L h^?1), the shortest extraction time (0.5–1 min), and the lowest energy costs, which could be applied in the industrial production of alkaloids from A. coreanum. Therefore, the application of the PEF extraction method is a promising and constructive method for extraction of GFA.     

四苯基钴卟啉化合物催化过亚硝酸根分解的研究

利用紫外-可见分光光度计在乙醇介质中研究了合成的4种对位取代四苯基钴卟啉对过亚硝酸根分解的催化作用. 首次发现钴卟啉可以催化ONOO^－分解, 且对位带吸电子基团的钴卟啉比对位带供电子基团的钴卟啉催化活性高. TPPCoCl, T(p-CH₃)PPCoCl, T(p-OCH₃)PPCoCl和T(p-Cl)PPCoCl在乙醇中的k_cat分别为1.69×10², 1.52×10², 1.43×10²和1.20×10³ mol^－1•L•s^－1. 动力学曲线和时间分辨谱证明这些钴卟啉是通过形成中间体催化过亚硝酸根分解的.     

金属-有机纳米管分散固相萃取-气相色谱-串联质谱高灵敏分析环境水样中痕量多氯联苯

采用含铅金属-有机纳米管为吸附剂,基于分散固相萃取和气相色谱-串联质谱建立了一种高灵敏分析环境水样中痕量多氯联苯的方法.采用正交设计响应面法对影响萃取效果的重要因素(如离子强度、萃取时间和吸附剂用量等)进行了优化.获得的最优条件为:离子强度4.92 %(w/V)NaCl,萃取时间4.5 min,正己烷为解吸剂,吸附剂用量62.5 mg.在优化条件下,方法的线性范围为2~1000 ng/L,检出限为0.26~0.82 ng/L. 日内和日间相对标准偏差分别为0.8%~5.5% (200 ng/L, n=6)和2.7%~7.4% (200 ng/L, n=6).将本方法应用于实际环境水样中多氯联苯的分析,回收率为78.9%~113.3%,结果满意.     

固相萃取/高效液相色谱-串联质谱法测定黄瓜及土壤中的春雷霉素残留

建立了测定黄瓜和土壤中春雷霉素残留的固相萃取/高效液相色谱-串联质谱(SPE/HPLC-MS/MS)方法。黄瓜和土壤样品分别经1%甲酸的甲醇、0.5%甲酸水提取后,采用MCX固相萃取柱净化,以Waters Xbridge BEH Amide色谱柱分离,0.2%甲酸水-乙腈溶液进行梯度洗脱,电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式检测,基质匹配标准曲线外标法定量。该方法灵敏、准确、简单快速、重复性好,在2~250μg/L浓度范围内,不同基质中春雷霉素的线性相关系数均大于0.999,检出限为0.002 mg/kg,定量下限为0.008 mg/kg;在0.008、0.040、0.200、0.400 mg/kg 4个加标水平下,春雷霉素在黄瓜和土壤样品中的平均回收率为77.5%~97.0%,相对标准偏差为2.6%~10.7%,能够满足黄瓜及土壤中春雷霉素残留的检测需求。应用该法对田间样品进行检测,结果表明,春雷霉素在黄瓜中的残留量不超过0.053 mg/kg,小于我国规定的黄瓜中最大残留限量(0.2 mg/kg);土壤中春雷霉素的残留量不超过0.013 mg/kg。     

钒毒性的研究进展

综述了钒的一般毒性，生殖毒性，胚胎毒性，致畸，致突变，致癌毒性的研究进展。