Concentration and clean-up of trace hydrocarbons from atmospheric particulate matter

Summary The aim of this work is to establish the best conditions for concentration and purification steps in the trace analysis of aliphatic and polycyclic aromatic hydrocarbons (PAH) from atmospheric particulate matter by gas chromatography-flame ionisation detection (GC-FID) and high performance liquid chromatography with ultraviolet and fluorescence detection (HPLC-UV-FL). The best results for the more volatile compound were obtained with a combination of rotary evaporation and a stream of nitrogen (near to 100% for aliphatic hydrocarbons and from 70 to 105% for PAH). Two types of solid phase extraction (SPE)cartridges (Supelclean ^tm LC-Silica SPE tubes and Sep-Pak^? Plus silica cartridges) and glass column were examined for the purification and fractionation step. Blank chromatograms of both types of cartridges analysed by GC-FID made this study difficult, because a PSS (programmed split-splitless) injector was employed thereby increasing the sensitivity. This problem was not observed in the HPLC-UV-FL blank chromatograms of these cartridges. Glass columns filled with silica and alumina were chosen because no interference was found in the GC-FID blank chromatograms and the best recoveries in the fractionation of both aliphatic hydrocarbons and PAH were achieved. This is especially important when aliphatic hydrocarbons concentrations are lower than 1 μg mL⁻¹. Finally, the selected conditions were applied to the analysis of hydrocarbons in real atmospheric particulate samples.     

胍类化合物的合成进展

胍类化合物是精氨酸残体的一部分，它在具有生物活性的蛋白质、肽中起着重要作用，从天然产物分离得到的胍类化合物大部分具有生理活性，如抗病毒、抗肿瘤、抗艾滋病等。所以，在温和条件下高产率的合成胍类化合物显得非常重要。本文综述了胍类化合物的合成进展。参考文献32篇。     

电子俘获材料Zn_4B_6O_(13)∶Dy~(3+)的热释光特性研究

通过高温固相扩散反应合成了稀土元素镝掺杂的 Zn4 - x B6 O1 3∶ x Dy3+ 磷光体 .测定了该化合物在高能6 0 Co伽玛射线辐照下的热释发光曲线和三维热释光谱 .三维热释光谱表明 ,位于大约 480 nm和 5 80 nm的发光谱带来自于 Dy3+ 离子的 f-f 跃迁 .基质中掺杂的 Dy3+ 离子浓度的变化能够改变陷阱的相对分布 ,随着Dy3+浓度的增加 ,发光峰温向高温方向移动 ,这可提高剂量器的热稳定性 .当辐照剂量增加时 ,发光峰温亦向高温方向移动 ,即陷阱加深 .确定了 Zn3.86 B6 O1 3∶ 0 .1 6Dy3+样品主峰的陷阱深度 E=0 .73 e V,频率因子S=2 .43× 1 0 9s- 1 .在 1～ 1 0 0 Gy治疗级范围内 ,Zn3.86 B6 O1 3∶ 0 .1 6Dy3+ 对 6 0 Co伽玛射线辐照的热释光剂量响应呈良好的线性关系 .实验结果表明 ,Zn3.86 B6 O1 3∶ 0 .1 6Dy3+是一个潜在的应用于临床医疗的伽玛射线电离辐射热释光剂量计材料 .     

线性扫描极谱法测定微量肉桂酸

在 1mol·L-1HOAc NaOAc介质中 (pH =3.6 ) ,肉桂酸有一还原峰 ,其峰电位为 - 1.4 7V(vs.SCE)。峰电流与肉桂酸浓度在 2 .0× 10 -5～ 8.0× 10 -4 mol·L-1之间呈线性关系 (r =0 .9989) ,检出限为 1.0× 10 -5mol·L-1。该法应用于肉桂酸含量的测定 ,结果满意 ,并对肉桂酸的电化学性质进行了研究     

Monitoring the Hydrolysis of p—Nitrophenyl Acetate Catalyzed by Seryl—histidine with Electrospray Ionization Mass Spectrometry

ＩｎｔｒｏｄｕｃｔｉｏｎＩｎｔｈｅｐａｓｔｄｅｃａｄｅ ,ｉｔｗａｓｆｏｕｎｄｔｈａｔｔｗｏａｍｉｎｏａｃｉｄｒｅｓｉｄｕｅｓ ,ＳｅｒａｎｄＨｉｓ ,ｗｏｒｋａｓｔｈｅａｃｔｉｖｅｓｉｔｅｓｉｎｔｈｅｓｅｒ ｉｎｅｐｒｏｔｅａｓｅ .1 3 Ｉｎｏｕｒｐｒｅｖｉｏｕｓｗｏｒｋ ,ａｄｉｐｅｐｔｉｄｅｓｅｒｙｌ ｈｉｓｔｉｄｉｎｅ (Ｓｅｒ Ｈｉｓ)ｗａｓｆｏｕｎｄｔｏｈａｖｅｔｈｅｐｒｏｔｅｉｎａｎｄｎｕ ｃｌｅｏｓｉｄｅｓｃｌｅａｖａｇｅａｃｔｉｖｉｔｙ .4 7ｐ Ｎｉｔｒｏｐｈｅｎｙｌａｃｅｔａｔｅ (ｐ ＮＰＡ)ｗ…     

4－（2－氨基噻唑）－间苯二酚为柱前衍化剂液相色谱／电化学检测Fe、Co、Ni

４－（２－氨基噻唑）－间苯二酚为柱前衍化剂液相色谱／电化学检测Ｆｅ、Ｃｏ、Ｎｉ格日勒，李惠梅，李南强，汪尔康（中国科学院长春应用化学研究所电分析化学开放实验室，北京大学化学系，长春，１３００２２）关键词液相色谱，Ｆｅ，Ｃｏ，Ｎｉ，４－（２－氨基噻唑）...     

吡啶二甲酸镓、铟配合物的合成及生物活性

吡啶二甲酸能与过渡、非过渡、镧系和锕系金属离子螯合形成稳定的配合物，而且配位方式不拘一格，既可以是双齿，三齿，也可以是桥式配位。吡啶二甲酸的另一重要意义在于它们的生物活性。由于镓具有抗癌，抗肿瘤的活性，吡啶二甲酸镓配合物可能会是一种非常有潜力的新型药物。基于上述事实，本文合成了六种新型的吡啶二甲酸（2，3-，2，5-，2，6-）镓（Ⅲ）、铟（Ⅲ）配合物，并进一步测试了三种镓配合物的生物活性。     

毛细管气相色谱法测定染发剂中七种染料组份

采用毛细管气相色谱法对染发剂中苯酚、邻苯二酚、对苯二酚、间苯二酚、邻苯二胺、对苯二胺和间苯二胺七种染料进行了分析。结果表明，该方法能有效地分离这七种染料，其检出限为苯酚50ng、邻苯二胺160ng、对苯二胺240ng、邻苯二酚280ng、间苯二胺180ng、对苯二酚190ng、间苯二酚180ng。方法测定精密度为2.07-4.33％，回收率为96.1％-103.3％。方法具有操作准确、简单、快速、实用等特点。     

Synthesis and Characterization of Novel Orange-emitting Iridium（Ⅲ） Complexes with Diphenylquinoline Ligands Containing Fluorinated Substituent

Three new cyclometalated iridium（m） complexes based on ligands of diphenylquinoline with fluorinated subsfituents were prepared, and characterized by elemental analysis （EA）, ^1H NMR, and mass spectroscopy （MS）. The photophysical and electrophosphorescent properties of the complexes were briefly discussed.