Poly[bis(μ‐4‐benzoyl‐1‐isonicotinoylthiosemicarbazide‐κ2N:S)dichloridocadmium(II)]

The asymmetric unit of the title complex, [CdCl₂(C₁₄H₁₂N₄O₂S)₂]_n, consists of one Cd^II ion located on the crystallographic inversion centre, one 4‐benzoyl‐1‐isonicotinoylthiosemicarbazide ligand and one chloride ligand. The central Cd^II ion adopts a distorted octahedral coordination geometry formed by two pyridyl N atoms of two ligands, two S atoms of two other ligands and two chloride ligands. The thiosemicarbazide ligands act as bridges, linking the metal ions into a two‐dimensional layered structure parallel to the bc plane. Intermolecular N—H...O hydrogen bonds and C—H...π interactions exist between adjacent layers.     

抽提物对生物质热裂解机理的影响研究

利用惰性溶剂从生物质中提取得到相应抽提物,在热重红外联用仪上研究了抽提物的热裂解行为,并探讨了其对生物质热裂解的影响。结果表明,因不同种类生物质中木质素结构单元中紫丁香基和愈创木基数量不同,从而导致抽提物成分存在差异,相应的热裂解产物分布也不一致。水曲柳抽提物因含有较多的酚类物质而在热解高温段生成了甲醇和甲烷。相比于原样,抽提残渣反应活化能增加,且主要产物析出时间提前,同时酸类物质和直链烷烃析出量减少,而水、CO2、CO和醛类物质的产量则有所增加。     

不同位置取代的噻唑烷-4-羧酸及其衍生物的研究进展

综述了近几十年来取代的噻唑烷-4-羧酸及其衍生物的研究进展及其在有机合成、药物合成、化学分析和化学计算中的应用.     

气相色谱/质谱法检测小鼠肌肉组织和血液中羟基多氯联苯

建立了测定小鼠肌肉和血液中3种羟基多氯联苯的气相色谱/质谱联用(GC-MS)方法.经正己烷-乙酸乙酯(1∶ 1, V/V)提取目标化合物后,结合H2SO4去脂,KOH反萃法对提取液进行净化,以双(三甲基硅烷基)三氟乙酰胺-三甲基氯硅烷(BSTFA-TMCS, 99∶ 1, V/V,)为衍生试剂对羟基多氯联苯进行硅烷化衍生后,在SIM模式下进行GC/MS分析.本方法检出限为2μg/kg.在3种添加水平2.0,5.0和20.0 μg/kg下,小鼠肌肉和血液中3种羟基多氯联苯的回收率范围为73.2%～113.2%;相对标准偏差为1.53%～10.4%.本方法可用于小鼠腹腔注射多氯联苯后,体内多氯联苯羟基代谢物的检测.     

高效液相色谱-电喷雾银离子诱导电离飞行时间质谱定性分析高沸点多环芳烃

建立了高效液相色谱-电喷雾飞行时间质谱联用技术快速鉴别高沸点多环芳烃的方法。多环芳烃经色谱柱分离后,通过柱后添加AgNO3溶液诱导其在电喷雾离子源中电离,生成多环芳烃[M]+及其复合[M+Ag]+和[2M+Ag]+特征离子,根据所获得的各特征离子的精确分子量和分子式,可实现多环芳烃类化合物的快速鉴别。将本方法用于美国环保局(USEPA)规定的16种优先控制多环芳烃及原油中多环芳烃类化合物的分析鉴别,结果表明,四环以上的PAHs质谱信号良好,说明本方法适用于四环以上的高分子量、高沸点多环芳烃类化合物的分析鉴别。     

毛细管电泳吡啶钌电化学发光检测天仙子中生物碱

1 引言 天仙子是一种天然中草药,它的主要活性成分为阿托品和东莨菪碱 .目前,分析天仙子的方法主要有:核磁共振技术、紫外分光光度法、高效液相色谱法和毛细管电泳分离法等.毛细管电泳技术(CE)具有进样体积小、分离效率高等优势.吡啶钌(Ru(bpy)2+3)电化学发光法具有激发态寿命长、发光效率高、试剂可循环再生等优点. CE与Ru(bpy)2+3电化学发光联用技术(CE-ECL)将二者优势有机组合,已成为分析化学领域中很好的分析工具.     

基于聚酰胺6纳米纤维膜的固相萃取-高效液相色谱法测定兔血浆中酮康唑对映体

以基于聚酰胺6纳米纤维膜的固相萃取法,结合高效液相色谱手性流动相添加剂法测定了兔血浆中的酮康唑对映体的浓度。仅用1.5mg聚酰胺6纳米纤维膜、100μL甲醇即可完成目标物的富集和洗脱。酮康唑的2个对映体在50.0～400.0μg/L范围内呈良好的线性;方法的定量限为40.0μg/L;日内和日间精密度分别小于6.3%和8.6%;平均绝对回收率为79.4%～85.6%;平均相对回收率为90.0%～96.5%。本方法灵敏、准确、重现性好,符合生物样本中酮康唑对映体分析测定的要求。     

Reaction mechanism of methanol decomposition on Pt‐based model catalysts: A theoretical study

The decomposition mechanisms of methanol on five different Pt surfaces, the flat surface of Pt(111), Pt‐defect, Pt‐step, Pt(110)(1 × 1), and Pt(110)(2 × 1), have been studied with the DFT‐GGA method using the repeated slab model. The adsorption energies under the most stable configuration of the possible species and the activation energy barriers of the possible elementary reactions involved are obtained in this work. Through systematic calculations for the reaction mechanism of methanol decomposition on these surfaces, we found that such a reaction shows the same reaction mechanism on these Pt‐based model catalysts, that is, the final products are all H (H_ads) and CO (CO_ads) via O? H bond breaking in methanol and C? H bond scission in methoxy. These results are in general agreement with the previous experimental observations. © 2010 Wiley Periodicals, Inc. J Comput Chem, 2010.     

Redox‐induced configuration conversion for thioacetamide dimer can function as a molecular switch

The electronic switching properties of thioacetamide dimer (TAD) were investigated using the nonequilibrium Green's function method combined with density functional theory for design of a novel molecular switch. The H‐bonded TAD can be converted upon hole‐trapping to a three‐electron (3e)‐bonded configuration with a S∴S linkage which could provide a more favorable channel for charge transfer than the before. The redox‐induced configuration conversion between the H‐bonded and the 3e‐bonded TADs could govern the charge migration through the molecular junction with a considerable difference in conduction currents. The calculated I–V characteristic curves of two configurations exhibit a switching behavior with an On‐Off ratio in a range of about 4.3–7.6 within the applied voltages. Clearly, this hypothetical scheme provides a potential way to explore the novel conformation‐dependent molecular switch. © 2010 Wiley Periodicals, Inc. J Comput Chem 2010     

Development of a capillary gel electrophoresis method for monitoring disulfide isomer heterogeneity in IgG2 antibodies

A CGE method for monitoring the disulfide isomer distribution characteristic of IgG2 MAbs is presented. Disulfide heterogeneity of MAbs has been studied using various chromatographic and electrophoretic methods. Although CGE operates using a different selectivity mechanism from that of sorption chromatographic techniques, similar trends are present in the data, which allow the CGE method to be used as a complementary method for studying disulfide isomer distribution. This article focuses on the optimization of a capillary‐based gel electrophoresis method that can be used to support antibody development including bioprocess optimization, antibody characterization, release, and formulation stability assessment.