Development and validation of a derivative ultraviolet spectrophotometric method for the determination of darifenacin in tablets using experimental designs and its comparison with chromatographic method

A set of experimental designs was applied to develop and validate a spectrophotometric method using derivative transformation coupled with zero-crossing methodology for the quantification of darifenacin hydrobromide in extended-release tablet form. In the presence of the matricial interference, a central composite (face-centered) design was necessary to reach the best condition without interference in the quantification. The optimal system was confirmed using the function named Derringer’s desirability to assess high precision and low quantification limit. The best condition pointed was the first order to derivative transformation, Δλ = 4, scale factor 150, scanning speed 280 nm/s and anulation point in 239.4 nm as wavelength. From these parameters it was possible to perform the method validation resulting in R ² = 0.999, concentration ranging from 0.10 to 2.50 μg/mL, recovery 98.65% and mean precision 97.67% (RSD = 0.0136). Additionally, robustness was assessed by a Plackett-Burman design, and no significant variability was obtained. The spectrophotometric method was compared with high-performance liquid chromatography method, resulting in no significant difference between the methods.     

磁性纳米颗粒系统偶极相互作用的Monte Carlo研究

采用局域Monte Carlo方法模拟不同易轴分布的简单立方排列单分散单畴Fe纳米颗粒系统的ZFC-FC曲线及磁滞回线.结果表明：随着偶极相互作用的增强，系统的阻塞温度T_B逐渐增大，且ZFC曲线的峰变宽.说明偶极相互作用使得系统的有效能垒提高，分布宽度增加.研究FC曲线磁化强度的倒数与温度关系，发现偶极相互作用系统中存在反铁磁有序.系统的阻塞态及超顺磁态的磁滞回线表明，极低低温下，随着偶极相互作用的增强，系统的矫顽力和剩磁减小，偶极相互作用阻碍系统的磁化；系统处于超顺磁态，各向异性作用及偶极相互作用使得系统的磁化曲线偏离Langevin曲线且偶极相互作用展现出退磁相互作用效应.偶极相互作用增强，系统磁化曲线与Langevin曲线偏差量的最大值向低场移动.在偶极相互作用下，易轴与外场夹角为45°的磁性纳米颗粒系统的平均有效能垒和有效能垒分布宽度较易轴随机分布系统的大.     

Microwave-Assisted Direct Synthesis of 4H-1,2,4-Benzothiadiazine 1,1-Dioxide Derivatives

Abstract

We describe a rapid and convenient methodology for the preparation of diverse 3-aryl and 3-trifluoromethyl 4H-1,2,4-benzothiadiazine-1,1-dioxides in a one-pot microwave-promoted reaction between 2-aminobenzenesulfonamides and benzaldehydes, trifluoroacetic acid or benzoic acids.

GRAPHICAL ABSTRACT      

Br-掺杂Bi2WO6的水热法合成及其可见光催化性能

以Bi（NO₃）₃·5H₂O和Na₂WO₄·2H₂O为主要原料,采用水热法合成了纯相Bi₂WO₆,并对其进行非金属离子Br^-掺杂改性。采用XRD、SEM、TEM、XPS、Raman、PL和DRS研究了Br^-掺杂对Bi₂WO₆的物相结构、形貌和可见光催化性能的影响。结果表明,Br^-掺杂可有效提高Bi₂WO₆的可见光催化性能,当掺杂量（物质的量百分数）为8%时,溴掺杂Bi₂WO₆的光催化性能最好,可见光照射40 min后,可降解96.73%的罗丹明-B,与未掺杂Bi₂WO₆相比,其降解率提高了36.32%。     

一种二维多孔窗口型膦酸锆材料的合成及其对不同金属离子的吸附性能

合成了一种二维窗口型膦酸锆材料β-丙氨酸-N,N-双亚甲基膦酸锆(ZrNCP),采用X射线衍射仪、扫描电镜、透射电镜分析了合成产物的相组成和微观结构;利用N2吸脱附试验装置测定了合成产物对不同金属离子的吸附性能,考察了浓度、温度及pH对其吸附性能的影响.结果表明,合成产物内部存在大量分布均匀的微介孔,材料微观形貌为规整片状.随着金属离子半径的增大,ZrNCP对各种金属离子的平衡吸附量(mmol/g)呈逐渐减小趋势.     

Reactivity Studies of Iridium Pyridylidenes [TpMe2Ir(C6H5)2(C(CH)3C(R)NH] (R=H,Me, Ph)

The reactivity of a series of iridium? pyridylidene complexes with the formula [Tp^Me2Ir(C₆H₅)₂(C(CH)₃C(R)N H] ( 1 a – 1 c ) towards a variety of substrates, from small molecules, such as H₂, O₂, carbon oxides, and formaldehyde, to alkenes and alkynes, is described. Most of the observed reactivity is best explained by invoking 16 e^? unsaturated [Tp^Me2Ir(phenyl)(pyridyl)] intermediates, which behave as internal frustrated Lewis pairs (FLPs). H₂ is heterolytically split to give hydride? pyridylidene complexes, whilst CO, CO₂, and H₂C?O provide carbonyl, carbonate, and alkoxide species, respectively. Ethylene and propene form five‐membered metallacycles with an IrCH₂CH(R)N (R=H, Me) motif, whereas, in contrast, acetylene affords four‐membered iridacycles with the IrC(?CH₂)N moiety. C₆H₅(C?O)H and C₆H₅C?CH react with formation of Ir? C₆H₅ and Ir? C?CPh bonds and the concomitant elimination of a molecule of pyridine and benzene, respectively. Finally the reactivity of compounds 1 a – 1 c against O₂ is described. Density functional theory calculations that provide theoretical support for these experimental observations are also reported.     

电感耦合等离子体-发射光谱法测定纯锑中硫的含量

建立了用电感耦合等离子体-发射光谱法(ICP-AES)测定锑锭中硫元素含量的分析方法。样品用王水溶解,加入适量的酒石酸作为稳定剂,稀释定容后直接进行ICP-AES分析。硫元素的测定下限为0.0008%;0.20μg/mL的硫标准溶液平行7次进样的相对标准偏差为3.7%。利用所建立的方法,对两个批次的锑锭进行了分析,加标回收率分别为96.0%和100.6%,并与国标分析方法进行了实验数据比对。     

扫帚状氧化铈制备及其对Pt基阳极催化剂催化性能的影响

采用水热合成法,合成了比表面积为175 m²·g^-1,孔径在2~4nm范围内的扫帚状CeO₂。通过微波辅助乙二醇还原氯铂酸法制备了Pt-CeO₂/RGO催化剂,探究扫帚状CeO₂的添加对Pt基催化剂电催化性能的影响。利用X射线衍射仪（XRD）、扫描电镜（SEM）、N₂吸附-脱附、X射线光电子能谱（XPS）对所制备的CeO₂及催化剂进行表征。利用电化学工作站对催化剂进行电化学性能测试。结果表明,催化剂中CeO₂保持原有扫帚状,Pt纳米粒子均匀分布于石墨烯载体表面;当m_RGO∶m_CeO2=1∶2时,添加了扫帚状CeO₂的Pt-CeO₂/RGO催化剂的电催化性能最优,电化学活性表面积为102.83 m²·g^-1,对乙醇氧化的峰值电流密度为757.17 A·g^-1,1 000 s的稳态电流密度为108.17 A·g^-1,对乙醇催化氧化反应的电荷转移电阻最小,活化能最低。