Implementation and efficiency of an automatic peak-purity-control procedure in HPLC-UV-VIS-coupling based on principal component analysis

Summary Based on a thorough knowledge of the actual system precision significance testing of the primary eigen values, resulting from principal component analysis of the two-dimensional data array of HPLC with photodiode-array detection, is a powerful means to uncover unresolved chromatographic peaks. The implementation of this chemometric technique for assuring peak homogeneity and results showing the efficiency for two-component peaks in regard to spectral characteristics, chromatographic resolution and absorbance ratio of the investigated compounds are presented.     

Study on inclusion complexes of meso-tetrakis(2-thienyl)porphyrin and Cu-meso-tetrakis(2-thienyl)porphyrin with cyclodextrins by spectroscopy method

In phosphate buffer solution of pH5.4, the interaction of meso-tetrakis(2-thienyl)porphyrin(H₂TTP) and Cu-meso-tetrakis(2-thienyl)porphyrin(Cu-TTP) with α-cyclodextrin(α-CD), β-CD, γ-CD, heptakis(2,3,6-tri-O-methyl)-β-CD(TM-β-CD) has been studied by means of UV-vis, fluorescence and ¹HNMR spectroscopy, respectively. The H₂TTP and Cu-TTP can form 1:2 inclusion complexes with TM-β-CD and 1:1 inclusion complexes with the other three cyclodextrins. In this paper, the inclusion constants (K) of H₂TTP and Cu-TTP for the formation of the inclusion complexes have been estimated from the changes of absorbance and fluorescence intensity in phosphate buffer solution. The inclusive capabilities of different kinds of cyclodextrins are compared. The result shows that the inclusion ability of α-CD with H₂TTP and Cu-TTP is the strongest among the three native CDs. The inclusion ability of modified β-CD with H₂TTP and Cu-TTP is stronger, compared to the native β-CD, which indicates that the capacity matching plays a crucial role in the inclusion procedure except for the hydrophobic effect. In addition ¹HNMR spectra supports the inclusion conformation of the TM-β-CD-Cu-TTP inclusion complex, indicating the interaction mechanism of inclusion processes.     

光电协同效应降解饮用水中邻氯酚的机理与动力学

要 在集成光解电解一体化反应器中, 以邻氯酚(2-CP)为模型污染物, 通过产物和动力学分析详细探讨了光电复合作用的协同效应机理, 建立了光电复合作用的动力学模式. 表观动力学常数的对比表明复合协同作用对于总有机碳(TOC)的去除具有显著的协同效应. 研究表明, 光电复合作用在研究条件下对污染物的降解具有多层次、多途径的互补效应, 降解反应的途径不止是单独的光解与电解途径的简单累加, 而是通过新的作用途径组合构成光电协同效应. 通过紫外光辐射激发和定向直流电场作用控制电极中毒和污染物分子的激发态及其迁移趋势, 从而大大提高了降解反应的效率. 通过光电复合作用能够触发构成高级氧化的多种自由基链反应, 从而取得水中有机污染物的快速、完全的矿化. 动力学分析表明, 光电协同作用在溶液中形成的羟基自由基(OH·)反应是去除TOC的主要途径.     

Surface chemical analysis of raw cotton fibres and associated materials

The surface chemical composition of raw unscoured cotton was successfully investigated by the surface analytical techniques X-ray Photoelectron Spectroscopy (XPS) and Time of Flight Secondary Ion Mass Spectrometry (ToF-SIMS). The presence of non-cellulosic material at the fibre surface was established and determined to be a complex mixture of fatty acids, alcohols, alkanes, esters and glycerides. The effect of scouring and bleaching was to reduce the surface concentration of these materials but even after aqueous processing some non-cellulosic material residue was still detected at the fibre surface.     

A new poly(2-hydroxy-3-phenoxypropylacrylate, 4-hydroxybutyl acrylate, diethyl maleate) membrane controlled clonidine linear release in the transdermal drug delivery system

Oral clonidine, used as an antihypertensive, can result in some side effects such as dry mouth, drowsiness, dizziness and sedation; thus, clonidine transdermal drug delivery (TDD) was considered. Use of the controlled release membrane was one of the methods in TDD systems to regulate the permeation properties. A new type of copolymer membrane that controlled clonidine linear release in TDD system was synthesized by UV radiation. This membrane consisted of three monomers: 2-hydroxy-3-phenoxypropylacrylate, 4-hydroxybutyl acrylate and diethyl maleate. The membrane had both fine permeation properties and perfect physical properties when three monomers were in the weight ratio of 4:4:2; this type of membrane was chosen as an optimized membrane. It was found that the membrane controlled clonidine zero-order release, the permeation rates decreased with the thicknesses of membranes increasing, and the permeation rates were linearly dependent on the square root of the concentration of clonidine. Furthermore, the optimized membranes were characterized by FTIR, DSC and SEM.     

High-performance liquid chromatography with continuous gradient elution in screening for unknown metabolites of butoprozine directly in dog bile

This paper describes the screening for metabolites of butoprozine, a new anti-anginal drug, in dog bile by means of reverse-phase HPLC. Although it does involve a simple clean-up step to remove a substantial amount of endogenous bile compounds, this screening method nevertheless avoids extraction of metabolites and thus allows all metabolites to be introduced into the chromatographic system. A single run of 100 minutes from 100% water to 100% methanol in a linear gradient effects adequate separation of the great majority of metabolites without interference from remaining endogenous compounds. Two methods of differentiating between metabolite peaks and endogenous peaks have been worked out. The first one makes use of ¹⁴C-labeled butoprozine by measuring the amount of radioactivity in the column effluent while simultaneously recording the UV absorbance. The second method compares continuous gradient chromatograms of bile recorded before and after butoprozine administration under very similar conditions. The latter method can be applied to both radioactive and non-radioactive materials.     

Cesium lead halide perovskite nanocrystals for ultraviolet and blue light blocking

Using cesium lead halide perovskite nanocrystals, CsPb(Cl/Br)_3, as a light absorber, we report a highly effective UV and blue light blocking film. The CsPb(Cl/Br)_3 nanocrystals are well dispersed in the ethyl cellulose(EC) matrix to compose a UV and blue light shielding film, and the absorption edge of the film is tunable by adjusting Cl to Br ratio using anion exchange. The CsPbCl_2 Br-EC film exhibits a transmittance of 5% at 459 nm, 90% at 478 nm and 95% in the range of 500–800 nm, which makes it excellent for UV and blue light shielding. In addition, the as-prepared EC-CsPb(Cl/Br)_3 film shows excellent photostability under UV irradiation. Results demonstrate that this EC-CsPb(Cl/Br)_3 based materials with sharp absorbance edges, tunable blocking wavelength, and high photostability can be useful for the applications in UV and blue light blocking and optical filters     

Characterization of Autocatalytic Reactions in Modified Cellulose/NMMO Solutions by Thermal Analysis and UV/VIS Spectroscopy

The thermal stability of cellulose/N-methylmorpholine-N-oxide (NMMO) solutions were investigated using UV/VIS spectrometry with a temperature programming cuvette and caloric measurements by means of the Systag calorimeter RADEX (mini-autoclave). Both analytical methods allow to characterize the influences of stabilizers and additives. With the temporal course of the optical density, temperature and pressure thermal runaway reactions with gas evolution and accumulation of chromophoric degradation products were recognized. Kinetic model calculations compared with UV/VIS measurements demonstrate the existence of autocatalytic reactions in cellulose/NMMO solutions. Varying the heating rate autocatalysis can be proved by dynamic caloric measurements as well.     

双(1,3-二硫杂环戊烯-2-硒酮-4,5-二硫)金属配合物的合成及其电化学性质的研究

以1，3-二硫杂环戊烯-2-硒酮-4，5-二硫盐为配体与二价金属离子配位合成了4种双(1，3-二硫杂环戊烯-2-硒酮-4，5-二硫)金属配合物，研究了它们的电化学性质和UV—Vis光谱，并讨论了形成中性产物的原因。