Structure–retardation factor relationship of natural amino acids in two different mobile phases of RP-TLC

Abstract

Separation of amino acids (AAs) and their simple and inexpensive determination/identification is an interesting topic in biological and protein science, different food industries, and drug factories. Also, the presentation of the chromatographic behavior of compounds in a predictive model can be effective to estimate the structural/chemical properties of analyte and mobile phases. In this work for the first time, retardation factor (R_F) of 42 AAs in reversed-phase thin layer chromatography (RP-TLC) was modeled. Acetonitrile-sodium azide solution and 1,2 dioxane-sodium azide solution were two mobile phases which have been studied in this work. Results showed that the values of R_F are correlated with the structural properties of AAs and these properties had some similarities and differences in two noted mobile phases. For the TLC data in two mobile phases, five parametric linear models were suggested (R²_train = 0.93 and 0.97; R²_test = 0.93 and 0.99). The models were also evaluated with different statistical approaches. It was shown that increasing the sum of geometrical distances between N and O in AAs causes decreasing their R_F in RP-TLC using both mobile phases. Other structural effects of AAs on their separation in the desired RP-TLC system were also discussed.     

Thermal analysis and X-ray studies of chiral ferroelectric liquid crystalline materials and their binary mixtures

Summary Thermal properties of a homologous series of ferroelectric liquid crystals S-(-)-[4-(2-n-alkoxy-propionyloxy)]biphenyl-4'-[n-alkoxy-(3,5-dimethyl)]benzoate have been investigated by polarizing optical microscopy and differential scanning calorimetry. The mesophases were identified and confirmed by X-ray too. Three binary mixtures were prepared from the individual homologues. In one of the mixtures (Mix1), the ferroelectric SmC* phase has broadened and became enantiotropic. This mesophase remained monotropic in the other two mixtures (Mix2, Mix3). The chiral nematic N* phase did not appear in Mix1, but remained monotropic for the other two mixtures. Two molecular parameters, the layer spacing and the average intermolecular distance have been calculated from the X-ray results for the homologues and their mixtures. An intercalated tail-to-tail packing of molecules was found both in the single compounds and their mixtures resulting in the layer spacing about half of the molecular length of the single compounds.     

Accounting for the Adsorption of Anions When Interpreting the Mechanism of Electrodeposition of Metals from Complex Electrolytes: The Reaction Order by the Electrochemically Active Ion

The relationship between the current and the bulk concentration of complex ions during concurrent specific adsorption of an electrochemically active complex ion and a complexing ligand is considered. The effect of parameters that characterize adsorption of such ions and the structure of the electrical double layer on this relationship is analyzed.__________Translated from Elektrokhimiya, Vol. 41, No. 7, 2005, pp. 817–822.Original Russian Text Copyright © 2005 by Rogozhnikov.     

Distribution of Helium Isotopes in Western Pacific Upper Layer

3He/4He ratios in samples of sea water obtained at depths from surface to 300 m in the upper layer of the Western Pacific Ocean were measured by a mass spectrometer VG5400. The lateral and vertical distribution of He isotopes in the studied area was discussed in detail on the basis of 3He/4He ratios. Excess and depleted 3He. in relation to δ3He value of surface water in equilibrium with air has been discussed in the area, which may be mainly attributed to the incorporation of the North Pacific Intermediate Water with the Equatorial Upwelling and the exchange of water masses between the South China Sea and the Western Pacific, respectively. The present work in Western Pacific has also indicated that He isotopes may be used as a tracer for mixing processes of water masses and oceanic circulation.     

薄层色谱法在香兰素合成中的应用

应用薄层色谱法对愈创木酚、3－甲氧基－4－羟基扁桃酸和香兰素进行了分析，以硅胶GF254作为吸附剂，从几种溶剂系统中选出氯仿：乙酸乙酯：正丙醇：冰乙酸：水＝20：1：1：1：2溶液作为展开剂。建立了 香兰素的薄层扫描定量分析方法，测定波长为500nm，参比波长为570nm，线性范围为0．31－6．2μg。     

不同类型聚合物溶液对采油残余油的作用机理研究

通过实验测定了HPAM溶液和黄原胶溶液的流变性、在多孔介质中的流变性和残余阻力系数 ,计算了衰竭层效应 .用不同的浓度和注入速度进行了驱油实验 .提出聚合物分子缠结作用的增强不仅引起表观粘度增加或衰竭层厚度降低 ,而且使平行于油水界面的拉动残余油的力增加 ,从而使残余油饱和度降低 ,采收率提高 .随浓度增加 ,HPAM溶液的表观粘度和残余阻力系数增加 ,衰竭层厚度减小 ;黄原胶溶液的浓度高于缠结浓度时 ,衰竭层厚度和表观粘度变化不大 .注入速度增加时 ,两种聚合物溶液的衰竭层厚度均降低 ,HPAM溶液的残余阻力系数不变 ,粘弹性增加 ;而黄原胶溶液的残余阻力系数下降 .不同浓度和注入速度情况下两种聚合物溶液的驱油结果证实了文中提出的聚合物分子缠结作用和衰竭层效应对残余油的作用机理 .分子结构的不同是造成两种聚合物溶液在多孔介质中渗流规律和对残余油作用机理的差别的根本原因 .     

2－氰基－4－硝基苯胺的薄层色谱紫外光度分析

本文应用薄层色谱紫外光度法，测定了产品中的主要成分２－氰基－４－硝基苯胺和杂质，得到了满意的分析结果。与经典化学法比较，这种方法具有简单、快速、精确的特点。回收率９９％～１０１％，相对标准偏差０．７％～１．１％，２－氰基－４－硝基苯胺含量在０～１３５μｇ／２５ｍＬ范围内遵守比耳定律。     

Weak Interactions and 2D Layer Structure of a New Ion-pair Complex Bis(1-benzyl-4-methylquinolinium)-bis(maleonitriledithiolato)nickel(Ⅱ)

A new ion-pair complex,[BzMeQl]2[Ni(mnt)2] 1 ([BzMeQl]+=1-benzyl-4-methylquino-linium,mnt2-= maleonitriledithiolate) has been synthesized and structurally characterized by IR,ESI-MS and X-ray diffraction methods. Complex 1 is of triclinic,space group P1,with a=9.079(2),b=10.154(2),c=11.243(2),α=81.58(1),β=69.63(1),γ=68.02(1)°,V=940.1(3)3,Dc=1.427 g/cm3,Z=1,F(000)=418 and R=0.0442. A 2D layer structure is formed via the cation-cation π…π and C–H…π interactions observed in the solid state of the complex.     

Applicability of polymer theories to the thermodynamics of proteins at the air/water interface: example of β-lactoglobulin

Knowledge of the equation of state of adsorbed or deposited layers of proteins at the air/water interface is of fundamental interest in the understanding of the surface activity of these molecules. Using scaling laws of current polymer theories, it has been shown that the equation of state of the interfacial layer in the semi-dilute regime should relate the surface pressure to the surface concentration through a power law. The exponent of this power law should reflect the quality of the solvent and the conformation of the adsorbed polypeptide chain. In the case of β-lactoglobulin layers, in the range of surface concentrations that should correspond to the semi-dilute regime, the relationship between surface pressure and surface concentration is expressed as a power law. The exponent of this power law is strongly influenced by the nature of the aqueous substrate and by the net charge of the protein molecule. The use of scaling laws gives a coherent view of the expansion of the polypeptide chain in the interfacial layer and of the relationship between surface concentration and surface pressure in the semi-dilute regime. This result favours a strong similarity between β-lactoglobulin and a polymer chain in the interfacial layer. It is concluded that current theories of polymer adsorption could be applied to interfacial protein layers.     

The application of the concept of reaction layer to the study of electrode processes coupled with the second-order chemical reactions at microelectrodes under steady-state conditions

Under steady-state conditions, the current equations of the second-order EC, ECE and DISPI reactions at microdisk, microspherical and microring electrodes are derived with the aid of the concept of the reaction layer. The conditions under which these equations would be valid are also discussed. Using these equations, methods to determine the kinetic parameters for the second-order EC, ECE and DISPI reactions are presented. The reduction of 2,6-diphenyl-pyrylium cation and oxidation of triphenylamine were investigated as examples of the second-order EC and ECE reactions.