Modeling of chromatographic retention of the selected antiarrhythmics and structurally related compounds in the hydrophilic interactions under the TLC and HPLC conditions

Abstract

High-performance liquid chromatography (HPLC) plays an important role in testing the pharmaceutically active compounds. In despite of the advantages of HPLC, thin-layer chromatography (TLC) retains its applicability to the different experimental tasks. The experimental conditions which allow hydrophilic interactions in the chromatographic system were tested in the HPLC and TLC systems for ivabradine, its related compounds, diltiazem and verapamil. Under the TLC conditions, retention behavior of the investigated compounds was tested on silica gel modified with cyanopropyl ligands as stationary phase and acetonitrile?+?methanol containing 25% v/v formic acid. Under the HPLC conditions, we used silica gel modified with cyanopropyl ligands as a column packing and the acetonitrile + 0.25% aqueous solution of formic acid as mobile phase. Retention behavior of the investigated analytes depending on the changing volume fractions of the mobile phase modifier was characterized both for TLC and HPLC data sets by the Soczewiński–Wachtmeister equation. Linear relationships were established between the retention coefficients characterizing the retention mechanism (R_M⁰/m, logk₀/m) and molecular properties of the investigated compounds. The Quantitative Structure Retention Relationship (QSRR) modeling was performed with the use of the stepwise multiple linear regression, in order to select molecular properties which influence retention.     

The effect of pomegranate seed powder addition on radical scavenging activity determined by TLC–DPPH test and selected properties of gluten-free pasta

The aim of the present work was to study the effect of pomegranate seeds powder (PSP) supplementation to gluten-free (GF) sheeted pasta on cooking properties, sensory characteristics and antioxidants properties using TLC-DPPH test. Five levels of pomegranate seed powder were used (2.5, 5.0, 7.5, 10.0 and 12.5%) on formula replacement basis. Antioxidant potential of GF pasta increased with the addition of pomegranate seeds powder. The GF pasta without additives and with 2.5% concentration of PSP did not reveal ability to scavenge free radicals. The highest aforementioned activity was observed for crude pomegranate seed extract followed by GF pasta with 12.5, 10.0, 7.5 and 5.0% addition of PSP. The total dietary fibers content of pasta increased from 5.68 to 14.80?g/100?g with the increase in the incorporation of PSP from 0 to 12.5%. The results revealed that cooking loss of gluten-free pasta increased from 9.09 to 10.18%, whereas pasta firmness decreased from 381.43 to 366.30?N, upon incorporation of PSP. Pomegranate seeds powder decreased the lightness of the pasta from 82.26 to 57.27. Sensory analysis suggested that control pasta (without PSP) and pasta supplemented with low levels of PSP have the most acceptable quality. In conclusion, incorporating PSP at low levels enhanced the nutritional quality of pasta without a significant adverse effect on its cooking, textural and sensory properties.     

Effects of starvation for 4-20 days on the amino acid content of Biomphalaria glabrata as determined by cellulose HPTLC-densitometry with confirmation of identity using silica gel and RP-18 W plates with two mobile phases causing inversion of the separation mechanism

The effects of starvation at 4, 7, 10, 14, and 20 days on the amino acid content of Biomphalaria glabrata was determined by high performance thin layer chromatography (HPTLC)-densitometry. Cultures of control and starved snails were prepared for each duration of time. Samples were extracted using ethanol-water (70:30), and supernatant was collected after multiple centrifugations. Samples and standards were applied as bands using a CAMAG Linomat 4 onto cellulose HPTLC plates and developed in a 2-butanol-pyridine-acetic acid-water (39:34:10:26) mobile phase before spraying with ninhydrin detection reagent and scanning with a CAMAG 3 scanner to quantify ornithine (Orn), glycine (Gly), alanine (Ala), valine (Val), and leucine (Leu). Amino acid identification was confirmed by HPTLC on silica gel plates and RP-18?W plates using two different mobile phases causing inversion of the separation mechanism. Starvation led to an overall decrease in amino acid content in comparison to the control snails, however, the amount of amino acids in the starved snails had no correlation with the duration of starvation.     

Analysis of gardenia blue in foods by thin-layer chromatography

In the present study, a thin-layer chromatography (TLC) method for the analysis of gardenia blue was described. Gardenia blue is obtained from the fruits of Gardenia augusta Merrill or Gardenia jasminoides Ellis. Recently, gardenia blue has frequently been used in Japan as a natural coloring in various foods. However, the structural characterization of gardenia blue components has not been yet clarified and even chromatographic separation of the components has not been reported. Synthetic colors in foods are generally analyzed by TLC; so, we therefore investigated the analysis of gardenia blue in foods with TLC. We established two TLC conditions; reversed phase C-18 TLC using a solvent system of aqueous 0.2% TFA–acetonitrile–ethanol (1:2:3) and TLC on cellulose plate using a solvent system consisting of acetone–3-methyl-1-butanol–water (6:5:5). Both conditions yielded three well-delineated spots with good separation. We applied these separations to the analyses of gardenia blue in coloring matter preparations from different manufacturers and in foods on the market. After the gardenia blue was extracted from the samples with water, the extract was evaporated and the residue was dissolved in water–methanol (1:1). Aliquots of the dissolved solutions were then applied to TLC and their chromatographic behaviors were observed. Each preparation showed characteristic spot patterns depending on the manufacturers. The R_f values of the separated spots when extracted from foods are slightly different from the R_f values of the spots observed for standards, and we were thus able to identify the manufacturers using the spot pattern of gardenia blue. The present study is considered to be useful for the establishment of a method of analysis for gardenia blue in coloring preparations and foods.     

β－环糊精固载相薄层层析法直接拆分氨基酸D，L－对映体

以环氧氯丙烷作为多功能官能团交联剂，经化学合成反应，将β－环糊精固载在活性轻质二氧化硅表面上，以此为固定相制备成层析薄板，直接用于拆分氨基酸的Ｄ，Ｌ－对映异构体．实验结果表明：该层析薄板在脱氧胆酸或尿素的协同作用下，可用于拆分亲脂性基因与手性碳直接相连的氨基酸Ｄ，Ｌ－对映体．研究了在展开剂中不同浓度的脱氧胆酸和尿素两种立体选择助剂对这３种氨基酸的Ｄ，Ｌ－对映异构体的分离效果的影响，并对其机理进行了初步讨论．     

亲核试剂亲核取代竞争的薄层色谱扫描测定法

用薄层色谱扫描法测定Cl~-和Br~-在亲核取代竞争反应中所生成的相应卤代物混合物各组分摩尔含量,以确定其亲核性强弱.此法操作简便,快速,重现性好,准确度高,可一次同时测定多个样品.     

棱萼母草的生药学研究

目的对玄参科母草属植物棱萼母草的显微特征进行生药学研究。方法按照常规生药学方法进行来源、性状、显微鉴别和薄层鉴别。结果棱萼母草的性状,显微特征和薄层特征明显。结果可为棱萼母草的鉴别和开发提供科学依据。     

黑龙江汉麻叶中化学成分研究与大麻二酚（CBD）含量测定

研究黑龙江汉麻叶中相关化学成分,建立大麻二酚(CBD)含量检测方法.采用硅胶柱色谱、C18反相中压柱及半制备色谱对汉麻叶乙酸乙酯提取物进行分离纯化,得到5个单体化合物,经核磁NMR解析确定结构为:大麻二酚(CBD)、大麻萜酚(CBG)、大麻酚(CBN)、Δ9-四氢大麻酚酸(Δ9-THCA)、大麻色烯(CBC);以石油醚-二氯甲烷(1∶1)为展开剂,采用碘和1%香草醛乙醇-硫酸(10∶1)分别显色,建立了CBD薄层色谱(TLC)检测方法;以乙腈-0.05%磷酸溶液(80∶20)为流动相,选择CBD吸收峰较高的检测波长,建立了CBD高效液相色谱(HPLC)检测方法;该方法在3.125～100μg/mL线性关系良好(R~2=0.9997),平均回收率为103.69%,RSD 1.32%(n=5).     

薄层色谱指纹图谱在丹参药材质量评价中的应用研究

利用薄层色谱（TLC）技术对中药材丹参的有效成分进行了指纹图谱分析．以不同等级的中江丹参和不同采收期的丹参、南丹参为分析对象，采用适宜的水溶性及脂溶性成分提取方法和TLC分析条件，可获得其相应的TLC图像及色谱图．通过对不同丹参药材的色谱图像的分析，结合化学计量学方法对其各主要指标成分的信息进行提取，初步构建了丹参的TLC指纹图谱．结果表明，在254nm波长下获取脂溶性和水溶性成分共7个共有指纹峰，各峰相对比移值（R1）和峰面积的相对标准偏差分别小于1．7％和4．0%．通过对薄层色谱斑点的RI值、斑点颜色和大小的比较。并进行主成分分析和聚类分析，实现了对不同等级的丹参进行归属，并确立了最佳采收期．本实验建立的薄层色谱指纹图谱方法具有较高的稳定性、良好的精密度和重现性，可用于丹参药材的质量评价和控制．     

用数理统计选择CTP薄层层析系统中的流动相

本实验对防焦剂CTP的薄层层析流动相进行选择。用正交设计法安排实验,对其R_f值用极差分析方法进行处理,找到了较好的流动相。