scholarly journals Estimation of Solute-Stationary Phase and Solute-Mobile Phase Interactions in the Presence of Ionic Liquids

Separations ◽  
2019 ◽  
Vol 6 (3) ◽  
pp. 40
Author(s):  
María José Ruiz-Ángel
Keyword(s):  
Ionic Liquids ◽  
Stationary Phase ◽  
Mobile Phase ◽  
Stationary Phases ◽  
Reversed Phase ◽  
Retention Mechanism ◽  
Chromatographic Behavior ◽  
Chemical Equilibria ◽  
Suppression Effect ◽  
Mobile Phases

The presence of free silanols on alkyl-bonded reversed-phase stationary phases is responsible for broad and asymmetrical peaks when basic drugs are chromatographed with conventional octadecylsilane (C18) columns due to ionic interactions. In the last few years, ionic liquids (ILs) have attracted attention to reduce this undesirable silanol activity. ILs should be considered as dual modifiers (with a cationic and anionic character), which means that both cations and anions are able to adsorb on the stationary phase, creating a positively or negatively charged layer, depending on the relative adsorption. The accessibility of basic compounds to the silanols is prevented by both the IL cation and anion, improving the peak profiles. A comparative study of the performance of six imidazolium-based ILs, differing in their cation/anions, as modifiers of the chromatographic behavior of a group of ten β-adrenoceptor antagonists, is addressed. Mobile phases containing cationic amines (triethylamine and dimethyloctylamine) were used as a reference for the interpretation of the results. Using a mathematical model based on two chemical equilibria, the association constants between the solutes and modified stationary phase as well as those between solutes and the additive in the mobile phase were estimated. These values, together with the changes in retention and peak shape, were used to obtain conclusions about the retention mechanism, changes in the nature of the chromatographic system, and silanol suppression effect.

scholarly journals Reversed-phase thin-layer chromatography behavior of aldopentose derivatives

2012 ◽  
Vol 66 (3) ◽  
pp. 365-372 ◽  
Author(s):  
Dragana Livaja-Popovic ◽  
Eva Loncar ◽  
Lidija Jevric ◽  
Radomir Malbasa
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Stationary Phases ◽  
Reversed Phase ◽  
Chromatographic Behavior ◽  
Log P ◽  
Retention Factors ◽  
Mobile Phases ◽  
Acetone Water ◽  
Layer Chromatography

Quantitative structure-retention relationships (QSRR) have been used to study the chromatographic behavior of some aldopentose. The behavior of aldopentose derivatives was investigated by means of the reversed-phase thin-layer chromatography (RP TLC) on the silica gel impregnated with paraffin oil stationary phases. Binary mixtures of methanol-water, acetone-water and dioxane-water were used as mobile phases. Retention factors, RM0, corresponding to zero percent organic modifier in the aqueous mobile phase was determined. Lipophilicity C0 was calculated as the ratio of the intercept and slope values. There was satisfactory correlation between them and log P values calculated using different theoretical procedures. Some of these correlations offer very good predicting models, which are important for a better understanding of the relationships between chemical structure and retention. The study showed that the hydrophobic parameters RM0 and C0 can be used as a measures of lipophilicity of investigated compounds.

scholarly journals Abnormal retention of s-triazine herbicides on porous graphitic carbon

2021 ◽  
Vol 41 (1) ◽  
pp. 1-9
Author(s):  
Oksana Grinevich ◽  
Zoya Khesina ◽  
Alexey Buryak
Keyword(s):  
Stationary Phase ◽  
High Performance ◽  
Reversed Phase ◽  
Retention Mechanism ◽  
Porous Graphitic Carbon ◽  
Graphitic Carbon ◽  
Chromatographic Behavior ◽  
Triazine Herbicides ◽  
Pesticide Monitoring ◽  
Modeling Of Adsorption

Abstract Porous graphitic carbon (PGC) is a widely used stationary phase for reversed-phase high-performance liquid chromatography (HPLC) that allows separation of structurally similar compounds retained in mixed form on a flat graphite surface. Such a stationary phase can be used in analytical chemistry to provide good separation and selectivity in pesticide monitoring. In this article, we studied the chromatographic behavior of five common triazine herbicides (simazine, atrazine, desmetryn, propazine, prometryn) on PGC vis-à-vis octadecyl-functionalized silica gel (ODS). It was found that the herbicides studied have an abnormal elution order on PGC compared to ODS. PGC was also characterized by higher selectivity of analyte separation. This behavior of triazine herbicides on PGC cannot be explained either with the help of existing theory or by mathematical modeling of adsorption processes on graphite. Therefore, we have proposed a possible retention mechanism, explaining the effects observed, due to the shielding of the amino group in the triazine ring by alkyl substituents, which decreases the “polar retention effect” of PGC. Satisfactory separation efficacy was obtained with the proposed analytical method, using convenient UV-detection and without resort to laborious techniques such as HPLC coupled with mass spectrometry.

A Complementary Study of Mechanisms and Behaviors in Chromatography via Modeling

2015 ◽  
Vol 98 (5) ◽  
pp. 1462-1470 ◽  
Author(s):  
Maria G Kouskoura ◽  
Constantina V Mitani ◽  
Catherine K Markopoulou
Keyword(s):  
Stationary Phases ◽  
Chemical Compounds ◽  
Structural Features ◽  
Retention Mechanism ◽  
Chromatographic Behavior ◽  
Polar Surface Area ◽  
Hydrogen Bond Donor ◽  
Solubility In Water ◽  
Mobile Phases ◽  
Complementary Study

Abstract Evolution in preparation of chromatographic columns has created the need for studying and evaluating them with the use of smart software. This research is an attempt to compare the retention mechanism between two stationary phases (butyl and phenyl) with the use of multivariate analysis for a large number of probes. Partial least squares has the ability to spot either major or minor differences in the chromatographic behavior of probes, with regard to changes in the stationary or mobile phases. The models developed refer to a total of 108 miscellaneous chemical compounds, described by 63 X variables (physicochemical properties and structural features) and one Y variable (retention time). The results showed that in both columns and mobile phases (40% methanol or 40% acetonitrile) the retention of an analyte is mainly affected by its lipophilicity, molar volume, and refractivity, which tend to cause delayed elution. On the contrary, solubility in water, polar surface area, and hydrogen bond donor or acceptor properties promote faster elution. The most important difference proved to be the effect of the presence of the carboxylic group and the solubility that affected the retention in a similar way in both columns but not with both mobile phases.

scholarly journals A simple TLC and HPTLC method for separation of selected steroid drugs

2013 ◽  
Vol 11 (8) ◽  
pp. 1297-1308 ◽  
Author(s):  
Joanna Nowakowska ◽  
Piotr Pikul ◽  
Krzesimir Ciura ◽  
Jakub Piotrowicz
Keyword(s):  
Stationary Phase ◽  
Mobile Phase ◽  
Stationary Phases ◽  
Principal Component ◽  
Reversed Phase ◽  
Chromatographic Retention ◽  
Retention Data ◽  
Binary Mobile Phases ◽  
Acetone Water ◽  
Steroid Drugs

AbstractChromatographic properties of five steroid drugs: cortisone, hydrocortisone, methylprednisolone, prednisolone and norgestrel have been studied by normal-, reversed-phase and hydrophilic neutral cyano-bonded silica stationary phase with five binary mobile phases (acetonitrile-water, acetonitrile-DMSO, acetonitrile-methanol, acetone-petroleum ether, acetone-water) in which the concentration of organic modifier was varied from 0 to 100% (v/v). This study reports the optimization of steroid hormones separation. Chromatographic retention data and possible retention mechanisms are discussed. Separation abilities of mobile and stationary phases were studied using the principal component analysis method. The best separation of methylprednisolone and prednisolone is with a chromatographic system included silica gel as stationary phase and mixture of acetonitrile and DMSO (10:90 v/v). These two anti-inflammatory drugs can be fast separated from norgestrel when CN is used as stationary phase and acetone and water (40:60 v/v) as mobile phase. The highest values of the parameter Δ(ΔG°) and alfa for cortisone and hydrocortisone was observed in case of using CN as stationary phase and water-acetonitryle (40:60 v/v) as mobile phase.

scholarly journals Thermodynamic Insights into the Separation of Carotenoids in Reversed-Phase Liquid Chromatography

2019 ◽  
Vol 2019 ◽  
pp. 1-7 ◽  
Author(s):  
Nicola Marchetti ◽  
Pier Paolo Giovannini ◽  
Martina Catani ◽  
Luisa Pasti ◽  
Alberto Cavazzini
Keyword(s):  
Liquid Chromatography ◽  
Stationary Phase ◽  
Mobile Phase ◽  
Reversed Phase ◽  
Retention Mechanism ◽  
Thermodynamic Quantities ◽  
Reversed Phase Liquid Chromatography ◽  
Mobile Phase Composition ◽  
Solute Transfer ◽  
Phase Liquid

The retention mechanism of four major carotenoids, two xanthophylls (i.e., lutein and zeaxanthin) and two carotenes (i.e., lycopene and β-carotene), was investigated in reversed-phase liquid chromatography with the aim of thermodynamic analysis. The experimental variables considered in this study were the composition of mobile phase (MP) and the temperature. Chromatographic elutions were undertaken under linear, isocratic conditions by using a C18 stationary phase, four different MP compositions (by varying the ratio methanol/acetonitrile from 66.5/28.5 to 47.5/47.5 v/v), and column temperatures in the range 283–313 K. Traditional Van’t Hoff analysis has been used to estimate changes of standard enthalpy (ΔH∘) and Gibbs free energy (ΔG∘) associated with the solute transfer from the mobile to the stationary phase at each mobile phase composition. The thermodynamic quantities have been correlated to the structure of investigated carotenoids and their interaction with the octadecyl silica stationary phase.

scholarly journals Chromatographic behavior and lipophilicity of s-triazine derivatives on silica gel impregnated with paraffin oil

2010 ◽  
pp. 159-168 ◽  
Author(s):  
Lidija Jevric ◽  
Gordana Koprivica ◽  
Nevena Misljenovic ◽  
Bratislav Jovanovic
Keyword(s):  
Silica Gel ◽  
Volume Fraction ◽  
Reversed Phase ◽  
Retention Mechanism ◽  
Chromatographic Behavior ◽  
Oil Retention ◽  
Paraffin Oil ◽  
Mobile Phases ◽  
Acetone Water ◽  
Triazine Derivatives

The chromatographic behavior of four group of s-triazine derivatives (14 compounds) has been studied by TLC on silica gel impregnated with paraffin oil. Retention mechanism has been determined using the following mobile phases: water-acetone, water-acetonitrile, water-dioxane, water-tetrahydrofuran, water-methanol and water-ethanol, by changing the volume fraction of modifier in the mobile phase. On impregnated silica gel, a reversed-phase chromatographic process occurs. Good correlation was obtained between the retention constants, RM 0 (determined by linear extrapolation), and slope, S, of chromatographic equations. There was also satisfactory correlation between these retention constants and logP values calculated using different theoretical methods. The study showed that the retention constants can be used as a measure of lipophilicity of investigated compounds.

Application of Mobile Phases Containing Ionic Liquid for HPLC Analysis of Selected Isoquinoline Alkaloids

2017 ◽  
Vol 100 (6) ◽  
pp. 1652-1659 ◽  
Author(s):  
Anna Petruczynik ◽  
Justyna Misiurek ◽  
Tomasz Tuzimski ◽  
Monika Waksmundzka-Hajnos
Keyword(s):  
Ionic Liquid ◽  
Stationary Phases ◽  
Reversed Phase ◽  
System Efficiency ◽  
Organic Modifier ◽  
Optimal Conditions ◽  
Retention Behavior ◽  
Isoquinoline Alkaloids ◽  
Mobile Phases ◽  
Chemical Groups

Abstract An HPLC procedure on a polar reversed-phase column with mobile phases containing ionic liquid (IL) was developed for the analysis of selected alkaloids from different chemical groups. We aimed to obtain optimal conditions for the separation of alkaloids because widely used silica-based stationary phases exhibit a silanol effect, rendering analysis of basic analytes extremely difficult. Retention, separation selectivity, peak symmetry, and system efficiency were examined in various eluent systems containing different concentrations of IL and acetonitrile. The obtained results revealed substantial influence from the concentrations of IL, the organic modifier, and temperature on the retention behavior of the investigated alkaloids. The most selective and efficient chromatographic systems were applied for the analysis of several alkaloids in a plant extract.

scholarly journals HPLC FINGERPRINT OF ORGANIC ACIDS IN FRUIT JUICES

1970 ◽  
Vol 62 ◽  
Author(s):  
Loredana Leopold ◽  
Diehl Horst ◽  
Carmen Socaciu
Keyword(s):  
Organic Acids ◽  
Stationary Phase ◽  
Organic Acid ◽  
Mobile Phase ◽  
Reversed Phase ◽  
Fruit Juices ◽  
Hplc Fingerprint ◽  
Organic Acid Profile ◽  
Phase Column ◽  
Reversed Phase Column

Organic acids give fruit products their characteristic tartness and vary in combination and in concentrations among different juices. The organic acid profile can be used to identify a juice or verify its purity. Typically, organic acids in fruit juices are identified and quantified by using methods such as HPLC. In this procedure, reversed phase column is used to separate and identificate six organic acids. Because several of the analytes are extremely difficult to resolve, a aqueous mobile phase is needed to enhance interaction between the acids and the C18 stationary phase.

scholarly journals Retention behaviour of acyclic polyfunctional D-arabinose derivatives

2002 ◽  
pp. 35-44 ◽  
Author(s):  
Ljiljana Kolarov ◽  
Eva Loncar ◽  
Radomir Malbasa
Keyword(s):  
Mobile Phase ◽  
Volume Fraction ◽  
Retention Mechanism ◽  
Biologically Active ◽  
Polar Component ◽  
Chiral Molecules ◽  
Retention Behaviour ◽  
Polar Components ◽  
Solute Retention ◽  
Mobile Phases

It is well known that some of biologically active compounds are chiral molecules. Natural monosaccarides are applicable as chiral precursors. D-arabinose is an appropriate chiral precursor in the synthesis of very important biomolecules such as biotin and its analogues and feromon )-exobrevicomin. Acyclic poly functional D- arabinose derivatives are intermediates in the synthesis of the former biomolecules. This paper deals with the retention behaviour and retention mechanism of acyclic poly functional D-arabinose derivatives. The tested compounds have been chromato graphed on silica gel thin layer using binary organic mobile phases with a different polarity. With increasing polarity of the eluent polar components the solute retention is decreasing. The linear relationship is obtained between the values of retention constant, RM' and the logarithm of the mobile phase polar component volume fraction for all solutes tested and eluents used.

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