0000000000014968
AUTHOR
E. Peris-garcía
Comparison of surfactant-mediated liquid chromatographic modes with sodium dodecyl sulphate for the analysis of basic drugs
In reversed-phase liquid chromatography (RPLC), basic drugs are positively charged at the usual working pH range and interact with free anionic silanols present in conventional silica-based stationary phases. This translates into stronger retention and tailed and broadened peaks. This problem can be resolved by the addition of reagents to the mobile phase that are adsorbed on the stationary phase, avoiding the access of solutes to silanols. Among these additives, surfactants under micellar conditions have provided good silanol suppressing potency through the technique known as micellar liquid chromatography (MLC). The most common example of this is anionic sodium dodecyl sulphate (SDS). Whe…
Isocratic and gradient elution in micellar liquid chromatography with Brij-35
Polyoxyethylene(23)lauryl ether (known as Brij-35) is a nonionic surfactant, which has been considered as an alternative to the extensively used in micellar liquid chromatography anionic surfactant sodium lauryl (dodecyl) sulfate, for the analysis of drugs and other types of compounds. Brij-35 is the most suitable nonionic surfactant for micellar liquid chromatography, owing to its commercial availability, low cost, low toxicity, high cloud temperature, and low background absorbance. However, it has had minor use. In this work, we gather and discuss some results obtained in our laboratory with several β-blockers, sulfonamides, and flavonoids, concerning the use of Brij-35 as mobile phase mo…
Effect of buffer nature and concentration on the chromatographic performance of basic compounds in the absence and presence of 1-hexyl-3-methylimidazolium chloride
Abstract In reversed-phase liquid chromatography, the performance for basic compounds is affected by the interaction of the protonated (cationic) species with the anionic free silanols on the alkyl-bonded stationary phases. Using aqueous-organic mobile phases in the absence of additives, the retention may be too high, and the peaks be broad and asymmetric. The performance is improved by addition to the mobile phase of ionic liquids, from which 1-hexyl-3-methylimidazolium chloride ([C6MIm][Cl]) has especially good characteristics. A recent report has also revealed that the use of the phosphate system as buffer, at varying concentration and pH, may have a significant role in the chromatograph…
Oil-In-Water Microemulsion Liquid Chromatography
Oil-in-water microemulsions (O/W MEs) are obtained spontaneously by mixing two immiscible liquids (water and oil) in the presence of a surfactant. A co-surfactant is also often needed for ME stabil...
Protocol to compare column performance applied to hydrophilic interaction liquid chromatography
Abstract The lack of retention of highly polar solutes in liquid chromatography with reversed phase columns (RPLC) can be solved through the use of the hydrophilic interaction liquid chromatographic (HILIC) mode. Due to the complexity of the separation mechanisms in HILIC and the different factors that may have significant influence, the selection of the appropriate stationary phase plays a fundamental role in the development of analytical procedures to obtain good performance. In this work, the chromatographic performance of bare silica and six polar stationary phases with different functionalized groups (with neutral, cationic, anionic and zwitterionic character) are investigated. The beh…
Analysis of tricyclic antidepressants in pharmaceuticals by microemulsion liquid chromatography
Abstract Basic compounds yield long retention times and broad and asymmetric peaks in reversed-phase liquid chromatography, due to interaction with residual silanols in the columns. The addition of the surfactant sodium dodecyl sulphate in the so called micellar liquid chromatography enhances the efficiency, but long retention is achieved, due to electrostatic interaction between the cationic species of basic compounds and the anionic sulphate group of the surfactant. This forces the addition of a strong organic solvent to get appropriate times. An alternative is the use of a microemulsion (ME), formed by mixing surfactant, oil and an alcohol as co-surfactant. Association of hydrophobic com…
Reversed-phase liquid chromatography with mixed micellar mobile phases of Brij-35 and sodium dodecyl sulphate: a method for the analysis of basic compounds
Micellar liquid chromatography (MLC) is a reversed-phase liquid chromatographic (RPLC) mode, which uses a surfactant as a modifier, with significant changes in retention and selectivity with regard to the classical RPLC mode that employs mixtures of water and organic solvent. The anionic sodium dodecyl sulphate (SDS) is the most usual surfactant in MLC, but it also requires the addition of an organic solvent to decrease the retention times and increase the efficiency. In particular, positively charged basic compounds are strongly retained by the stationary phase modified by adsorption of SDS monomers and require the addition of a strong solvent, such as propanol or pentanol. The non-ionic s…
Effect of sodium dodecyl sulphate and Brij-35 on the analysis of sulphonamides in physiological samples using direct injection and acetonitrile gradients
Micellar liquid chromatography (MLC) is a reversed-phase (RP) mode, which often does not require gradient elution, since the peaks of mixtures of compounds within a large range of polarities appear more evenly distributed in the chromatograms of isocratic elution, giving rise to a “gradient effect”. However, the use of a gradient of organic solvent may still be convenient to shorten the total analysis time. This work compares the separation of 15 sulphonamides using conventional hydro-organic RPLC and MLC with the surfactants sodium dodecyl sulphate (SDS) and Brij-35, and both isocratic and gradient elution with acetonitrile. The observed behaviour is rationalized attending to the interacti…
Suitability of 1-hexyl-3-methylimidazolium ionic liquids for the analysis of pharmaceutical formulations containing tricyclic antidepressants
Abstract The reversed-phase chromatographic behaviour of six tricyclic antidepressants (amitryptiline, clomipramine, doxepin, imipramine, nortryptiline and maprotiline) was examined in this work with acetonitrile-water mobile phases, in the absence and presence of the ionic liquids 1-hexyl-3-methylimidazolium chloride and 1-hexyl-3-methylimidazolium tetrafluoroborate, which have interesting features for the separation of basic compounds, in terms of peak shape combined with reduced retention. Tricyclic antidepressants are low polarity drugs that strongly associate to the alkyl chains of conventional stationary phases. They are also positively charged in the usual working pH range (2–8) in r…
Analysis of basic drugs by liquid chromatography with environmentally friendly mobile phases in pharmaceutical formulations
Abstract Basic drugs are positively charged in the usual working pH (2–8) in reversed-phase liquid chromatography. This gives rise to a strong association with the residual ionized silanols in conventional silica-based stationary phases, which is translated in poor peak shape and high consumption of organic solvent to get appropriate retention times. Micellar mobile phases containing surfactants give rise to modified stationary phases, where silanols are masked, improving the peak shape. However, mobile phases containing the anionic surfactant sodium dodecyl sulfate (SDS) require a small amount of organic solvent to conveniently decrease the retention of cationic analytes. An alternative is…
Performance and modelling of retention in microemulsion liquid chromatography
Abstract The capability of liquid chromatography with microemulsions (MEs) as mobile phases was studied for the analysis of four parabens (butylparaben, ethylparaben, methylparaben, and propylparaben) and seven β-adrenoceptor antagonists (acebutolol, atenolol, carteolol, metoprolol, oxprenolol, propranolol, and timolol). MEs were formed by mixing aqueous solutions of the anionic surfactant sodium dodecyl sulphate, the alcohol 1-butanol that played the role of co-surfactant, and octane as oil. In order to guarantee the formation of stable MEs, a preliminary study was carried out to determine the appropriate ranges of concentrations of the three components. For this purpose, mixtures of varia…
Modulation of retention and selectivity in oil-in-water microemulsion liquid chromatography: A review
Microemulsions (MEs) are stable, isotropically clear solutions consisting of an oil and water stabilized by a surfactant and a co-surfactant. Oil-in-water microemuslion liquid chromatography (MELC) is a relatively new chromatographic mode, which uses an O/W ME as mobile phase. Retention, selectivity and efficiency can be modified by changing the concentration of the ME components and the ratio between the aqueous and oil phases. This work makes a critical survey on the information found in the literature about the mobile phase compositions that lead to the creation of successful O/W ME mobile phases, as well as the effect of pH for ionizable compounds and temperature. The viability of perfo…