Analytical Techniques for Furosemide Determination
Abstract Due to the clinical importance of furosemide, a large number of analytical procedures to detect the presence of this drug in pharmaceutical and physiological samples has been developed. In this manuscript, a review of the most frequent analytical techniques described to determine furosemide is presented. Special attention has been paid to spectrophotometric and chromatographic techniques, but also to relevant methods using capillary electrophoresis or flow‐injection analysis, as well as the detection modes coupled to these techniques. The review also focuses on the different degradation pathways of the drug and cautions to prevent it, otherwise rarely or confusedly mentioned in the…
On the use of ionic liquids as mobile phase additives in high-performance liquid chromatography. A review.
The popularity of ionic liquids (ILs) has grown during the last decades in several analytical separation techniques. Consequently, the number of reports devoted to the applications of ILs is still increasing. This review is focused on the use of ILs (mainly imidazolium-based associated to chloride and tetrafluoroborate) as mobile phase additives in high-performance liquid chromatography (HPLC). In this approach, ILs just function as salts, but keep several kinds of intermolecular interactions, which are useful for chromatographic separations. Both cation and anion can be adsorbed on the stationary phase, creating a bilayer. This gives rise to hydrophobic, electrostatic and other specific in…
Ionic Liquid Based Headspace Solid-Phase Microextraction-Gas Chromatography for the Determination of Volatile Polar Organic Compounds
Solid-phase microextraction (SPME) with an ionic liquid (IL) coating was developed for headspace extraction of a group of low molecular weight alcohols (ethanol, n-propanol, butanol, and isopropyl alcohol), acetone, ethyl acetate, and acetonitrile. A first SPME fiber was simply coated with a dedicated IL whose synthesis is described. A second SPME fiber was prepared by gluing silica (Si) particles on which the synthesized IL was chemically bonded. The analytes SPME extraction was optimized for time, temperature, and NaCl salting out content. The headspace extracted analytes were determined by simple temperature desorption into the hot injection port of a gas chromatograph. The coated-IL fib…
Micellar versus hydro-organic mobile phases for retention-hydrophobicity relationship studies with ionizable diuretics and an anionic surfactant
Abstract Logarithm of retention factors (log k ) of a group of 14 ionizable diuretics were correlated with the molecular (log P o/w ) and apparent (log P app ) octanol–water partition coefficients. The compounds were chromatographed using aqueous–organic (reversed-phase liquid chromatography, RPLC) and micellar–organic mobile phases (micellar liquid chromatography, MLC) with the anionic surfactant sodium dodecyl sulfate (SDS), in the pH range 3–7, and a conventional octadecylsilane column. Acetonitrile was used as the organic modifier in both modes. The quality of the correlations obtained for log P app at varying ionization degree confirms that this correction is required in the aqueou…
Hydrophobicity of ionisable compounds studied by countercurrent chromatography
Countercurrent chromatography (CCC) is a liquid chromatography technique in which the stationary phase is also a liquid. The main chemical process involved in solute separation is partitioning between the two immiscible liquid phases: the mobile phase and the support-free liquid stationary phase. The octanol-water partition coefficients (P(o/w)) is the accepted parameter measuring the hydrophobicity of molecules. It is considered to estimate active principle partitioning over a biomembrane. It was related to the substance biological activity. CCC is able to work with an octanol stationary phase and an aqueous mobile phase. In this configuration, CCC is a useful and easy alternative to measu…
Are analysts doing method validation in liquid chromatography?
International audience; Method validation is being applied in the reported analytical methods for decades. Even before this protocol was defined, authors already somehow validated their methods without full awareness. They wished to assure the quality of their work. Validation is an applied approach to verify that a method is suitable and rugged enough to function as a quality control tool in different locations and times. The performance parameters and statistical protocols followed throughout a validation study vary with the source of guidelines. Before single laboratory validation, an analytical method should be fully developed and optimized. The purpose of the validation is to confirm p…
Ionic liquids in separation techniques.
The growing interest in ionic liquids (ILs) has resulted in an exponentially increasing production of analytical applications. The potential of ILs in chemistry is related to their unique properties as non-molecular solvents: a negligible vapor pressure associated to a high thermal stability. ILs found uses in different sub-disciplines of analytical chemistry. After drawing a rapid picture of the physicochemical properties of selected ILs, this review focuses on their use in separation techniques: gas chromatography (GC), liquid chromatography (LC) and electrophoretic methods (CE). In LC and CE, ILs are not used as pure solvents, but rather diluted in aqueous solutions. In this situation IL…
Effect of ionization and the nature of the mobile phase in quantitative structure-retention relationship studies.
Abstract The octanol–water distribution constant, commonly called partition coefficient, Po/w, is a parameter often retained as a measure of the hydrophobicity of a molecule. log Po/w, for a given molecule, can be conveniently evaluated constructing correlation lines between standard retention factor logarithms (log k) in reversed-phase liquid chromatography (RPLC) and standard log Po/w values. Many compounds of pharmaceutical interest can be quite hydrophobic and have, simultaneously, basic nitrogen atoms or acidic sulfur containing groups in their structure. This renders them ionizable. The hydrophobicity of the molecular drug form (Po/w value) is completely different from its ionic form …
Hydrophobicity of Ionizable Compounds. A Theoretical Study and Measurements of Diuretic Octanol−Water Partition Coefficients by Countercurrent Chromatography
Countercurrent chromatography was used to determine the octanol−water partition coefficients (Po/w) of 23 diuretic drugs. The measured Po/w values ranged over 4 orders of magnitude from 0.05 to 550 (−1.3 < log Po/w < +2.7). All the compounds, except spironolactone, were ionizable. The Po/w values were strongly depending on the aqueous-phase pH. A theoretical model linking these values with the pH was derived for four cases: (i) molecular acid−anionic base, (ii) cationic acid−molecular base, (iii) biprotic systems with two acidic or basic groups showing the same charge sign, and (iv) biprotic systems with ionizable groups showing different charges with special attention to the amino acid ca…
Recent advances on ionic liquid uses in separation techniques
International audience; The molten organic salts with melting point below 100°C, commonly called ionic liquids (ILs) have found numerous uses in separation sciences due to their exceptional properties as non molecular solvents, namely, a negligible vapor pressure, a high thermal stability, and unique solvating properties due to polarity and their ionic character of molten salts. Other properties, such as viscosity, boiling point, water solubility, and electrochemical window, are adjustable playing with which anion is associated with which cation. This review focuses on recent development of the uses of ILs in separation techniques actualizing our 2008 article (same authors, J. Chromatogr. A…
New Insights and Recent Developments in Micellar Liquid Chromatography
Abstract: Micellar liquid chromatography (MLC) is an efficient alternative to conventional reversed–phase liquid chromatography with hydro‐organic mobile phases. Almost three decades of experience have resulted in an increasing production of analytical applications. Current concern about the environment also reveals MLC as an interesting technique for “green” chemistry because it uses mobile phases containing 90% or more water. These micellar mobile phases have a low toxicity and are not producing hazardous wastes. After a rapid overview of the two first decades of the technique, this review focuses on the recent advances on fundamental aspects and analytical applications. Traditional and n…
Countercurrent chromatography: People and applications
The scientific literature was scanned for the published research articles dealing with countercurrent chromatography (CCC) over the time period 1980-May 2008. The search returned 1638 articles that were analyzed focussing on people and applications. Concerning the people, it was found that the geographical location of the CCC authors was relatively well balanced between USA, Asia with mainly China and Japan and Europe. Yoichiro Ito, the inventor of the technique, is by far the most productive author in the field with 331 articles or more than one over five CCC articles published in the time period. Without surprise, English is the dominant language with more than 82% of the articles. A sign…