Sense and nonsense of high-temperature liquid chromatography

Heinisch, Sabine; Rocca, Jean‐Louis

doi:10.1016/j.chroma.2008.11.079

Cited by 185 publications

(85 citation statements)

References 160 publications

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“…The high temperature LC did not affect the biochemical high-resolution assay for cathepsin B inhibitors (de Boer et al 2005b). An overview of the pros and cons of HT-HPLC was presented by Heinisch and Rocca (2009).…”

Section: High-temperature Hplcmentioning

confidence: 99%

Recent developments in the rapid analysis of plants and tracking their bioactive constituents

et al. 2009

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Section: High-temperature Hplcmentioning

confidence: 99%

Recent developments in the rapid analysis of plants and tracking their bioactive constituents

et al. 2009

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“…The first observation is that at 1 mL/min (1.4 mm/s), the velocity is above u opt for all solutes at 30°C while close to u opt at 80°C. The fact that higher temperatures generate higher optimal mobile phase velocities is well documented in the literature [22,26,31,35] and the result of the interplay between an increased B-term and a decreased C-term. …”

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confidence: 72%

“…of the retention for all compounds. The relationship is described by the Van 't Hoff equation [22,41]. Because retention is an exothermic process (∆H < 0) and generally entropy is lost upon transfer from the mobile to the stationary phase (∆S < 0), an increase in temperature leads to a shift of the equilibrium towards the mobile phase and therefore to a drop in retention [27,31,40,41].…”

Section: Experimental Verification Of the Kinetic Plotsmentioning

confidence: 99%

“…The only additional requirement is an appropriate mobile phase and column heating system [20,[22][23][24]. The use of elevated column temperatures in RP-LC to achieve high separation efficiencies have been investigated extensively [5,[25][26][27][28][29][30] …”

Section: Introductionmentioning

confidence: 99%

“…In several studies comparing different LC formats and approaches e.g. the use of monolithic supports, sub-2 µm particles or elevated column temperature, the latter is the most attractive option when efficiencies higher than 70,000 plates are required [20][21][22]. The use of UHPLC in combination with high temperature, would intuitively be the superior approach.…”

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confidence: 99%

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High-efficiency hydrophilic interaction chromatography by coupling 25cm×4.6mm ID×5μm silica columns and operation at 80°C

Louw

Lynen

Hanna-Brown

et al. 2010

Journal of Chromatography A

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Recently, hydrophilic interaction chromatography (HILIC) has emerged as a valuable orthogonal tool to reversed-phase liquid chromatography (RP-LC) as it allows for resolution of highly polar ionisable compounds. The relationships between separation efficiency, column length and speed of analysis for 4.6 mm ID x 5 µm silica particle columns in HILIC are demonstrated using kinetic plots. The kinetic plots constructed for conventional pressure systems operating at 350 bar and at 30 o C and 80°C are confirmed using experimental data for different column lengths. Efficiencies of more than 130,000 theoretical plates could be achieved by connecting up to six columns of 25 cm. As expected, a significant gain in analysis speed without loss of efficiency could be obtained by operating at 80°C compared to 30°C. The advantages of using long columns in HILIC in combination with elevated column temperature for the pharmaceutical industry are illustrated using test mixtures comprised of commercially available ionisable compounds (including some containing functional groups with potential genotoxic typical structural alerts) as well as real polar ionisable pharmaceuticals. Keywords:Hydrophilic interaction liquid chromatography, high efficiency, kinetic plots, temperature, speed 3 Correspondence:Professor Pat Sandra, Ghent University, Krijgslaan 281 S4-bis, B-9000, Ghent, Belgium E-mail: pat.sandra@richrom.comTel: +32 56 204031; Fax: +32 56 204858 IntroductionReversed-phase liquid chromatography (RP-LC) is by far the most widely employed analytical tool in drug discovery and development. In recent years, the efficiency of RP-LC has been drastically increased through various approaches including using sub-2µm particles in combination with ultra high pressure LC (UHPLC) [1][2][3], increasing the column length and operation at elevated temperature (ETLC) [4][5][6] or by combining both UHPLC and ETLC [7,8].These developments have certainly facilitated the development of generic methodologies for RP-LC for separations of active pharmaceutical ingredients (API's) and impurities [5].Furthermore, these advances have helped separation scientists to exploit early fundamental theories around the principles of separation optimisation with respect to efficiency and speed by utilisation of kinetic plots. For the pharmaceutical industry, which will certainly still have a plethora of conventional HPLC instrumentation in its good manufacturing practice (GMP) laboratories, kinetic plots can certainly serve a purpose in directing how conventional instrumentation and columns can be used more appropriately in combination with ETLC and long columns. This can help to optimize the use of conventional particle diameters (5 µm) to yield either maximum efficiency and to compared to sub-2µm particles, or to increased the speed of analysis.Since these developments, a chromatographic technique that has been enjoying recent attention in the pharmaceutical industry is hydrophilic interaction chromatography (HILIC).HILIC has become a valuable addition t...

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Chromatography, Liquid

Poole¹

2013

Kirk-Othmer Encyclopedia of Chemical Technology

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Liquid chromatography is a separation technique with three main variants: column liquid chromatography, planar (thin‐layer) chromatography, and capillary electrochromatography. Separations are achieved by the distribution of sample components between a mobile liquid phase and (generally) a porous solid stationary phase. Selectivity differences result from the differences in adsorption, partition, size exclusion, molecular recognition, and electrostatic interactions in the two phases. Defined by mechanism, the main types of liquid chromatography are known as liquid–solid (normal‐phase), reversed‐phase, size‐exclusion, ion‐exchange, affinity, chiral, hydrophilic interaction, and hydrophobic interaction liquid chromatography. These separation mechanisms are supported by a wide range of stationary phase materials whose surface chemistry and morphology are designed for optimum performance selected from porous inorganic oxide, porous organic polymers, porous graphitic carbon, chemically bonded inorganic oxides, and chemically modified porous polymers. Liquid chromatographic methods can also be classified by speed, separation performance, and scale. Here, system properties defined by instrumental parameters have to be considered simultaneously with the physical properties of the stationary phase. Analytical and preparative‐scale applications require different instrument platforms. The method used to control the mobile phase flow (capillary forces, pneumatic forces, or electroosmosis) are further important to design criteria. Liquid chromatographic methods are also sustained by a variety of detection possibilities based on the principles of bulk property and solute property methods employing spectroscopic, electrochemical, light scattering, and ion formation techniques.

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Sense and nonsense of high-temperature liquid chromatography

Cited by 185 publications

References 160 publications

Recent developments in the rapid analysis of plants and tracking their bioactive constituents

Recent developments in the rapid analysis of plants and tracking their bioactive constituents

High-efficiency hydrophilic interaction chromatography by coupling 25cm×4.6mm ID×5μm silica columns and operation at 80°C

Chromatography, Liquid

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