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Professor David McCalley's Outputs (65)

Practical examination of flow rate effects and influence of the stationary phase water layer on peak shape and retention in hydrophilic interaction liquid chromatography (2023)
Journal Article

The effect of flow velocity on retention and peak shape of neutral, acidic and basic probe compounds was studied using seven different UHPLC hydrophilic interaction chromatography (HILIC) columns. Surprisingly on some columns, the retention factor k... Read More about Practical examination of flow rate effects and influence of the stationary phase water layer on peak shape and retention in hydrophilic interaction liquid chromatography.

Understanding and managing peak shape for basic solutes in reversed-phase high performance liquid chromatography (2023)
Journal Article

While other separation mechanisms can challenge the dominance of reversed phase (for example in the separation of native proteins), reversed phase liquid chromatography is the method of choice for the analysis of a wide variety of samples. However, b... Read More about Understanding and managing peak shape for basic solutes in reversed-phase high performance liquid chromatography.

Influence of metals in the column or instrument on performance in hydrophilic interaction liquid chromatography (2021)
Journal Article

A method is proposed for measuring the relative contribution of extracolumn and column effects to the detrimental interactions which occur between metal-sensitive solutes and the complete HPLC system. The method involves the substitution of a length... Read More about Influence of metals in the column or instrument on performance in hydrophilic interaction liquid chromatography.

Alternative mobile phase additives for the characterization of protein biopharmaceuticals in liquid chromatography – Mass spectrometry (2021)
Journal Article

When analyzing large complex protein biopharmaceuticals, ion-pairing agents imparting low pH are widely used as mobile phase additives to improve the chromatographic performance. However, one of the most effective additives in RPLC and HILIC, trifluo... Read More about Alternative mobile phase additives for the characterization of protein biopharmaceuticals in liquid chromatography – Mass spectrometry.

Evaluation of a linear free energy relationship for the determination of the column void volume in hydrophilic interaction chromatography (2021)
Journal Article

The application of a linear free energy relationship (LFER) to a variety of hydrophilic interaction chromatography columns with different bonded ligands and pore sizes was studied in order to determine their void volume Vm. The method was based on th... Read More about Evaluation of a linear free energy relationship for the determination of the column void volume in hydrophilic interaction chromatography.

Evaluation of additives on reversed-phase chromatography of monoclonal antibodies using a 1000 Å stationary phase (2019)
Journal Article

© 2019 Elsevier B.V. A wide pore (1000 Å) diphenyl stationary phase was evaluated for the analysis of monoclonal antibodies (mAbs), comparing a conventional mobile phase of acetonitrile-water containing overall 0.1% trifluoracetic acid (TFA) with a s... Read More about Evaluation of additives on reversed-phase chromatography of monoclonal antibodies using a 1000 Å stationary phase.

Retention characteristics of some antibiotic and anti-retroviral compounds in hydrophilic interaction chromatography using isocratic elution, and gradient elution with repeatable partial equilibration (2018)
Journal Article

© 2018 Elsevier B.V. The separation of some zwitterionic, basic and neutral antibiotic and antiretroviral compounds was studied using hydrophilic interaction chromatography (HILIC) on bare silica, bonded amide and urea superficially porous phases. T... Read More about Retention characteristics of some antibiotic and anti-retroviral compounds in hydrophilic interaction chromatography using isocratic elution, and gradient elution with repeatable partial equilibration.

Effect of mobile phase additives on solute retention at low aqueous pH in hydrophilic interaction liquid chromatography (2016)
Journal Article

© 2016 Elsevier B.V. Trifluoracetic acid (TFA) added to the aqueous acetonitrile mobile phase induces some unexpected changes in the ionic component of retention in hydrophilic interaction separations when using Type B silica and amide-bonded silica... Read More about Effect of mobile phase additives on solute retention at low aqueous pH in hydrophilic interaction liquid chromatography.

Some factors that can lead to poor peak shape in hydrophilic interaction chromatography, and possibilities for their remediation (2016)
Journal Article

© 2015 Elsevier B.V. Some factors which present difficulties for obtaining good peak shape in hydrophilic interaction chromatography (HILIC) were studied. The effect of injection solvent composition and volume was systematically investigated using a... Read More about Some factors that can lead to poor peak shape in hydrophilic interaction chromatography, and possibilities for their remediation.

The impact of pressure and frictional heating on retention, selectivity and efficiency in ultra-high-pressure liquid chromatography (2014)
Journal Article

© 2014 Elsevier B.V. The effects of pressure and frictional heating deserve serious consideration in ultra-high-pressure liquid chromatography (UHPLC) separations, as the pressures used can be three times greater than those in conventional high-perfo... Read More about The impact of pressure and frictional heating on retention, selectivity and efficiency in ultra-high-pressure liquid chromatography.

Comparison of peak shape in hydrophilic interaction chromatography using acidic salt buffers and simple acid solutions (2014)
Journal Article

The retention and peak shape of neutral, basic and acidic solutes was studied on hydrophilic interaction chromatography (HILIC) stationary phases that showed both strong and weak ionic retention characteristics, using aqueous-acetonitrile mobile phas... Read More about Comparison of peak shape in hydrophilic interaction chromatography using acidic salt buffers and simple acid solutions.

Comparison of the kinetic performance and retentivity of sub-2ÎĽm core-shell, hybrid and conventional bare silica phases in hydrophilic interaction chromatography (2014)
Journal Article

© 2014 Elsevier B.V. The separation performance and retention properties of four sub-2μm underivatised silica materials were evaluated in the hydrophilic interaction chromatography (HILIC) mode. These included an organic/inorganic hybrid silica, conv... Read More about Comparison of the kinetic performance and retentivity of sub-2μm core-shell, hybrid and conventional bare silica phases in hydrophilic interaction chromatography.

Practical observations on the performance of bare silica in hydrophilic interaction compared with C18 reversed-phase liquid chromatography (2013)
Journal Article

The kinetic performance of a bare silica and C18 phase prepared from the same sub-2. ÎĽm and 3.5. ÎĽm base materials were compared in the HILIC and RP mode using both charged and neutral solutes. The HILIC column was characterised using the neutral sol... Read More about Practical observations on the performance of bare silica in hydrophilic interaction compared with C18 reversed-phase liquid chromatography.

Influence of phase type and solute structure on changes in retention with pressure in reversed-phase high performance liquid chromatography (2013)
Journal Article

The influence of pressure on the retention of several types of solute, including acids, bases and neutrals, was studied by the use of restriction capillaries added to the end of various monomeric and polymeric octadecylsilyl-modified 5. ÎĽm particle s... Read More about Influence of phase type and solute structure on changes in retention with pressure in reversed-phase high performance liquid chromatography.

Practical investigation of the factors that affect the selectivity in hydrophilic interaction chromatography (2013)
Journal Article

Retention data for a series of 29 compounds comprising acids, bases and neutrals were obtained on six different hydrophilic interaction (HILIC) columns including bare silica, zwitterionic and those bonded with neutral bonded ligands. The principal ai... Read More about Practical investigation of the factors that affect the selectivity in hydrophilic interaction chromatography.

The effect of pressure and mobile phase velocity on the retention properties of small analytes and large biomolecules in ultra-high pressure liquid chromatography (2012)
Journal Article

A possible complication of ultra-high pressure liquid chromatography (UHPLC) is related to the effect of pressure and mobile phase velocity on the retention properties of the analytes. In the present work, numerous model compounds have been selected... Read More about The effect of pressure and mobile phase velocity on the retention properties of small analytes and large biomolecules in ultra-high pressure liquid chromatography.

A comparison of overload behaviour for some sub 2ÎĽm totally porous and sub 3ÎĽm shell particle columns with ionised solutes (2012)
Journal Article

The overloading performance of some 2.7 ÎĽm shell and sub 2 ÎĽm totally porous columns, including one pair manufactured from similar materials with similar bonding chemistries, was compared using strongly acidic and basic probe compounds. In general, t... Read More about A comparison of overload behaviour for some sub 2ÎĽm totally porous and sub 3ÎĽm shell particle columns with ionised solutes.

Determination of catecholamines in urine using hydrophilic interaction chromatography with electrochemical detection (2011)
Journal Article

The determination of catecholamines in urine was investigated using hydrophilic interaction chromatography (HILIC) as an alternative to the commonly used reversed-phase (RP) method. A number of different approaches were explored, including per-aqueou... Read More about Determination of catecholamines in urine using hydrophilic interaction chromatography with electrochemical detection.

Some practical comparisons of the efficiency and overloading behaviour of sub-2ÎĽm porous and sub-3ÎĽm shell particles in reversed-phase liquid chromatography (2011)
Journal Article

At their optimum flow, sub-3 ÎĽm superficially porous or " shell" particles demonstrate similar efficiency to sub-2 ÎĽm totally porous particles. The performance of 0.21. cm i.d shell columns is however inferior to those of 0.46. cm i.d., presumably du... Read More about Some practical comparisons of the efficiency and overloading behaviour of sub-2ÎĽm porous and sub-3ÎĽm shell particles in reversed-phase liquid chromatography.

Instrumental considerations for the effective operation of short, highly efficient fused-core columns. Investigation of performance at high flow rates and elevated temperatures (2010)
Journal Article

Fused core or superficially porous columns offer the advantages of higher efficiency compared with totally porous columns of the same particle size, but similar operating pressures. However, their performance may be adversely affected by extra-column... Read More about Instrumental considerations for the effective operation of short, highly efficient fused-core columns. Investigation of performance at high flow rates and elevated temperatures.

Study of the selectivity, retention mechanisms and performance of alternative silica-based stationary phases for separation of ionised solutes in hydrophilic interaction chromatography (2010)
Journal Article

The separation of a mixture of neutral, strongly acidic and strongly basic compounds was studied in hydrophilic interaction chromatography using a bare silica phase, and bonded silica phases with diol, zwitterionic, amide and hydrophilic/hydrophobic... Read More about Study of the selectivity, retention mechanisms and performance of alternative silica-based stationary phases for separation of ionised solutes in hydrophilic interaction chromatography.

The challenges of the analysis of basic compounds by high performance liquid chromatography: Some possible approaches for improved separations (2010)
Journal Article

This review considers some of the difficulties encountered with the analysis of ionised bases using reversed-phase chromatography, such as detrimental interaction with column silanol groups, and overloading which both lead to poor peak shapes. Method... Read More about The challenges of the analysis of basic compounds by high performance liquid chromatography: Some possible approaches for improved separations.

Further investigations of the effect of pressure on retention in ultra-high-pressure liquid chromatography (2010)
Journal Article

In this study, we investigated further the large increases in retention with pressure that we observed previously in RP-LC especially for ionised solutes. These findings were initially confirmed on a conventional silica C18 column, which gave extreme... Read More about Further investigations of the effect of pressure on retention in ultra-high-pressure liquid chromatography.

Practical assessment of frictional heating effects and thermostat design on the performance of conventional (3 ÎĽm and 5 ÎĽm) columns in reversed-phase high-performance liquid chromatography (2009)
Journal Article

A practical investigation of frictional heating effects in conventional C18 columns was undertaken, to investigate whether problems found for sub-2 ÎĽm columns were also present for those of particle size 3 ÎĽm and 5 ÎĽm and different internal diameter.... Read More about Practical assessment of frictional heating effects and thermostat design on the performance of conventional (3 ÎĽm and 5 ÎĽm) columns in reversed-phase high-performance liquid chromatography.

A new approach to the determination of column overload characteristics in reversed-phase liquid chromatography (2009)
Journal Article

Column overloading is very common during the separations of basic analytes in analytical scale reversed-phase liquid chromatography (RPLC). Due to the complex interactions of ionic analytes with stationary and mobile phases, only a very small amount... Read More about A new approach to the determination of column overload characteristics in reversed-phase liquid chromatography.

Investigation of the effect of pressure on retention of small molecules using reversed-phase ultra-high-pressure liquid chromatography (2008)
Journal Article

The effect of inlet pressure on the retention of a series of low molecular weight acids, bases and neutrals, was investigated at constant temperature in reversed-phase liquid chromatography using a commercial ultra-high-pressure system (Waters UPLC i... Read More about Investigation of the effect of pressure on retention of small molecules using reversed-phase ultra-high-pressure liquid chromatography.

Evaluation of the properties of a superficially porous silica stationary phase in hydrophilic interaction chromatography (2008)
Journal Article

The sample capacity, column efficiency (and its variation with flow) of a superficially porous unbonded silica phase (Halo) was investigated using hydrophilic interaction chromatography (HILIC), particularly for separation of basic compounds. Sample... Read More about Evaluation of the properties of a superficially porous silica stationary phase in hydrophilic interaction chromatography.

Estimation of the extent of the water-rich layer associated with the silica surface in hydrophilic interaction chromatography (2008)
Journal Article

The possible presence of a mobile phase layer rich in water on the surface of silica columns used under conditions typical in hydrophilic interaction chromatography was investigated by the injection of a small hydrophobic solute (benzene) using aceto... Read More about Estimation of the extent of the water-rich layer associated with the silica surface in hydrophilic interaction chromatography.

Analysis of basic compounds by reversed-phase high-performance liquid chromatography using hybrid inorganic/organic phases at high pH (2008)
Journal Article

The retention and mass overload of five bases and a quaternary ammonium compound were studied on a bridged ethyl hybrid inorganic/organic phase (XBridge C18) over a pH range 2.7-12.0 using acetonitrile-phosphate and carbonate buffers. Some comparison... Read More about Analysis of basic compounds by reversed-phase high-performance liquid chromatography using hybrid inorganic/organic phases at high pH.

Is hydrophilic interaction chromatography with silica columns a viable alternative to reversed-phase liquid chromatography for the analysis of ionisable compounds? (2007)
Journal Article

The separation of acidic, neutral and particularly basic solutes was investigated using a bare silica column, mostly under hydrophilic interaction chromatography (HILIC) conditions with water concentrations >2.5% and with >70% acetonitrile (ACN). Pro... Read More about Is hydrophilic interaction chromatography with silica columns a viable alternative to reversed-phase liquid chromatography for the analysis of ionisable compounds?.

A study of retention and overloading of basic compounds with mixed-mode reversed-phase/cation-exchange columns in high performance liquid chromatography (2007)
Journal Article

The retention and overload of bases were studied on two new mixed-mode, silica based phases possessing ionic carboxylate functionalities of different acidity embedded within a hydrophobic ligand (SiELC Primesep™). At low pH, good peak shapes were obt... Read More about A study of retention and overloading of basic compounds with mixed-mode reversed-phase/cation-exchange columns in high performance liquid chromatography.

Study of overload for basic compounds in reversed-phase high performance liquid chromatography as a function of mobile phase pH (2006)
Journal Article

The retention and overloading properties for eight basic solutes and two quaternary ammonium compounds were studied over the pH range 2.7-10.0 using phosphate and carbonate buffers. At low pH, a hybrid inorganic-organic silica-ODS phase (XTerra RP-18... Read More about Study of overload for basic compounds in reversed-phase high performance liquid chromatography as a function of mobile phase pH.

Study of overloading of basic drugs and peptides in reversed-phase high-performance liquid chromatography using pH adjustment of weak acid mobile phases suitable for mass spectrometry (2005)
Journal Article

Serious losses in column efficiency for ionised basic drugs and peptides occur due to overloading of C18 phases when weak acid mobile phases of low ionic strength suitable for mass spectrometric detection are used. Measurable changes in retention tim... Read More about Study of overloading of basic drugs and peptides in reversed-phase high-performance liquid chromatography using pH adjustment of weak acid mobile phases suitable for mass spectrometry.

Comparison of an organic polymeric column and a silica-based reversed-phase for the analysis of basic peptides by high-performance liquid chromatography (2005)
Presentation / Conference Contribution

The performance of a purely polymeric and a Type B silica-based C 18 reversed-phase column was compared for the analysis of the basic peptide bradykinin and some analogues in order to assess the contribution of silanol interactions to peak shape. Goo... Read More about Comparison of an organic polymeric column and a silica-based reversed-phase for the analysis of basic peptides by high-performance liquid chromatography.

Rationalization of retention and overloading behavior of basic compounds in reversed-phase HPLC using low ionic strength buffers suitable for mass spectrometric detection (2003)
Journal Article

The retention and overloading behavior of some basic (and acidic) compounds has been studied on different RP-HPLC columns in buffers of varying ionic strength. Anomalous retention patterns of acids and bases were found on one phase in low-pH, volatil... Read More about Rationalization of retention and overloading behavior of basic compounds in reversed-phase HPLC using low ionic strength buffers suitable for mass spectrometric detection.

Overloading study of bases using polymeric RP-HPLC columns as an aid to rationalization of overloading on silica-ODS phases (2002)
Journal Article

The separation of ionized bases by reversed-phase liquid chromatography with alkyl silica columns often leads to severely tailed bands that are highly detrimental. Band shape and its dependence on sample mass are notably different when mobile-phase p... Read More about Overloading study of bases using polymeric RP-HPLC columns as an aid to rationalization of overloading on silica-ODS phases.

Towards the development of molecularly imprinted polymer based screen-printed sensors for metabolites of PAHs (2001)
Presentation / Conference Contribution

This paper describes the fabrication of a sensor for 1-hydroxypyrene (1-OHP) based on a screen-printed carbon electrode (SPCE) modified with a molecularly imprinted polymer (MIP); 1-OHP was chosen as a model metabolite of polyaromatic hydrocarbons (P... Read More about Towards the development of molecularly imprinted polymer based screen-printed sensors for metabolites of PAHs.