Aspects of the “Design Space” in high pressure liquid chromatography method development

Molnár, Imre; Rieger, Hans-Jürgen; Monks, K.

doi:10.1016/j.chroma.2010.02.001

Cited by 100 publications

(34 citation statements)

References 3 publications

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“…Conceptually, the presently proposed segmented gradient optimization methods can readily fit in the advanced 3D or 4D MD strategies used nowadays [31,32]. either as the final step after selection of the most promising stationary phase, modifier solvent, pH and T (typically done via a design of experiments approach), or as an integral part of the 3D or 4D search algorithm.…”

Section: Resultsmentioning

confidence: 99%

Enhanced selectivity and search speed for method development using one-segment-per-component optimization strategies

Tyteca

Vanderlinden

Favier

et al. 2014

Journal of Chromatography A

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a b s t r a c tLinear gradient programs are very frequently used in reversed phase liquid chromatography to enhance the selectivity compared to isocratic separations. Multi-linear gradient programs on the other hand are only scarcely used, despite their intrinsically larger separation power. Because the gradient-conformity of the latest generation of instruments has greatly improved, a renewed interest in more complex multisegment gradient liquid chromatography can be expected in the future, raising the need for better performing gradient design algorithms. We explored the possibilities of a new type of multi-segment gradient optimization algorithm, the so-called "one-segment-per-group-of-components" optimization strategy. In this gradient design strategy, the slope is adjusted after the elution of each individual component of the sample, letting the retention properties of the different analytes auto-guide the course of the gradient profile. Applying this method experimentally to four randomly selected test samples, the separation time could on average be reduced with about 40% compared to the best single linear gradient. Moreover, the newly proposed approach performed equally well or better than the multi-segment optimization mode of a commercial software package. Carrying out an extensive in silico study, the experimentally observed advantage could also be generalized over a statistically significant amount of different 10 and 20 component samples. In addition, the newly proposed gradient optimization approach enables much faster searches than the traditional multi-step gradient design methods.

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Section: Resultsmentioning

confidence: 99%

Enhanced selectivity and search speed for method development using one-segment-per-component optimization strategies

Tyteca

Vanderlinden

Favier

et al. 2014

Journal of Chromatography A

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“…To get the preferred retention time as well as proper tailing factor, several parameters like column length, column temperature, particle size of stationary phase, type of buffer, molarity of buffer, mobile phase composition, etc. have to be studied [33]. But due to the resource and time constraints only most critical parameters like molarity of ion-pair reagent/modifier in mobile phase and composition of mobile phase were studied.…”

Section: Retention Timementioning

confidence: 99%

Rapid Screening of Volatile Ion-Pair Reagents Using UHPLC and Robust Analytical Method Development Using DoE for an Acetyl Cholinesterase Inhibitor: Galantamine HBr

et al. 2011

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As over 70% of pharmaceutical compounds are bases, the analysis of these basic compounds by high performance liquid chromatography (HPLC) continues to be of great value and interesting. Acetyl cholinesterase inhibitors (AChEIs), which contain the basic compounds like Rivastigmine tartrate, Galantamine hydrobromide and Donepezil with different polarities, were chosen for the study. A rapid screening of the volatile ion-pairing reagents was performed using modern techniques like ultra high performance liquid chromatography (UHPLC). The experiments were planned using the 'Design of Experiments' (DoE) approach to identify the LC-MS compatible ion-pair reagent. In this study, Heptafluorobutyric acid (HFBA) has given a very good peak shape with tailing factor at 1.4 and theoretical plates up to *5,000 were observed, compared to tailing factor at 1.9 and theoretical plates up to *3,000 with non-volatile ion-pair reagent sodium heptane sulphonate (SHS). Similarly retention with HFBA was optimum as *5 min in short run time method compared to *13 min with SHS. This ion-pair reagent has proved to be good replacement of sodium alkyl sulphonate modifiers. HFBA can also be used for semi-preparative work for isolation of impurities by just evaporating the solvents. It avoids the extraction of other inorganic modifiers.Keywords Ultra high performance liquid chromatography (UHPLC) Á Volatile ion-pair reagents Á Design of experiments (DoE) Á Acetylcholinesterase inhibitor (AChEI) Á Alzheimer's disease (AD)

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“…step 1 of the LC method development strategy described in the Introduction) established protocols for retention modelling and optimisation (i.e. step 2) were employed to develop robust LC methodologies [39][40][41][42][43][44][45]. Retention modelling and optimisation using the DryLab® software was performed with an UHPLC system capable of operating at 1,200 bar of pressure and possessing a low dwell volume and system dispersion volume suitable for use with rapid column formats (i.e.…”

Section: Retention Modelling and Optimisationmentioning

confidence: 99%

Chromatographic retention behaviour, modelling and separation optimisation of the quaternary ammonium salt isometamidium chloride and related compounds on a range of reversed-phase liquid chromatographic stationary phases

Schad

Euerby²,

Skellern

et al. 2012

Anal Bioanal Chem

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This paper describes the reversed-phase liquid chromatographic behaviour of the trypanocidal quaternary ammonium salt isometamidium chloride and its related compounds on a range of liquid chromatographic phases possessing alkyl and phenyl ligands on the same inert silica. In a parallel study with various extended polar selectivity phases which possessed different hydrophobic/silanophilic (hydrogen bonding) activity ratios, the chromatographic retention/selectivities of the quaternary ammonium salts was shown to be due to a co-operative mechanism between hydrophobic and silanophilic interactions. The highly aromatic and planar isometamidium compounds were found to be substantially retained on stationary phases containing aromatic functionality via strong π-π interactions. The chemometric approach of principal component analysis was used to characterise the chromatographic behaviour of the isometamidium compounds on the differing phases and to help identify the dominant retention mechanism(s). Two-dimensional (temperature/gradient) retention modelling was employed to develop and optimise a rapid liquid chromatography method for the separation of the six quaternary ammonium salts within 2.5 min which would be suitable for bioanalysis using liquid chromatography-mass spectrometry. This is the first reported systematic study of the relationship between stationary phase chemistries and retention/selectivity for a group of quaternary ammonium salts.

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Aspects of the “Design Space” in high pressure liquid chromatography method development

Cited by 100 publications

References 3 publications

Enhanced selectivity and search speed for method development using one-segment-per-component optimization strategies

Enhanced selectivity and search speed for method development using one-segment-per-component optimization strategies

Rapid Screening of Volatile Ion-Pair Reagents Using UHPLC and Robust Analytical Method Development Using DoE for an Acetyl Cholinesterase Inhibitor: Galantamine HBr

Chromatographic retention behaviour, modelling and separation optimisation of the quaternary ammonium salt isometamidium chloride and related compounds on a range of reversed-phase liquid chromatographic stationary phases

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