Optimizing selectivity during reversed-phase high performance liquid chromatography method development: Prioritizing experimental conditions

Snyder, Lloyd R.; Dolan, John W.

doi:10.1016/j.chroma.2013.05.082

Cited by 23 publications

(10 citation statements)

References 16 publications

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“…The analytical method development and optimization were performed through a design of experiment (DoE) study by modifying simultaneously multiple critical method parameters (CMPs), which can affect critical method attributes (CMAs) such as resolution (Rs), peak tailing (T), and selectivity ( α ) (Lloyd R. Snyder & Dolan, 2013 ).…”

Section: Resultsmentioning

confidence: 99%

“…The reverse mode of elution was used due to the properties of the analytes present in plant matrices being of medium polarity to non-polar, and for the same reasons, the use of ionic paring was not considered as a variable. The orthogonality values for the pre-selected stationary phases were obtained from the results of Fs described on the website of the American Pharmacopoeia, which is based on the theory of hydrophobic subtraction developed by Snyder and collaborators ( USP, 2005 ; Snyder & Dolan, 2013 ; Cass, 2015 ; Lloyd R.).…”

Section: Resultsmentioning

confidence: 99%

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Chromatography Conditions Development by Design of Experiments for the Chemotype Differentiation of Four Bauhinia Species

et al. 2022

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The extensive use of medicinal herbs to traditionally treat disease persists for generations, and scientific evidence on plant-derived extracts has indicated their numerous biological activities. The Bauhinia, popular known as cow’s paw (“pata de vaca”), with more than 60 native species, are extensively used in Brazilian popular medicine for the control of diabetes. Therefore, in 2009, B. forficata, B. variegata and/or B. affinis were included in the Brazilian National List of Medicinal Plants of Interest to SUS (RENISUS - Brazil). In this context, this work reports the results of the chemical differentiation of B. forficata, B. variegata, B. longifolia, and B. affinis using liquid chromatography coupled to high-resolution mass spectrometry and unsupervised chemometric tools. Chromatographic conditions were optimized by using the design of experiments (DoE) and chromatographic knowledge. Furthermore, the chemical profile of the studied species was analyzed by principal component analysis (PCA) and hierarchical cluster analysis that differentiated the four species of Bauhinia, and 55 compounds were also inferred by MS2 experiments, some of them for the first time in B. affinis. In this manner, this work provides important information that could be used in quality control, development of new pharmaceuticals, and food products based on Bauhinia leaves, as well as to explain ethnomedicinal properties, pharmacological and toxicological actions.

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Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Chromatography Conditions Development by Design of Experiments for the Chemotype Differentiation of Four Bauhinia Species

et al. 2022

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“…We anticipate these results to be true for typical RP type phases but there have been few comparisons of the dependence of S , ln k w and their temperature derivatives on the different RP materials [61]. …”

Section: Discussionmentioning

confidence: 96%

“…The opposite trend is observed for t G . The change in the relative retention time at the three gradient times tested is not at all proportional to the gradient time.The retention times of the intermediately eluted compounds are more influenced by T , ϕ o and F whereas ϕ f and t G have more effect on the retention times of the later eluting compounds.Isocratic retention times are more sensitive to flow rate disturbances, temperature and mobile phase composition fluctuations than are gradient elution retention times.We anticipate these results to be true for typical RP type phases but there have been few comparisons of the dependence of S , ln k w and their temperature derivatives on the different RP materials [61]. …”

Section: Discussionmentioning

confidence: 99%

Instrument parameters controlling retention precision in gradient elution reversed-phase liquid chromatography

Beyaz

Fan

Carr

et al. 2014

Journal of Chromatography A

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The precision of retention time in RPLC is important for compound identification, for setting peak integration time windows and in fundamental studies of retention. In this work, we studied the effect of temperature (T), initial (ϕ0) and final mobile phase (ϕf)composition, gradient time (tG), and flow rate (F) on the retention time precision under gradient elution conditions for various types of low MW solutes. We determined the retention factor in pure water (k′w) and the solute-dependent solvent strength (S) parameters of Snyder's linear solvent strength theory (LSST) as a function of temperature for three different groups of solutes. The effect of small changes in the chromatographic variables (T, ϕ0, ϕf, tG and F) by use of the LSST gradient retention equation were estimated. Peaks at different positions in the chromatogram have different sensitivities to changes in these instrument parameters. In general, absolute fluctuations in retention time are larger at longer gradient times. Drugs showed less sensitivity to changes in temperature compared to relatively less polar solutes, non-ionogenic solutes. Surprisingly we observed that fluctuations in temperature, mobile phase composition and flow rate had less effect on retention time under gradient conditions as compared to isocratic conditions. Overall temperature and the initial mobile phase composition are the more important variables affecting retention reproducibility in gradient elution chromatography.

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“…It utilizes the theoretical or statistical models and is usually done in accordance with Quality by Design (QbD) principles . In this paradigm one does a set of carefully designed preliminary experiments (scouting experiments) and based on the gathered data decides about the conditions leading to the desired chromatogram . This approach can accommodate up to 12 experiments for three experimental variables (e.g., gradient time or isocratic %B, pH, and temperature) but it works well with two experimental runs if only organic modifier is considered.…”

Section: Introductionmentioning

confidence: 99%

Evaluation of sequential Bayesian‐based method development procedures for chromatographic problems involving one, two, and three analytes

Wiczling

2018

Separation Science Plus

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In this work, various sequential Bayesian‐based method development procedures associated with a search of isocratic chromatographic conditions ensuring baseline separation of one, two, and three analytes within the pre‐specified retention time window were evaluated. The accuracy and total analysis time of tested procedures were experimentally and theoretically verified and compared with the usual approaches utilizing one or two preliminary organic modifier gradients. The possession of strong and weakly informative priors about analytes was considered. The overall success rate of tested procedures was high with a small number of mistakes. It was shown that for simple problems considered here one is able to use a sequence of isocratic conditions to find the desired chromatogram. The use of one preliminary gradient was shown to be of similar accuracy and time requirements. Interestingly, the use of two preliminary gradients almost always required more time than procedures involving no or one preliminary gradient. Prior knowledge of analytes considerably shortened method development times for procedures involving no or one preliminary gradient. The sequential Bayesian‐based method development allows us to achieve a desired chromatographic separation by proper weighting of information available to the analyst at each stage of the method development process.

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Optimizing selectivity during reversed-phase high performance liquid chromatography method development: Prioritizing experimental conditions

Cited by 23 publications

References 16 publications

Chromatography Conditions Development by Design of Experiments for the Chemotype Differentiation of Four Bauhinia Species

Chromatography Conditions Development by Design of Experiments for the Chemotype Differentiation of Four Bauhinia Species

Instrument parameters controlling retention precision in gradient elution reversed-phase liquid chromatography

Evaluation of sequential Bayesian‐based method development procedures for chromatographic problems involving one, two, and three analytes

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