Improvements in the predictive accuracy of the hydrophobic subtraction model of reversed-phase selectivity

Stoll, Dwight R.; Dahlseid, Tina A.; Rutan, Sarah C.; Taylor, Tony; Serret, Josep M.

doi:10.1016/j.chroma.2020.461682

Cited by 15 publications

(11 citation statements)

References 16 publications

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“…Columns for screening were selected based on the different bonding, pH range, selectivity difference and different similarity factors ( Fs ) (Stoll et al, 2021). For screening experiments, five different column chemistries were selected based on the bonding, pH range and selectivity.…”

Section: Methodsmentioning

confidence: 99%

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Application of the “Method Operable Design Region” (MODR) approach for the development of a UHPLC method for the assay and purity determination of risperidone in risperidone drug substance and other formulations

Amit

Nancy

2022

Biomedical Chromatography

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To understand the role of analytics in drug development, regulatory bodies also started using the approach of Quality by Design (QbD) during analytical method developments. The present study deals with the development of the “Method Operable Design Region” for assay and purity determination of risperidone in risperidone drug substance and formulations usingy UHPLC. Five different column chemistries, five different pH buffers, oven temperatures from 25 to 45°C, and different organic modifier composition, column lengths and flow rates were studied and statistically evaluated using Fusion QbD software. The final method parameters were selected by performing multivariable changes in a single run and evaluated using the Monte Carlo simulation approach. The uniqueness of this method is that it is mass compatible, a total of 10 peaks are separated within a short run time of 12.0 min and it uses a “Platforming approach”, which means the use of a single method for testing the drug substance, different strengths of a drug product and different formulations. The same method can be also used for the determination of the preservative (benzoic acid) in risperidone 1 mg/ml oral solution. The use of the QbD approach is aligned with the US Pharmacopeia <1220>, BP supplementary chapter 2022 and the International Conference on Harmonization Q14 guidelines for life cycle management of analytical methods.

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Section: Methodsmentioning

confidence: 99%

“…Columns for screening were selected based on the different bonding, pH range, selectivity difference and different similarity factors (Fs) (Stoll et al, 2021)…”

Section: Selection Of Columnsmentioning

confidence: 99%

Application of the “Method Operable Design Region” (MODR) approach for the development of a UHPLC method for the assay and purity determination of risperidone in risperidone drug substance and other formulations

Amit

Nancy

2022

Biomedical Chromatography

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“…For example, several groups have worked on predicting the effect of the mismatch between sample solvent and the mobile phase on peak shape and width in both one-and two-dimensional liquid chromatography (LC) [1][2][3][4]. Other groups have advanced understanding of the effect of temperature on retention in reversed-phase separations [5], worked to improve general models of retention and selectivity in RP separations [6,7], and explored the limits and implementations of retention models as a key components of method development workflows for both one-and two-dimensional LC separations [8][9][10].…”

Section: Introductionmentioning

confidence: 99%

Characterization of a High Throughput Approach for Large Scale Retention Measurement in Liquid Chromatography

Kempen

Dahlseid

Lauer

et al. 2023

Preprint

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Many contemporary challenges in liquid chromatography - such as the need for “smarter” method development tools, and deeper understanding of chromatographic phenomena - could be addressed more efficiently and effectively with larger volumes of experimental retention data than we have been accustomed to historically. The paucity of publicly accessible, high-quality measurements has been due, at least in large part, to the high cost in time and resources associated with traditional retention measurement approaches. Recently we described an approach to improve the throughput of such measurements by using very short columns (typically 5 mm), while maintaining measurement accuracy. In this paper we present a perspective on the characteristics of results obtained using this approach using a dataset containing about 13,000 retention measurements, and describe an approach to sample introduction that improves upon the prior work. The dataset is comprised of results for 35 different small molecules, nine different stationary phases, and several mobile phase compositions for each analyte/phase combination. During the acquisition of these data, we have interspersed repeated measurements of a small number of compounds for quality control purposes. The data from these measurements not only enable detection of “out of control” measurements, but also assessment of the repeatability and reproducibility of retention measurements over time. For retention factors greater than 1, the mean relative standard deviation (RSD) of replicate (typically n=5) measurements is 0.4%, and the standard deviation of RSDs is 0.4%. Most differences between selectivity values measured six months apart for 15 non-ionogenic compounds were in the range of +/- 1%, indicating good reproducibility. A critically important observation from these analyses is that selectivity (defined here as retention of a given analyte relative to the retention of a reference compound; kx/kref) is a much more consistent measure of retention over time (months) compared to the retention factor alone. While this work and dataset also highlights the importance of stationary phase stability over time for achieving reliable retention measurements, we are nevertheless optimistic that this approach will enable the compilation of large databases (>> 10,000 measurements) of retention values over long time periods (years), which can in turn be leveraged to address some of the most important contemporary challenges in liquid chromatography. All of the data discussed in the manuscript are provided as Supplemental Information.

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“…Currently, these efforts depend on experimental data to build models that are accurate enough to be useful in method development. In our own work we are very interested in increasing the throughput of high quality measurements, both for the purpose of improving the accuracy of existing retention/selectivity models (e.g., HSM2 for RPLC [13]), and for opening new lines of investigation that would allow modeling aspects of LC separations that thus far have been relatively untouched, such as optimization of second dimension elution conditions in twodimensional liquid chromatography [3].…”

Section: Introductionmentioning

confidence: 99%

An approach to high throughput measurement of accurate retention data in liquid chromatography

Stoll

Kainz

Dahlseid

et al. 2022

Journal of Chromatography A

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Improvements in the predictive accuracy of the hydrophobic subtraction model of reversed-phase selectivity

Cited by 15 publications

References 16 publications

Application of the “Method Operable Design Region” (MODR) approach for the development of a UHPLC method for the assay and purity determination of risperidone in risperidone drug substance and other formulations

Application of the “Method Operable Design Region” (MODR) approach for the development of a UHPLC method for the assay and purity determination of risperidone in risperidone drug substance and other formulations

Characterization of a High Throughput Approach for Large Scale Retention Measurement in Liquid Chromatography

An approach to high throughput measurement of accurate retention data in liquid chromatography

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