A simple and efficient approach to reversed-phase HPLC method screening

Biswas, Kallol; Castle, Bryan C.; Olsen, Bernard A.; Risley, Donald S.; Skibic, Michael J.; Wright, Paul

doi:10.1016/j.jpba.2008.12.039

Cited by 24 publications

(10 citation statements)

References 20 publications

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“…Thus, during method development, it is prudent to incorporate some level of column and mobile phase screening in order to obtain appropriate mass spectrometric response, in addition to achieving the requisite chromatographic separation with symmetrical and effi cient peaks. Such screening and optimization could be achieved effi ciently using automated systems (Xia et al, 2006b;Krisko et al, 2006;Biswas et al, 2009).…”

Section: Column Stationary Phase and Mobile Phase Selectionmentioning

confidence: 99%

Systematic LC‐MS/MS bioanalytical method development that incorporates plasma phospholipids risk avoidance, usage of incurred sample and well thought‐out chromatography

Jemal

Ouyang

Xia

2009

Biomedical Chromatography

181

124

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This treatise summarizes the underlying principle and the road map for systematic LC-MS/MS bioanalytical method development. The three themes that have recently emerged as central to building quality during method development-phospholipids, incurred sample and sound chromatographic considerations-are the main focus of this article. In order to reduce the bioanalytical risk associated with plasma phospholipids, a dual approach involving extraction and chromatography is recommended. The use of incurred sample during method development is essential to avoid interference arising from drug-related components. This is different from the current practice of incurred sample reanalysis, which tests reproducibility during method application. LC column/mobile phase optimization is needed to achieve appropriate peak shape, sensitivity and the separation of the analyte from interfering metabolites and phospholipids. Related to sound chromatographic considerations, we lay out facts and myths related to UPLC, vis-à-vis HPLC. Incorporation of quality during method development avoids the costly experience of finding out by chance about the invalidity of a method after it has been used in support of a number of pivotal clinical and non-clinical studies. To this end, we put forth an outline of a protocol for a systematic LC-MS/MS bioanalytical method development.

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Section: Column Stationary Phase and Mobile Phase Selectionmentioning

confidence: 99%

Systematic LC‐MS/MS bioanalytical method development that incorporates plasma phospholipids risk avoidance, usage of incurred sample and well thought‐out chromatography

Jemal

Ouyang

Xia

2009

Biomedical Chromatography

181

124

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“…Although PCA and HCA have been frequently applied to find similarities among particular chromatographic conditions [1,8,9], or specific chromatographic columns, the non-supervised character renders an ambiguity to the pattern. The main disadvantage of PCA is a loss of information with consecutive reduction of dimensionality by projecting data only to few principal components.…”

Section: Comparison Of Chromatographic Columns By Means Of Srd and Gpcmmentioning

confidence: 99%

How to compare separation selectivity of high-performance liquid chromatographic columns properly?

Andrić

Héberger

2017

Journal of Chromatography A

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Comparison and selection of chromatographic columns is an important part of development as well as validation of analytical methods. Presently there is abundant number of methods for selection of the most similar and orthogonal columns, based on the application of limited number of test compounds as well as quantitative structure retention relationship models (QSRR), from among Snyder's hydrophobicsubtraction model (HSM) have been most extensively used.Chromatographic data of 67 compounds were evaluated using principal component analysis (PCA), hierarchical cluster analysis (HCA), non-parametric ranking methods as sum of ranking differences (SRD) and generalized pairwise correlation method (GPCM), both applied as a consensus driven comparison, and complemented by the comparison with one variable at a time (COVAT) approach. The aim was to compare the ability of the HSM approach and the approach based on primary retention data of test solutes (logk values) to differentiate among ten highly similar C18 columns.The ranking (clustering) pattern of chromatographic columns based on primary retention data and HSM parameters gave different results in all instances. Patterns based on retention coefficients were in accordance with expectations based on columns' physicochemical parameters, while HSM parameters provided a different clustering.Similarity indices calculated from the following dissimilarity measures: SRD, GPCM Fisher's conditional exact probability weighted (CEPW) scores; Euclidian, Manhattan, Chebyshev, and cosine distances Pearson's, Spearman's, and Kendall's, correlation coefficients have been ranked by the consensus based SRD. Analysis of variance confirmed that the HSM model produced statistically significant increases of SRD values for the majority of similarity indices, i.e. HSM transformation of original retention data yields significant loss of information, and finally results in lower performance of HSM methodology. The best similarity measures were obtained using primary retention data, and derived from Kendal's and Spearman's correlation coefficients, as well as GPCM and SRD score values. Selectivity function, Fs, originally proposed by Snyder, demonstrated moderate performance.

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“…a part of HPLC method development. It typically starts with the selection of the optimal combination of HPLC column and mobile phase (organic and pH modifiers) to maximize selectivity for the separation [18]. Then instrument parameters like UV wavelength, flow rate, injection volume, and temperature are further evaluated in order to optimize sensitivity, limit of detection (LOD), and signalto-noise ratio (S/N).…”

Section: Introductionmentioning

confidence: 99%

Multivariate figures of merit (FOM) investigation on the effect of instrument parameters on a Fourier transform-near infrared spectroscopy (FT-NIRS) based content uniformity method on core tablets

Doddridge

Shi

2015

Journal of Pharmaceutical and Biomedical Analysis

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A simple and efficient approach to reversed-phase HPLC method screening

Cited by 24 publications

References 20 publications

Systematic LC‐MS/MS bioanalytical method development that incorporates plasma phospholipids risk avoidance, usage of incurred sample and well thought‐out chromatography

Systematic LC‐MS/MS bioanalytical method development that incorporates plasma phospholipids risk avoidance, usage of incurred sample and well thought‐out chromatography

How to compare separation selectivity of high-performance liquid chromatographic columns properly?

Multivariate figures of merit (FOM) investigation on the effect of instrument parameters on a Fourier transform-near infrared spectroscopy (FT-NIRS) based content uniformity method on core tablets

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