A fundamental study of the impact of pressure on the adsorption mechanism in reversed-phase liquid chromatography

Åsberg, Dennis; Samuelsson, Jörgen; Fornstedt, Torgny

doi:10.1016/j.chroma.2016.06.036

Cited by 13 publications

(3 citation statements)

References 39 publications

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“…To investigate this, the housing experiment could be repeated inside a pressurized chamber. Pressure effects were observed by Fornstedt et al on the adsorption energy distribution measured on a C18 column and attributed to higher pressure making the higher-energy silanols on the silica support bed more accessible to the adsorbate …”

Section: Resultsmentioning

confidence: 95%

Characterization of Drug–Polymer Adsorption Isotherms in Body-on-a-Chip Systems by Inverse Liquid–Solid Chromatography

Schnepper

Roles

Hickman

2020

ACS Biomater. Sci. Eng.

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Body-on-a-chip and human-on-a-chip systems are currently being used to augment and could eventually replace animal models in drug discovery and basic biological research. However, hydrophobic molecules, especially therapeutic compounds, tend to adsorb to the polymer materials used to create these microfluidic platforms, which may distort the dose–response curves that feed into pharmacokinetic/pharmacodynamic (PK/PD) models, which translate preclinical data into predictions of clinical outcomes. Inverse liquid–solid chromatography paired with a numerical optimization based on the Langmuir model of adsorption was used to characterize the adsorption isotherm parameters of drugs to polydimethylsiloxane (PDMS) and polymethylmethacrylate (PMMA), polymers commonly used in these platforms. The adsorption isotherms were then compared against concentration measurements of drugs recirculated in these platforms. This research further illustrates the point that by quantifying drug or drug candidate interactions before system dosing and including this data in the PK/PD models, then polymers used in these platforms need not be limited to “less-adsorbing” materials.

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Section: Resultsmentioning

confidence: 95%

Characterization of Drug–Polymer Adsorption Isotherms in Body-on-a-Chip Systems by Inverse Liquid–Solid Chromatography

Schnepper

Roles

Hickman

2020

ACS Biomater. Sci. Eng.

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“…The impact of the higher pressure limits and the larger pressure drops in UHPLC as compared to HPLC has been studied in depth by Asberg et al. . It has been observed that, in reversed phase LC, pressure influences retention, selectivity, and efficiency.…”

Section: Resultsmentioning

confidence: 99%

Ultra high performance liquid chromatography method development for separation of omeprazole and related substances on core‐shell columns using a Quality by Design approach

Johansson

Ludvigsson

2019

J of Separation Science

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An updated and improved method for analysis of omeprazole/esomeprazole and related substances on core‐shell columns was developed using Fusion LC Method Development™. The method was optimized with respect to column type, column temperature, mobile phase pH level, and gradient time. Four different core‐shell columns were examined to develop a method suitable for both high performance‐ and ultra‐high performance liquid chromatography using a Quality by Design approach. The final method offers two alternative columns: Poroshell EC C18 (3.0 × 100 mm, 2.7 µm) or Poroshell HPH (3.0 × 100 mm, 2.7 µm) with the same gradient elution condition and mobile phase composition. Total run time is 18 min with 12 min of gradient elution. Phosphate buffer (15 mM, pH 7.8) is selected as the aqueous mobile phase and acetonitrile as the organic mobile phase. Column temperature is set at 40°C and ultraviolet detection at 302 nm. Furthermore, by studying parameters in a systematic way, an understanding of the effect of the input parameters enhances the method robustness and should allow for regulatory flexibility in terms of post‐approval changes. Compared to the current United States Pharmacopeia method, the updated method is faster, more efficient and performs well above acceptance criteria.

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“…Alternatively, computerized and direct methods can be privileged to solve this problem. In contrast to the inverse methods, direct methods predict the outcome (retention times) directly from the independent and accurate measurements of the relevant properties of the column (hold-up volume, temperature, pressure), LC system (gradient dwell volume and dispersion), strong solvent (excess adsorption isotherm), and the analyte (retention behavior or Henry’s constant). − The advantage of direct methods is that they are not biased from any arbitrary decision regarding these properties. Therefore, they require universal conventions for their accurate measurement across all laboratories.…”

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confidence: 99%

Perspective on the Future Approaches to Predict Retention in Liquid Chromatography

Gritti

2021

Anal. Chem.

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The demand for rapid column screening, computer-assisted method development and method transfer, and unambiguous compound identification by LC/MS analyses has pushed analysts to adopt experimental protocols and software for the accurate prediction of the retention time in liquid chromatography (LC). This Perspective discusses the classical approaches used to predict retention times in LC over the last three decades and proposes future requirements to increase their accuracy. First, inverse methods for retention prediction are essentially applied during screening and gradient method optimization: a minimum number of experiments or design of experiments (DoE) is run to train and calibrate a model (either purely statistical or based on the principles and fundamentals of liquid chromatography) by a mere fitting process. They do not require the accurate knowledge of the true column hold-up volume V 0, system dwell volume V dwell (in gradient elution), and the retention behavior (k versus the content of strong solvent φ, temperature T, pH, and ionic strength I) of the analytes. Their relative accuracy is often excellent below a few percent. Statistical methods are expected to be the most attractive to handle very complex retention behavior such as in mixed-mode chromatography (MMC). Fundamentally correct retention models accounting for the simultaneous impact of φ, I, pH, and T in MMC are needed for method development based on chromatography principles. Second, direct methods for retention prediction are ideally suited for accurate method transfer from one column/system configuration to another: these quality by design (QbD) methods are based on the fundamentals and principles of solid–liquid adsorption and gradient chromatography. No model calibration is necessary; however, they require universal conventions for the accurate determination of true retention factors (for 1 < k < 30) as a function of the experimental variables (φ, T, pH, and I) and of the true column/system parameters (V 0, V dwell, dispersion volume, σ, and relaxation volume, τ, of the programmed gradient profile at the column inlet and gradient distortion at the column outlet). Finally, when the molecular structure of the analytes is either known or assumed, retention prediction has essentially been made on the basis of statistical approaches such as the linear solvation energy relationships (LSERs) and the quantitative structure retention relationships (QSRRs): their ability to accurately predict the retention remains limited within 10–30%. They have been combined with molecular similarity approaches (where the retention model is calibrated with compounds having structures similar to that of the targeted analytes) and artificial intelligence algorithms to further improve their accuracy below 10%. In this Perspective, it is proposed to adopt a more rigorous and fundamental approach by considering the very details of the solid–liquid adsorption process: Monte Carlo (MC) or molecular dynamics (MD) simulations are promising tools to explain and interpret ...

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A fundamental study of the impact of pressure on the adsorption mechanism in reversed-phase liquid chromatography

Cited by 13 publications

References 39 publications

Characterization of Drug–Polymer Adsorption Isotherms in Body-on-a-Chip Systems by Inverse Liquid–Solid Chromatography

Characterization of Drug–Polymer Adsorption Isotherms in Body-on-a-Chip Systems by Inverse Liquid–Solid Chromatography

Ultra high performance liquid chromatography method development for separation of omeprazole and related substances on core‐shell columns using a Quality by Design approach

Perspective on the Future Approaches to Predict Retention in Liquid Chromatography

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