Theoretical Interpretation of High-Performance Chromatographic Data for a Heterogeneous Series of Compounds

1992 ◽  
Vol 57 (1) ◽  
pp. 33-45
Author(s):  
Vladimír Jakuš
Keyword(s):  
Experimental Data ◽  
High Performance ◽  
Theoretical Interpretation ◽  
Retention Data ◽  
Theoretical Evaluation ◽  
New Approach ◽  
Free Energy Of Solvation ◽  
Rp Hplc ◽  
Mobile Phases ◽  
Reversed Phases

A new approach to theoretical evaluation of the Gibbs free energy of solvation was applied for estimation of retention data in high-performance liquid chromatography on reversed phases (RP-HPLC). Simple and improved models of stationary and mobile phases in RP-HPLC were employed. Statistically significant correlations between the calculated and experimental data were obtained for a heterogeneous series of twelve compounds.

Theoretical interpretation of retention data of polychlorinated biphenyls in liquid chromatography

1991 ◽  
Vol 56 (12) ◽  
pp. 2833-2848
Author(s):  
Vladimír Jakuš ◽  
Stanislav Miertuš
Keyword(s):  
Polychlorinated Biphenyls ◽  
Biologically Active ◽  
Dominant Factor ◽  
Theoretical Interpretation ◽  
Retention Data ◽  
Theoretical Evaluation ◽  
Retention Model ◽  
New Approach ◽  
Rp Hplc ◽  
Mobile Phases

The new approach to the theoretical evaluation of Gibbs free energy of solvation is applied to the estimation of retention data in RP-HPLC. Simple models of stationary and mobile phases in RP-HPLC are used. The correlation between retention data of a series of 15 polychlorinated biphenyls (measured on chemically bonded stationary phase with C18 alkyl chains) and the contribution of the Gibbs solvation energy is investigated in order to determine the dominant factor controlling retention. The retention in RP-HPLC can be predicted on the basis of our thermodynamic retention model. This approach is suitable especially when no standards are available for some derivatives (e.g. metabolites of biologically active substances) and when the interpretation of experimental elution is not clear.

scholarly journals Retention Modelling of Phenoxy Acid Herbicides in Reversed-Phase HPLC under Gradient Elution

Molecules ◽  
2020 ◽  
Vol 25 (6) ◽  
pp. 1262 ◽  
Author(s):  
Alessandra Biancolillo ◽  
Maria Anna Maggi ◽  
Sebastian Bassi ◽  
Federico Marini ◽  
Angelo Antonio D’Archivio
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Retention Factor ◽  
Reversed Phase ◽  
Model Complexity ◽  
Retention Data ◽  
Rp Hplc ◽  
Phenoxy Acid Herbicides ◽  
Acid Herbicides ◽  
Phenoxy Acids

Phenoxy acid herbicides are used worldwide and are potential contaminants of drinking water. Reversed phase high-performance liquid chromatography (RP-HPLC) is commonly used to monitor phenoxy acid herbicides in water samples. RP-HPLC retention of phenoxy acids is affected by both mobile phase composition and pH, but the synergic effect of these two factors, which is also dependent on the structure and pKa of solutes, cannot be easily predicted. In this paper, to support the setup of RP-HPLC analysis of phenoxy acids under application of linear mobile phase gradients we modelled the simultaneous effect of the molecular structure and the elution conditions (pH, initial acetonitrile content in the eluent and gradient slope) on the retention of the solutes. In particular, the chromatographic conditions and the molecular descriptors collected on the analyzed compounds were used to estimate the retention factor k by Partial Least Squares (PLS) regression. Eventually, a variable selection approach, Genetic Algorithms, was used to reduce the model complexity and allow an easier interpretation. The PLS model calibrated on the retention data of 15 solutes and successively tested on three external analytes provided satisfying and reliable results.

scholarly journals A new RP-HPLC method as an auxiliary tool for optimization of sample preparation procedures for tracing of PPCPs of different hydrophilicities

2021 ◽  
Vol 71 (2) ◽  
pp. 305-315
Author(s):  
Omar J. Portillo-Castillo ◽  
Rocío Castro-Ríos ◽  
Abelardo Chávez-Montes ◽  
Azucena González-Horta ◽  
Norma Cavazos-Rocha ◽  
...  
Keyword(s):  
Sample Preparation ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Suitable Alternative ◽  
Analytical Technique ◽  
Rp Hplc ◽  
Mobile Phases ◽  
Wide Range ◽  
Gradient Mode

AbstractRecently, pharmaceutical and personal care products (PPCPs) have received considerable attention because of their increasing use. Analysis of PPCPs presents a significant analytical challenge, with high-performance liquid chromatography (HPLC) in reversed-phase mode, as the most widely used analytical technique. To facilitate the optimization of the procedures that are applied in the early stages of sample preparation, a simple and fast HPLC method is proposed in this work for the separation of some PPCPs with a wide range of hydrophilicity. Two columns were evaluated (Atlantis dC18 and Discovery HS F5); as for mobile phases: a formate buffer (40 mmol L−1, pH 4) and methanol were tested in a gradient mode. The fluorinated column allowed better separation in a shorter time and better resolution for all analytes (Rs > 1). The proposed method delivered good performance for the tracing of PPCPs and is a suitable alternative to traditional C18-based HPLC methods.

scholarly journals Highly accurate and New approach for quantiϐication of Gramicidin in medication by RP-HPLC

2020 ◽  
Vol 11 (SPL4) ◽  
pp. 3053-3058
Author(s):  
Naveen V M K ◽  
Veeraswami B
Keyword(s):  
Present Method ◽  
High Performance ◽  
Dosage Forms ◽  
Specific Flow Rate ◽  
Reverse Phase ◽  
Allowable Limit ◽  
Specific Flow ◽  
New Approach ◽  
Rp Hplc ◽  
Medication Dosage

A significant Reverse Phase-High performance Liquid Chromatography technique was developed for a more accurate, unique and quick economical method was developed for the analysis of Gramicidin in medication dosage forms. The separation of this drug Gramicidin was done by using the X-Bridge phenyl column as a stationary phase, and a mixture of acetonitrile + buffer in 50:50 v/v ratio was used as a movable phase. The buffer used in this method was Octane sulphonic acid of pH-2.5 adjusted with OPA. The maximum absorbance of eluents was observed at 235 nm. A specific flow rate (1 ml/minute) was maintained throughout the runtime of 8 min. The selected drug is eluted at 2.49 minutes. The selected drug obeys Beer Lambert's law in the concentration range of 0.5-7.5 µg/ml of Gramicidin. The percentage of recovery was found to be within the acceptable limit. The selected approach was corroborated with ICH standard ground rules, and the results of parameters like method precision, accuracy, ruggedness, robustness, and degradation studies were found to be within the allowable limit. Thus, the present method was successfully applied for the simultaneous analysis of Gramicidin in routine industrial work.

scholarly journals Lipophilicity assessment of some 5,5-disubstituted hydantoins by the means of reversed phase liquid chromatography

2013 ◽  
Vol 19 (1) ◽  
pp. 1-6
Author(s):  
Vesna Despotovic ◽  
Nemanja Trisovic ◽  
Anamarija Mandic ◽  
Gordana Uscumlic ◽  
Tatjana Djakovic-Sekulic
Keyword(s):  
Liquid Chromatography ◽  
High Performance ◽  
Principal Component ◽  
Reversed Phase ◽  
Retention Data ◽  
Reversed Phase Liquid Chromatography ◽  
Mobile Phases ◽  
Statistical Level ◽  
Phase Liquid ◽  
Layer Chromatography

The retention of some 5,5-disubstituted hydantoins was investigated by reversed phase high performance thin-layer chromatography (RP HPTLC) and reversed phase high-pressure liquid chromatography (RP HPLC). The mobile phases were mixtures of methanol-water and acetonitrile-water in various volume fractions. In order to explore and visualize similarities and differences among the investigated compounds and chromatographic system Principal Component Analysis (PCA) was used. Results show that the experimental lipophilicity indices estimated from retention data (RM,W, logkw) and PC1 are directly correlated with logP values at a high significant statistical level.

scholarly journals Development and Validation of Stability-Indicating RP-HPLC Method for the Estimation of Lenalidomide and its Impurities in Oral Solid Dosage Form

2019 ◽  
Vol 35 (1) ◽  
pp. 140-149 ◽  
Author(s):  
Somana Siva Prasad ◽  
G. V. Krishna Mohan ◽  
A. Naga Babu
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Stability Robustness ◽  
Rp Hplc ◽  
Mobile Phases ◽  
Limit Of Quantitation ◽  
Successful Separation ◽  
Quality By Design Approach

In this study, a novel, simple and precise RP-HPLC method has been developed for the quantitative analysis of Lenalidomide (LLM) in pharmaceutical formulations using analytical quality by design approach. An X-bridge-C18 column (150 mm × 4.6 mm × 3.5 µ) with mobile phases containing a Potassium dihydrogen orthophosphate anhydrous buffer and methanol in the ratio of (90:10 v/v) and (35:65 v/v) are used for the estimation of LLM and its degradation products. The flow rate of 0.8 mL/min is maintained and all degradation studies are performed at 210 nm using photodiode array (PDA) detector. Method Validation is carried out according to International Council for Harmonisation (ICH) guidelines and the parameters namely; precision, accuracy, specificity, stability, robustness, linearity, limit of quantitation (LOQ) and limit of detection (LOD) are evaluated. The present developed RP-HPLC method shows the purity angle of peaks is less than their threshold angle, signifying that it to be suitable for stability studies. Hence, the developed method can be used for the successful separation of LLM and its impurities in the pharmaceutical dosage formulations.

scholarly journals Development and validation of RP-HPLC method for estimation of brexpiprazole in its bulk and tablet dosage form using Quality by Design approach

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Amol S. Jagdale ◽  
Nilesh S. Pendbhaje ◽  
Rupali V. Nirmal ◽  
Poonam M. Bachhav ◽  
Dayandeo B. Sumbre
Keyword(s):  
Flow Rate ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Control Analysis ◽  
Uv Detector ◽  
Mobile Phase Flow Rate ◽  
Rp Hplc ◽  
Quality By Design Approach ◽  
Bulk Drug

Abstract Background A new, sensitive, suitable, clear, accurate, and robust reversed-phase high-performance liquid chromatography (RP-HPLC) method for the determination of brexpiprazole in bulk drug and tablet formulation was developed and validated in this research. Surface methodology was used to optimize the data, with a three-level Box-Behnken design. Methanol concentration in the mobile phase, flow rate, and pH were chosen as the three variables. The separation was performed using an HPLC method with a UV detector and Openlab EZchrom program, as well as a Water spherisorb C18 column (100 mm × 4.6; 5m). Acetonitrile was pumped at a flow rate of 1.0 mL/min with a 10 mM phosphate buffer balanced to a pH of 2.50.05 by diluted OPA (65:35% v/v) and detected at 216 nm. Result The developed RP-HPLC method yielded a suitable retention time for brexpiprazole of 4.22 min, which was optimized using the Design Expert-12 software. The linearity of the established method was verified with a correlation coefficient (r2) of 0.999 over the concentration range of 5.05–75.75 g/mL. For API and formulation, the percent assay was 99.46% and 100.91%, respectively. The percentage RSD for the method’s precision was found to be less than 2.0%. The percentage recoveries were discovered to be between 99.38 and 101.07%. 0.64 μg/mL and 1.95 μg/mL were found to be the LOD and LOQ, respectively. Conclusion The developed and validated RP-HPLC system takes less time and can be used in the industry for routine quality control/analysis of bulk drug and marketed brexpiprazole products. Graphical abstract

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