Liquid chromatography method development and optimization by statistical experimental design and chromatogram simulations

Harang, Valérie; Josefson, Mats

doi:10.1007/bf02492487

Cited by 21 publications

(5 citation statements)

References 23 publications

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“…In another work [80] a liquid chromatography method was optimized based on an experimental design and chromatogram simulations and applying an experimental design. Results from the optimization of an LC method, including the separation of six peaks within 11 min were presented.…”

Section: Computer-assisted Optimization Of Se-parationsmentioning

confidence: 99%

Computer-Assisted Optimization of Liquid Chromatography Separations of Drugs and Related Substances

Bączek

2008

CPA

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Nowadays, liquid chromatography (LC) has an established place among other analytical techniques. This separation technique is commonly used in pharmaceutical laboratories. LC method optimization is usually realized by a trialand-error method based on the knowledge of the chromatographic process. Therefore, LC method development is often time-consuming and involves intensive exploitation of equipment and a substantial consumption of chemicals. Over the last few years, the progress in computer program development has assisted chromatographers in method development also. The rational selection of optimized experimental conditions for the chromatographic separation of analytes can also be realized nowadays by means of specialized algorithms (especially applying those used in the commercially available DryLab and ChromSword software). The aim of the study is to present recent achievements associated with the optimization of chromatographic separations of drugs and related compounds realized in reversed-phase liquid chromatography (RP-LC) systems. Considering applications in pharmaceutical analysis, several examples are provided. Optimization based just on experimental chromatographic measurements and additionally employing the quantitative structure-retention relationships (QSRR) is discussed in view of the opportunity to obtain practically useful separation information.

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Section: Computer-assisted Optimization Of Se-parationsmentioning

confidence: 99%

Computer-Assisted Optimization of Liquid Chromatography Separations of Drugs and Related Substances

Bączek

2008

CPA

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“…The desirability values generally in the range of 0-1. If the value is near to zero means the solution of the method is not strong whereas the value toward 1 means the solution or method is very strong [44]. The obtained desirability value was found to be; D=0.899 which indicated that the method is effective.…”

Section: Optimization Of Hplc Methods By Doementioning

confidence: 93%

“…The polynomial equation in terms of the actual components and factors was shown in Table 2. A positive value represents an effect that favors optimization and negative value shows an inverse relationship between the factor and response [44,47]. Table 2 illustrated that A, C, BC and C 2 were significant (<0.0001) model term for Rt of LAM.…”

Section: Optimization Of Hplc Methods By Doementioning

confidence: 99%

“…In spite of that Development and optimization of isocratic RP-HPLC method is a tedious process that involves instantaneous determination of several factors [37][38][39][40]. Therefore, Design of Experiment (DOE) which includes Box Behnken Design (BBD) [41] in Response Surface methodology (RSM) was used to optimize the developed method [38,44]. It is recognized to provide risk-based understanding of the analytical as well as major factors affecting the performance of analytical method [42,43].…”

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confidence: 99%

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Optimization of RP-HPLC Method for Simultaneous Estimation of Lamivudine and Raltegravir in Binary Mixture by Using Design of Experiment

Singh¹,

Daharwal²

2016

Eurasian J Anal Chem

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A simple, sensitive, cost effective and robust RP-HPLC method for the simultaneous estimation of the Lamivudine (LAM) and Raltegravir (RAL) in laboratory prepared binary mixture was developed, optimized and validated. Separation was achieved on phenomenex C18 column (150 X 4.6 mm id, 5μ particle size) and mobile phase was composed of 75% methanol: 15% Acetonitril: 10 % (0.05mM) phosphate buffer (at pH 3.0), with flow rate 1.2 ml/min at 254nm. Developed method was optimized by using Box Behnken Design (BBD) in response surface methodology (RSM). The independent variables such as the concentration of methanol, pH in mobile phase and flow rate were selected for the optimization and Retention time (Rt) were used as responses for both drugs. Derringer's desirability function was used to concurrently optimize the selected responses. The LOD and LOQ were found to be 1.04 and 3.18 μg/ mL for LAM and 0.36 and 1.08μg/mL of RAL. The percentage recoveries were found to be less than 2% for LAM and RAL. Retention time of LAM and RAL was 3.13±0.07 and 7.27±0.01 minutes respectively. Conclusion: The developed and optimized method was fully validated. The validated method further can be potentially used for estimation of these drugs in combined dosage form.

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“…The experimental design and information data analysis detects the factors that are significant and whether there are any interaction influences between the factors. Experimental statistical design has several uses in chemistry, e.g., in synthesis, separation, optimization of logical approaches (Harang et al, 2001;Rautio et al, 2009;Singireddy et al, 2019).…”

Section: Introductionmentioning

confidence: 99%

Optimization and modeling of reactive conditions for free radical solution polymerization of SA-co-BA copolymer based on the yield using response surface methodology

Elarbe¹,

Elganidi²,

Abdullah³

et al. 2021

Mal. J. Fund. Appl. Sci.

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In the recent years, response surface methodology (RSM) is one of the most common optimization methods employed in the chemical process. The satisfactory model for predicting the maximum yield in solution polymerization has been a challenge due to various conditions during the synthesis process. In this study, interactive impacts of three parameters which are reaction time, concentration of initiator, and reaction temperature on the yield in free radical polymerization of SABA copolymer using toluene as solvent was investigated using experimental design central composite design (CCD) model under response surface methodology (RSM). The result showed the optimization conditions were reaction time of 7 h, initiator concentration of 1 wt %, and reaction temperature of 90 oC with the corresponding yield of 97.31%. The analysis of the regression model (ANOVA) detected an R2 value of 0.9844, that the model is able to clarify 98.44% of the data variation, and just 1.23% of the whole differences is not clarified by the model. Three experimental validation runs were carried out using the optimal replicate conditions and the highest average yield value obtained is 97.15%. There is an error of about 0.97% as compared to the expected value.Therefore, the results indicate that this model is reliable and is able to predict the yield response accurately. it established that the regression model is extremely significant, indicating a strong agreement between the expected and the experimental values of SABA yield.

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Liquid chromatography method development and optimization by statistical experimental design and chromatogram simulations

Cited by 21 publications

References 23 publications

Computer-Assisted Optimization of Liquid Chromatography Separations of Drugs and Related Substances

Computer-Assisted Optimization of Liquid Chromatography Separations of Drugs and Related Substances

Optimization of RP-HPLC Method for Simultaneous Estimation of Lamivudine and Raltegravir in Binary Mixture by Using Design of Experiment

Optimization and modeling of reactive conditions for free radical solution polymerization of SA-co-BA copolymer based on the yield using response surface methodology

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