Reversed-Phase Liquid Chromatographic Method Development in an Analytical Quality by Design Framework

Reid, George L.; Cheng, Guilong; Fortin, David T.; Harwood, Jeffrey W.; Morgado, João; Wang, Jian; Xue, Gang

doi:10.1080/10826076.2013.765457

Cited by 34 publications

(17 citation statements)

References 15 publications

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“…At a high level, the aim of QbD is to design a quality product that consistently delivers the intended performance. Analogous to process QbD, the aim of AQbD is to design a quality, robust method that consistently delivers the intended performance (Reid et al, 2013). Design of experiments (DoE) is the simple method to optimize the experimental condition with two or more variables (Anderson and Patrick, 2004;Krull et al, 2009;Monks et al, 2011).…”

Section: Captoprilmentioning

confidence: 99%

HPLC-PDA analysis of ACE-inhibitors, hydrochlorothiazide and indapamide utilizing design of experiments

Dawud

Shakya

2019

Arabian Journal of Chemistry

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A simple, rapid, precise, accurate and sensitive high performance liquid chromatographic method has been developed for simultaneous determination of ACE inhibitors with hydrochlorothiazide and indapamide in pharmaceutical formulations. 'Design of Experiments' (DoE) using 'central composite design' (CCD) was applied to facilitate method development and optimization. Mobile phase was optimized utilizing response surface methodology using Design Expert software. Chromatographic separation was achieved on HypersilÒ-Gold C 18 (100 · 4.6 mm, 3 lm, Thermo Fisher Scientific, USA), column at 25°C. The mobile phase was 58% buffer (5 mM KH 2 PO 4 , containing triethylamine 0.25 ml/L), 25% acetonitrile and 17% methanol (pH adjusted to 2.8 ± 0.1). The analysis was performed at 215 nm. The mobile phase flow rate was 1.0 ml/min and injection volume 10 ll. The method was validated for linearity, limits of quantitation and detection, accuracy, precision, ruggedness and robustness as per the International Conference on Harmonization (ICH) guidelines. Calibration curves (for lisinopril, hydrochlorothiazide, captopril, imidapril, perindopril, indapamide and trandolapril) were linear in the concentration range of 5-35 lg/ml. The limit of detection and limit of quantitation for experimental drugs ranged from 0.03 to 0.61 and 0.08-1.84 lg/ml respectively. ª 2014 The Authors. Production and hosting by Elsevier B.V. on behalf of King Saud University. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/3.0/).

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Section: Captoprilmentioning

confidence: 99%

HPLC-PDA analysis of ACE-inhibitors, hydrochlorothiazide and indapamide utilizing design of experiments

Dawud

Shakya

2019

Arabian Journal of Chemistry

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“…Therefore, studying how the change in flow rate affects CQAs is critical. Although the effects of other operational parameters, such as sample concentration, sample injection volume and initial and final organic modifier percentages in mobile phase have been studied by DOE [4]. These factors were not studied in this work because these parameters can be very well controlled by careful sample preparation and the high quality of the modern chromatography instrument systems.…”

Section: Selection Of Doe Factors and Doe Techniquesmentioning

confidence: 99%

“…The same QbD principles have been applied to the HPLC method development [4][5][6]. Using Design of Experiment (DOE) technique, the Method Operable Design Region (MODR) can be established.…”

Section: Introductionmentioning

confidence: 99%

A Quality by Design (QbD) Framework for Reversed-Phase Liquid Chromatography Method Development

Huang¹

2016

IJAT

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A framework for reversed-phase HPLC method development was developed by combining computer simulation, UPLC scouting experiments and surface response design. An interactive computer simulation program was developed for optimizing the gradient elution conditions. This simulation program integrated the kinetics and flow resistance parameters of 18 commonly used columns. Accurate prediction of retention times by this simulation program was demonstrated in this work. This program was used to propose the optimum gradient operational conditions under given constraints, which greatly reduced the time required for method development. The Box-Behnken design was used to evaluate the optimum operational conditions obtained from the simulation and experiments and define the method operable design space. Further insights into the separation mechanisms were obtained from the statistical analysis results of DOE.

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“…The present validated analytical method for estimation of everolimus is based on the quality by design (QbD) approach which is build up for the understanding of intended purposes, predictive solutions and following the design of experiments (DOE) approach [16][17][18][19][20]. The analytical method is validated and developed by the guidelines of the International Conference on Harmonization (ICH) Q8, Q9, Q10 and Q11 [21][22][23][24].…”

Section: Introductionmentioning

confidence: 99%

Development of Simple and Robust RP-HPLC Method for Determination of Everolimus and its Impurities in Oral Solid Dosage Form

2019

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A novel reversed-phase high performance liquid chromatographic (HPLC) technique for the determination of everolimus (Isomer-B) and its impurities in the tablet dosage form has been optimized using analytical quality by design (QbD) approach. All the compounds are monitored with the photodiode array (PDA) detector at 280 nm and the parameters namely; precision, accuracy, specificity, stability, linearity, limit of quantitation (LOQ) and limit of detection (LOD) are evaluated. The quantitation limits of IMP-A, IMP-B, IMP-C, IMP-D, IMP-E, Sirolimus and TGR are found to be 0.08, 0.08, 0.10, 0.10, 0.10, 0.08 and 0.08, respectively. Recovery studies from 0.9 mg/L to 9.0 mg/L are performed for all impurities and the values were obtained between 85-110 %. Injection volume and test concentrations have been optimized to achieve LOQ values under the reporting threshold. The whole technique is developed and validated as per International Council for Harmonization (ICH) guidelines. The proposed method is robust, sensitive, rapid and successful and helpful in the regions where regulatory agencies recommend HPLC analytical method.

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Reversed-Phase Liquid Chromatographic Method Development in an Analytical Quality by Design Framework

Cited by 34 publications

References 15 publications

HPLC-PDA analysis of ACE-inhibitors, hydrochlorothiazide and indapamide utilizing design of experiments

HPLC-PDA analysis of ACE-inhibitors, hydrochlorothiazide and indapamide utilizing design of experiments

A Quality by Design (QbD) Framework for Reversed-Phase Liquid Chromatography Method Development

Development of Simple and Robust RP-HPLC Method for Determination of Everolimus and its Impurities in Oral Solid Dosage Form

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