Method ruggedness studies incorporating a risk based approach: A tutorial

Borman, Phil J.; Chatfield, Marion J.; Damjanov, Ivana; Jackson, Patrick

doi:10.1016/j.aca.2011.07.008

Cited by 38 publications

(17 citation statements)

References 19 publications

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“…The precision is related to the ruggedness of the method [48] and is obtained with repeatability and inter-day intermediate precision [49], both calculated through relative standard deviation (RSD). The highest value for repeatability and intermediate precision were 0.80% and 1.09% lower than 1.8% defined in the ATP (Table 4).…”

Section: Validation Criteriamentioning

confidence: 99%

Development and Validation of an in-line API Quantification Method Using AQbD Principles Based on UV-Vis Spectroscopy to Monitor and Optimise Continuous Hot Melt Extrusion Process

et al. 2020

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A key principle of developing a new medicine is that quality should be built in, with a thorough understanding of the product and the manufacturing process supported by appropriate process controls. Quality by design principles that have been established for the development of drug products/substances can equally be applied to the development of analytical procedures. This paper presents the development and validation of a quantitative method to predict the concentration of piroxicam in Kollidon® VA 64 during hot melt extrusion using analytical quality by design principles. An analytical target profile was established for the piroxicam content and a novel in-line analytical procedure was developed using predictive models based on UV-Vis absorbance spectra collected during hot melt extrusion. Risks that impact the ability of the analytical procedure to measure piroxicam consistently were assessed using failure mode and effect analysis. The critical analytical attributes measured were colour (L* lightness, b* yellow to blue colour parameters—in-process critical quality attributes) that are linked to the ability to measure the API content and transmittance. The method validation was based on the accuracy profile strategy and ICH Q2(R1) validation criteria. The accuracy profile obtained with two validation sets showed that the 95% β-expectation tolerance limits for all piroxicam concentration levels analysed were within the combined trueness and precision acceptance limits set at ±5%. The method robustness was tested by evaluating the effects of screw speed (150–250 rpm) and feed rate (5–9 g/min) on piroxicam content around 15% w/w. In-line UV-Vis spectroscopy was shown to be a robust and practical PAT tool for monitoring the piroxicam content, a critical quality attribute in a pharmaceutical HME process.

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Section: Validation Criteriamentioning

confidence: 99%

Development and Validation of an in-line API Quantification Method Using AQbD Principles Based on UV-Vis Spectroscopy to Monitor and Optimise Continuous Hot Melt Extrusion Process

et al. 2020

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“…Quantified guarantees of achieving good levels of total error definitely represent a movement towards the next steps of the analytical method lifecycle, i.e. robust assessments and routines that can be used in the laboratory [27].…”

Section: Part I: Pre-validation Study During the Qbd Optimization Stepmentioning

confidence: 99%

“…The ME refers to the ionization suppression or enhancement caused by unobserved substances coeluted from biological matrix. This kind of co-elution competition takes place between compounds during the ionization process, and especially when considering ESI mode [25][26][27].…”

Section: Matrix Effect Assessmentmentioning

confidence: 99%

“…Therefore, a more specific methodology was envisaged in order to assess this problematic. In the case of HILIC method, ME is largely encountered due to a coelution between early-eluted analytes and endogenous phospholipids or formulation vehicles [27]. Thanks this methodology, the separative DS could manage the ME throughout the envisaged experimental domain as requested by FDA recommendations.…”

Section: Matrix Effect Assessmentmentioning

confidence: 99%

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Towards a full integration of optimization and validation phases: An analytical-quality-by-design approach

Hubert

Houari

Rozet

et al. 2015

Journal of Chromatography A

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20When using an analytical method, defining an Analytical Target Profile (ATP) focused on 21 quantitative performance represents a key input, and this will drive the method development 22 process. In this context, two case studies were selected in order to demonstrate the potential of 23 a Quality-by-Design (QbD) strategy when applied to two specific phases of the method 24 lifecycle: the pre-validation study and the validation step. The first case study focused on the 25 improvement of a Liquid Chromatography (LC) coupled to Mass Spectrometry (MS) 26 stability-indicating method by the means of the QbD concept. The Design of Experiments 27 (DoE) conducted during the optimization step (i.e. determination of the qualitative Design 28 Space (DS)) was performed a posteriori. Additional experiments were performed in order to 29 simultaneously conduct the pre-validation study to assist in defining the DoE to be conducted 30 during the formal validation step. This predicted protocol was compared to the one used 31 during the formal validation. A second case study based on the LC/MS-MS determination of 32 glucosamine and galactosamine in human plasma was considered in order to illustrate an 33 innovative strategy allowing the QbD methodology to be incorporated during the validation 34phase. An operational space, defined by the qualitative DS, was considered during the 35 validation process rather than a specific set of working conditions as conventionally 36 performed. Results of all the validation parameters conventionally studied were compared to 37 those obtained with this innovative approach for glucosamine and galactosamine. Using this 38 strategy, qualitative and quantitative information were obtained. Consequently, an analyst 39 using this approach would be able to select with great confidence several working conditions 40 within the operational space rather than a given condition for the routine use of the method. 41This innovative strategy combines both a learning process and a thorough assessment of the 42 risk involved. 43 3

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“…[9][10][11][12][13][14][15][16][17] In the AQbD approach, the relationships between the analytical parameters and the quality of the analytical methods are systematically investigated using risk assessment and the design of experiments (DoE) methodologies, and are then quantitatively represented in the form of mathematical models using multivariate statistical modeling methods. The AQbD approach is introduced in this work to acquire retention rules, i.e., to construct models relating the analytical parameters to the chromatographic parameters.…”

mentioning

confidence: 99%

Rapid HPLC Analytical Method Development for Herbal Medicine Formulae Based on Retention Rules Acquired from the Constituting Herbs

et al. 2018

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Herbal medicines (HMs), which offer a plethora of treatment options for complex diseases, have become increasingly popular worldwide in recent years. HM formulae, which are the combinations of two or more types of herbs, and therefore contain chemical compounds from each of the individual herbs, are the main form of HMs used in clinic. In this work, this type of sample matrix is regarded as a compound matrix, which is a mixture of their constituting ingredients. Similarly, a dietary supplement can also be regarded as a compound matrix if it is composed of multiple nutrients and/or extracts from several types of foods/plants. HPLC is the most commonly used method to analyze compound matrices in various fields. [1][2][3][4][5][6][7][8] However, due to the complexity of the matrices, chromatographic separation for these samples is challenging. Comprehensive pre-experiments to optimize the analytical parameters (e.g., gradient and pH of the mobile phase) are often needed to achieve good separation performance, which makes HPLC method development complicated and time-consuming. In the commonly used approach, the analytical parameters are optimized one by one in a process that is dependent on the experience of the researchers.Although many HPLC experiments are conducted and large amounts of raw data are acquired during method development, the rules of how the analytical parameters impact chromatographic separation are not effectively summarized and recorded. Consequently, when the composition of the compound matrix changes, a new analytical method must be developed from the very beginning if the performance of the original method becomes undesirable.An efficient approach to develop HPLC methods for compound matrices is needed.Since a compound matrix is the combination of its constituting ingredients, and HPLC methods for the individual ingredients have usually been developed before method development for the compound matrix, a question is raised: Are there any mutual retention rules between the compound matrix and its ingredients? If the answer is yes, then based on the retention rules acquired from the constituting ingredients, the impacts of the analytical parameters on the chromatographic separation of the compound matrix are predictable, which will enable rapid optimization of the analytical parameters for the compound matrix. When analyzing compound matrices and their constituting ingredients with the same HPLC analytical parameters, the same chemical compounds in these different samples have the same chromatographic parameters like retention time (tR) and peak width. Therefore, the relationships between the analytical parameters and these chromatographic parameters can be defined as the mutual retention rules between the compound matrices and their constituting ingredients. By effectively acquiring and utilizing the retention rules, the HPLC method development efficiency can be increased.In recent years, the analytical quality by design (AQbD) approach was proposed and has been successfully applied in the develo...

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Method ruggedness studies incorporating a risk based approach: A tutorial

Cited by 38 publications

References 19 publications

Development and Validation of an in-line API Quantification Method Using AQbD Principles Based on UV-Vis Spectroscopy to Monitor and Optimise Continuous Hot Melt Extrusion Process

Development and Validation of an in-line API Quantification Method Using AQbD Principles Based on UV-Vis Spectroscopy to Monitor and Optimise Continuous Hot Melt Extrusion Process

Towards a full integration of optimization and validation phases: An analytical-quality-by-design approach

Rapid HPLC Analytical Method Development for Herbal Medicine Formulae Based on Retention Rules Acquired from the Constituting Herbs

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