Critical Review of Near-Infrared Spectroscopic Methods Validations in Pharmaceutical Applications

in Journal of Pharmaceutical & Biomedical Analysis (2012), 69

Based on the large number of publications reported over the past five years, near-infrared spectroscopy (NIRS) is more and more considered an attractive and promising analytical tool regarding Process ... [more ▼]

Based on the large number of publications reported over the past five years, near-infrared spectroscopy (NIRS) is more and more considered an attractive and promising analytical tool regarding Process Analytical Technology and Green Chemistry. From the reviewed literature, few of these publications present a thoroughly validated NIRS method even if some guidelines have been published by different groups and regulatory authorities. However, as any analytical method, the validation of NIRS method is a mandatory step at the end of the development in order to give enough guarantees that each of the future results during routine use will be close enough to the true value. Besides the introduction of PAT concepts in the revised document of the European Pharmacopoeia (2.2.40) dealing with near-infrared spectroscopy recently published in Pharmeuropa, it agrees very well with this mandatory step. Indeed, the latter suggests to use similar analytical performance characteristics than those required for any analytical procedure based on acceptance criteria consistent with the intended use of the method. In this context, this review gives a comprehensive and critical overview of the methodologies applied to assess the validity of quantitative NIRS methods used in pharmaceutical applications. [less ▲]

Quality by design compliant analytical method validation

in Analytical Chemistry (2012), 84

The concept of quality by design (QbD) has recently been adopted for the development of pharmaceutical processes to ensure a predefined product quality. Focus on applying the QbD concept to analytical ... [more ▼]

The concept of quality by design (QbD) has recently been adopted for the development of pharmaceutical processes to ensure a predefined product quality. Focus on applying the QbD concept to analytical methods has increased as it is fully integrated within pharmaceutical processes and especially in the process control strategy. In addition, there is the need to switch from the traditional checklist implementation of method validation requirements to a method validation approach that should provide a high level of assurance of method reliability in order to adequately measure the Critical Quality Attributes (CQAs) of the drug product. The intended purpose of analytical methods is directly related to the final decision that will be made with the results generated by these methods under study. The final aim for quantitative impurity assays is to correctly declare a substance or a product as compliant with respect to the corresponding product specifications. For content assays, the aim is similar: making the correct decision about product compliance with respect to their specification limits. It is for these reasons that the fitness of these methods should be defined, as they are key elements of the Analytical Target Profile (ATP). Therefore, validation criteria, corresponding acceptance limits and method validation decision approaches should be settled in accordance with the final use of these analytical procedures. This work proposes a general methodology to achieve this in order to align method validation within the QbD framework and philosophy. β-expectation tolerance intervals are implemented to decide about the validity of analytical methods. The proposed methodology is also applied to the validation of analytical procedures dedicated to the quantification of impurities or active product ingredients (API) in drug substances or drug products and its applicability is illustrated with two case studies. [less ▲]

Silicone-based drug reservoirs manufacturing process - Critical quality attributes evaluation using NIR and Raman spectroscopy

Poster (2011, October)

A BAYESIAN PREDICTIVE PROBABILITY CRITERION TO ASSESS ANALYTICAL METHODS VALIDITY

Poster (2011, September)

LCA-GE-005- Rapport de validation - VR001_V01

Report (2011)

Protocole d'essai LC/MS - P001 - V01

Report (2011)

Qualitative analysis of potentials compounds contained in an aged matrix of a pharmaceutical speciality at the RT of an impurity

Report (2011)

Espectroscopia aplicada

Scientific conference (2011, May)

Développement d'une méthodologie statistique basée sur l'intervalle de tolérance pour la sélection et l'évaluation de modèles robustes dans le domaine de la spectroscopie et de l'imagerie proche infrarouge

Report (2011)

Le fléau des faux médicaments

E-print/Working paper (2011)

The traffic in counterfeit medicines is booming. It misleads, and it kills. A University of Liège team is making Rwandan and Congolese health care workers aware of the problem, whilst informing and ... [more ▼]

The traffic in counterfeit medicines is booming. It misleads, and it kills. A University of Liège team is making Rwandan and Congolese health care workers aware of the problem, whilst informing and training them, so that they may detect and monitor these products, thanks to made to measure appropriate technical systems. [less ▲]