Bioanalytical method validation is one of the essential steps in the lifecycle of a pharmaceutical product. It incorporates generating established documented evidence for providing a high degree of assurance about a specific method. All the ancillary instruments included in the process will consistently oblige to produce intended results. Furthermore, these bioanalytical testing results are efficient enough to aptly reflect the quality characteristic of the product selected for the quality control analysis.
These steps should be validated according to the ICH method validation guidelines, which address the query of validating a particular analytical method. All those methods which fall beyond the categorization of the International Conference on Harmonization (ICH) should be thoroughly validated.
The purpose of using ICH guidelines is to create a harmonized balance between the technical requirements to register a particular pharmaceutical product at three prime geographical markets – Japan, the US, and Europe. Mostly, the typical characteristics applicable to the bioanalytical services method validation are precision, accuracy, detection limit, specificity, quantitation limit, robustness, and linearity range. Also, the analytical method validation process should be inclusive of robust analytical solutions and system suitability.
Performance Characteristics for Bioanalytical Method Validation –
The following characteristics are involved in the process of FDA bioanalytical method validation –
This is a parameter for unequivocally measuring the concentration of the analyte of interest in the presence of other components. This is usually detected with the assistance of identification and purity tests.
Accuracy of a bioanalytical method assesses the relative closeness of agreement between the conventionally actual value and the one that is acknowledged to be a reference value.
The precision of a particular bioanalytical method expresses the closeness of agreement between a measurable series derived through sampling the same homogenous sample multiple times within the set of prescribed conditions.
Detection Limit –
The detection limit for a particular analyte in a given solution helps in the detection of the lowest concentration of the analyte present in the sample under analysis, which is necessarily detected and cannot be quantified to represent its exact value.
Quantitation Limit –
The quantitation limit defines the lowest amount of the analyte of interest that is present in a given sample, which is quantified with a certain level of precision and accuracy.
The linearity is defined as the ability of the analytical procedure to produce test results, which are in direct proportion to the analyte concentration in the given sample.
The analytical procedure range determines the interval between the upper concentration and the lower concentration of the analyte of interest that is present in the given sample for which the analytical procedure demonstrates a certain level of linearity, accuracy, and precision.
Robustness is one of the prime method validation parameters which measures its ability or capacity to remain unaltered or unaffected throughout the process of bioanalytical evaluation. This is one of the deliberate, analytical method parameters for determining the reliability of its usage.
ICH method validation protocol at a glance –
- Define the objectives of the validation
- List responsibilities
- Define the laboratories to be involved and what all roles will be assigned to them
- Categorize methods
- Prepare a list of standards and reagents
- Define evaluation test procedure
- Define the requirement for the final bioanalytical method validation report