Validation services for analytical methods in a laboratory

Validating an analytical method is an essential step in demonstrating that the method is suitable for its intended use. It confirms that the method produces reliable and reproducible results that meet scientific and regulatory expectations. Organizations such as the ICH, the FDA, and ISO 17025 define the parameters to be verified: accuracy, precision (repeatability and reproducibility), specificity, limit of detection (LOD), limit of quantification (LOQ), linearity, measurement range, and robustness.

Used for regulatory purposes (itself linked to notions of product quality and safety), it requires a prior framework to establish the parameters to be respected such as: sample preparation, the technique to be used, its parameters, its environment, expected results, acceptable uncertainty, deadlines, etc. These criteria must be the subject of the drafting and signing of a study protocol prior to validation.

When choosing a method validation laboratory, several criteria must be considered. First, it is essential to assess the laboratory's skills and expertise in the specific field of the method to be validated.

You can then refer to the laboratory's credentials, previous experience, and the technical skills of its staff.

Next, it is important to check the laboratory's certifications and accreditations. Accreditations, issued by recognized organizations such as ISO, attest to the laboratory's competence and compliance with quality and reliability standards.

Finally, it is recommended to use a method validation laboratory with state-of-the-art infrastructure and equipment.

By considering these various elements, you will be able to choose a competent and reliable laboratory to perform your method validation. With a team of experts and an analytical park of more than 2000 m², the FILAB laboratory offers you its method validation services and support in research and development.

During laboratory method validation, our experts seek to verify whether the analytical method is appropriate for the analyte or compound being measured, based on various criteria:

• The method is sufficiently sensitive and capable of detecting the lowest levels.
• The method is specific and measures the desired analyte without interference from other compounds present in the sample.
• The method is precise and reproducible, producing consistent results when repeated.
• The method is robust, producing reliable results despite variations in analytical conditions.
• The method used is appropriate in terms of detection and quantification limits, allowing for the accurate detection and measurement of the lowest levels of the analyte.
• The method complies with regulatory requirements and industry standards.
• The method incorporates quality control procedures to ensure the validity of the results obtained.
• The method details the protocols, including acceptance criteria for each parameter evaluated.

These questions help evaluate all relevant aspects of an analytical method to ensure its reliability and suitability for laboratory use.

Analytical methods are the techniques used to identify, quantify or characterize a compound or matrix. They can be classified into broad families: chromatographic methods (HPLC, GC, IC), spectroscopic methods (UV-Vis, IR, NMR, ICP-OES, ICP-MS), electrochemical methods, titrimetric or gravimetric methods, as well as coupled techniques such as LC-MS or GC-MS. Each method is based on a physical or chemical principle and must be validated in the context of its application.

No. Analytical validation criteria depend on both the nature of the method and its objective. For example, an HPLC-type chromatographic method used to quantify an active ingredient in a pharmaceutical formulation will need to meet strict criteria for linearity, accuracy, precision, and limits of quantification to ensure assay precision. Conversely, infrared (IR) spectroscopy used to identify an impurity will place greater emphasis on specificity and robustness, as the primary objective is the qualitative recognition of a compound rather than its precise quantification.

Test method validation involves demonstrating that the test method used in a laboratory produces reliable results that are appropriate for the purpose of the test. This applies in particular to laboratories accredited according to ISO 17025, where each test method must be validated or verified before use. Test method validation involves evaluating the performance of the method as a whole, taking into account the sample, the matrix and the analysis context. It ensures that the results obtained meet the expected quality criteria, both technically and regulatoryly.

Analytical procedure validation focuses on the operational application of a method within a laboratory. An analytical procedure is a detailed protocol that describes all the steps necessary to implement a method: sample preparation, operating conditions, instrumental parameters, data processing, and acceptance criteria. Analytical procedure validation therefore consists of demonstrating that, under the specific conditions defined by the laboratory, the procedure can produce compliant and robust results. It is essential to ensure day-to-day reliability, reduce the risk of error, and guarantee regulatory compliance.

Analytical validation is the generic term that encompasses the entire validation process.

The validation of an analytical method or analytical method focuses on the scientific technique itself (e.g., chromatography, spectroscopy).

Test method validation is often used in accredited laboratories and refers to the validation of tests applied to real samples.

Finally, analytical procedure validation is more operational and concerns the detailed protocol implemented in a given laboratory.

A validated analytical method requires maintenance! It is recommended that any validated method be monitored for its suitability for its intended use throughout its lifecycle. To this end, the implementation of control charts allows for monitoring the reliability of the method in routine use.

Furthermore, in the event of a change, it will be necessary to assess the need for partial or complete revalidation, depending on the case. Among the non-exhaustive list of changes that lead to revalidation of the analytical method, ICH Q2(R1) cites changes in the composition of the finished product, raw materials, or analytical procedures (criteria).