Method Development and Method Validation

For cosmetic products, the Cosmetics Act stipulates that the ingredients must be declared on the packaging. Many ingredients are allowed to be contained only to defined maximum concentrations, e.g. UV filters or preservatives. For new cosmetic products, it can therefore be necessary to develop and validate suitable analysis methods for quality controls, particularly for the active components.

As a service laboratory, we can draw on an enormous wealth of analytical knowledge and can provide support and contribute to your achieving the desired result quickly with targeted literature researches and feasibility studies.

The validation of analytical methods

Validation of an analytical method provides evidence that the selected method is both suitable for and applicable to the analysis purposes intended. As a result, it will be ensured that analysis results obtained from the method are reliable.

The scope of the validation will be determined together with you in a validation protocol. The experimental work will be carried out by qualified and trained personnel and the results will be summarised in a comprehensive validation report.

Types of analysis

Distinctions are made between the following different types of analysis:

• Identification testing
• Quantitative determination of the level of impurities
• Limit tests for the monitoring of impurities.
• Quantitative determination of the active substance content

The identity of an analyte is confirmed by means of an identification. This is generally performed by comparing a sample with a reference standard using chromatographic or spectroscopic methods.

The test for contamination can be performed either by using a limit test or by quantitative determinations. Different validation parameters are required according to the type of the test.

Content determinations enable the quantitative determination of the analyte in a sample. Chromatographic methods are mainly used and validated in content determinations.

Procedure for validations

The procedure parameters to be determined are dependent on the type of analysis and are described in the ICH guideline Q2(R1). The “Validation of Analytical Methods” table gives an overview of this.

- signifies that this caracteristic is not normally evaluated

+ signifies that this characteristic is normally evaluated

¹ in cases where reproducibility (see glossary) has been performed, intermediate precision is not needed

² lack of specificity of one analytical procedure could be compensated by other supporting analytical procedure(s)

³ may be needed in some cases

In addition to the process parameters given in the table, further validation requirements can also be tested. Particular value is placed on the robustness of a method. Evidence is required to show that small variations, such as in buffer composition, HPLC flow or temperature etc. do not influence the validity of the method.

Stability indicating

As part of a stability study, a method for the determination of contents and degradation products (nowadays typically the HPLC methods) must also be demonstrated to be “stability indicating”. That is done by performing forced degradation studies. Forced degradation is obtained by using severe chemical and physical influences and evidence is gained that the degradation products and the active ingredient in the chromatogram can be separated with the analytical method selected.

Our services in detail:

• Consultation and literature research for method development
• Method development in the laboratory
• Consultation on the scope of the validation and creation of a validation protocol (validation plan)
• Validation of analytical methods
• Additional services are according to the directory of services or upon request.