Qualification, validation and Analytical Method Transfer

Qualification and validation

The qualification and validation protocol should be determined based on Quality Risk Management (QRM) principles and must be provided by the Supplier (SU) to the Recipient (RU) in a well-documented manner.

All equipment must undergo the following stages of validation:

1. Design Qualification (DQ)
2. Installation Qualification (IQ)
3. Operational Qualification (OQ)
4. Performance Qualification (PQ)

1. Design Qualification (DQ): Design Qualification is the initial phase of equipment or system validation. It involves documenting and verifying that the design of the equipment or system is suitable for its intended purpose and meets all relevant regulatory and quality standards. DQ ensures that the design specifications, requirements, and functionality are well-defined and correctly understood before any physical equipment or system is built or installed.

2. Installation Qualification (IQ): Installation Qualification is the second phase of validation and focuses on ensuring that the equipment or system is properly installed in accordance with the manufacturer's specifications and installation requirements. IQ involves documenting and verifying that the equipment is correctly placed, connected, and configured. It ensures that all components and accessories are in place and functioning as intended.

3. Operational Qualification (OQ): Operational Qualification is the stage where the equipment or system is tested to ensure that it operates consistently and reliably within its specified operating range. OQ involves a series of tests and procedures to verify that the equipment functions correctly under different operational conditions. This phase aims to establish that the equipment or system can consistently produce results that meet predetermined specifications and quality standards.

4. Performance Qualification (PQ): Performance Qualification is the final stage of equipment or system validation. It focuses on demonstrating that the equipment or system can consistently produce results that meet the predetermined acceptance criteria under real operating conditions. PQ involves testing the equipment or system using production materials and processes. It ensures that the equipment or system performs reliably and consistently in its intended environment and that it meets all regulatory and quality requirements.

All processes should undergo validation through the following approaches:

1. Prospective Validation
2. Concurrent Validation
3. Retrospective Validation

1. Prospective Validation: Prospective Validation is a validation approach where the validation process is carried out before a new product, process, or system is put into routine use. It involves establishing documented evidence demonstrating that a process or system consistently produces results that meet predetermined specifications and quality attributes. Prospective validation is typically conducted for new processes or systems or when significant changes are made to existing ones. The validation protocol and criteria are defined in advance, and data is collected during actual production or operation to confirm compliance with established standards.

2. Concurrent Validation: Concurrent Validation is a validation approach that occurs during routine production or operation of a process or system. In this method, the validation activities are conducted in real-time as part of the ongoing manufacturing or operation process. It involves continuously monitoring and collecting data to ensure that the process or system consistently meets predefined quality standards. Concurrent validation is often used for well-established processes or systems where there is a high degree of confidence in their performance. It helps ensure that quality is maintained throughout regular production.

3. Retrospective Validation: Retrospective Validation is a validation approach used for processes or systems that have been in use for some time without formal validation documentation. In this method, historical data and records of the process or system's performance are reviewed and analyzed to determine whether it has consistently met the required quality standards. If the historical data demonstrates that the process or system has consistently produced acceptable results, retrospective validation can be used to establish formal validation documentation after the fact. However, if discrepancies or issues are identified during the retrospective analysis, corrective actions may be required.

Analytical Method Transfer

Analytical Method Transfer is essential for ensuring the accurate analysis of raw materials, finished products, packaging materials, and cleaning samples. This transfer process should include comprehensive information regarding analytical testing. The Supplier (SU) is responsible for providing the following information for analytical method transfer:

• Methods for analyzing and testing raw materials and finished products.
• Equipment details used for testing.
• Training programs for analysts and staff.
• Testing parameters.
• Experimental principles, design, and methodologies.
• Quality control test results.
• Validation reports.

Once the Supplier (SU) provides this information, the Recipient (RU) also has responsibilities for a successful analytical transfer, including:

• Agreement on acceptance criteria.
• Review of analytical methods.
• Training of competent staff.
• Availability of necessary equipment.

Additionally, both the Supplier (SU) and Recipient (RU) must fulfill the following responsibilities and jointly prepare the transfer protocol report:

• Documenting analytical results.
• Executing the transfer protocol.
• Ensuring proper validation to implement the process.

Various analytical parameters must be considered during the transfer, including:

• Precision
• Accuracy
• Limit of detection
• Limit of quantification
• Specificity
• Linearity
• Range

Moreover, access to relevant Pharmacopoeias is essential for comprehensive analytical testing.

The World Health Organization (WHO) has outlined possible experimental designs for analytical testing, encompassing tests for:

• Assay or percentage purity of components.
• Identification tests.
• Content uniformity.
• Solubility.
• Dissolution parameters.
• Qualitative and quantitative microbiological assays.
• Limit tests for impurities.
• Residue recovery.

To ensure the successful execution of the transfer protocol, both the Supplier (SU) and Recipient (RU) must collaborate and jointly prepare the necessary reports.