SOP for Analytical Method Transfer | Analytical Method Transfer Guidelines | Analytical Method Transfer Acceptance Criteria | Analytical Method Transfer Protocol Template |
- Analytical Method Transfer SOP Checklist:
- Responsibilities of originating laboratory for the transfer of analytical methods
- Responsibilities of receiving Laboratory for the transfer of analytical methods
- Preparation of protocol
- Procedure for method transfer
- Experimental design
- Guideline for Acceptance Criteria
- Analytical Method Transfer Protocol Template
1.0 OBJECTIVE :
- To lay down a procedure for successfully transfer the analytical method from analytical development Laboratory or from the other sources (from vendors) to Q.C. (receiving Laboratory) with pre-determine acceptance criteria.
2.0 SCOPE :
- This SOP is applicable for conduction the analytical method transfer of drug substance and drug products. This SOP also deals with discussion of all critical points of analytical method.
3.0 RESPONSIBILITY :
- The Officer-ADL shall be responsible for:
- Performing the analysis as per protocol at both sending unit and at receiving unit.
- The Officer-QC/Chemist-QC shall be responsible for:
- Performing the analysis as per protocol at receiving unit.
- The Executive-ADL shall be responsible for:
- Preparing the protocol and monitoring entire analysis, evaluation of raw data.
- The Section head shall be responsible for:
- Monitoring entire analysis and discussing the critical points of analytical method with ADL and final evaluation of raw data.
- The Manager-ADL will be responsible for:
- Reviewing protocol and report.
- The Manager-QC shall be responsible for:
- Reviewing protocol and report.
- Ensuring compliance of the SOP
- The Manager-QA shall be responsible for:
- Approving protocol and report and for final acceptance of method transfer.
5.0 PROCEDURE :
5.1 Responsibilities of originating laboratory for the transfer of analytical methods:
- Preparation of the protocol.
- Providing the method-specific training for analysts and other quality control staff.
- Assist in the analysis of quality control testing results. Define all critical methods to be transferred for a testing of the given product.
- Define experimental design, sampling methods and acceptance criteria.
- Providing any validation reports for methods under transfer, and demonstrate their robustness.
- Providing details of the equipment used, as necessary (part of validation report, if available) and any standard reference samples.
- Providing approved procedures used in the testing.
- Providing the working standards or reference standards, columns during the initial analysis along with the required chemicals.
- Review and approval of the transfer reports.
5.2 Responsibilities of receiving Laboratory for the transfer of analytical methods:
- Reviewing the analytical method transfer protocol received from ADL.
- Reviewing the analytical methods provided by the Originating laboratory, and formally agrees on acceptance criteria before execution of the transfer protocol.
- Ensure that the necessary equipment for quality control is available and qualified at the receiving Laboratory site. The equipment used by the receiving Laboratory during the analytical method transfer should meet appropriate specifications to ensure the requirements of the method/specification are met.
- Procuring the columns, standards and chemicals as suggested by the ADL.
- Ensure that adequately trained and experienced personnel are in place for analytical testing.
- Generate and approval of the transferred reports.
- Appropriate training should be carried out on transferred methods and all training activities and outcomes should be documented.
5.3 Preparation of protocol:
- Analytical method transfer protocol shall be normally prepared by originating lab and it should be reviewed by the Head of originating lab and head of receiving lab and the Protocol should be approved by Head of QA.
- The analytical methods transfer protocol should describe (but not limited to) objective, scope, responsibilities of the Originating laboratory and the receiving Laboratory. A specification of material and methods and the experimental design and acceptance criteria, documentation including information to be supplied with the results, and report forms to be used if any, deviations, references, signed approval, and details of samples (starting materials, intermediates and finished products).
- In case of availability of customer’s protocol and acceptance criteria, the same method transfer procedure described above will be followed for the respective customer.
5.4 Procedure for method transfer:
- Analytical method transfer shall be perform for the tests of Assay, Related substances, Dissolution, Residual solvents for method precision and system precision.
- Any other tests which need to be performed shall be address in method transfer protocol.
- Prior to the transfer of the analytical method, the method shall be validated by the Originating laboratory.
- Once the method is validated, the Originating laboratory shall send method transfer protocol to receiving Laboratory for approval along with the STP.
- The working standard, impurity standard and test sample required for system suitability test and method transfer experiments shall be ensured before proceeding for transfer activity.
- The method transfer protocol shall be approve by the QC and QA of receiving lab and the dates for the execution of the same shall be communicated to the originating lab prior to transfer of the method to check and to depute the analyst from the originating lab for the activity.
- After the transfer of the analytical method package, receiving Laboratory shall approve the method transfer protocol and start method transfer experiments as per the protocol.
- The analytical performance parameters requirements for individual analytical techniques are as follows:
- System suitability
- System precision
- Method precision etc.
- In case of any deficiencies in the method of analysis, the Originating laboratory shall inform the same to receiving Laboratory. The receiving Laboratory shall review the completed analytical method transfer results and inform accordingly to the Originating laboratory.
5.5 If the acceptance criteria are not met then the same shall be recorded as a deviation in the protocol and further activity for continuing method transfer shall be as per the recommendations given by the originator laboratory:
- If the results do not meet the acceptance criteria, the method is not qualified for transfer.
- The receiving Laboratory shall keep records of the method transfer protocol, record of test results and chromatograms of all experiments.
5.6 Experimental design:
- Testing and Acceptance Criteria:
- Testing and acceptance criteria should be based upon the intended use of the method, in conjunction with the data obtained during method validation and any historical data generated by the transferring laboratory.
- There are two equally valid means by which acceptable method transfer may be demonstrated:
- A comparison of data generated by the receiving laboratory against the reference data generated by the transferring laboratory, or
- By assuming equivalence of the two laboratories, then demonstrating that this assumption is valid.
- Alternative procedures and acceptance criteria may be applied based on characteristics of the analytical method.
5.7 Guideline for Acceptance Criteria:
- The following acceptance criteria are provided as a guide and may be varied on a case by case basis provided that any deviation is justified and documented.
- Main Component Assay / Preservative Assay (HPLC, GC, Spectrophotometry, etc.), Bulk Assays
- All system suitability requirements should be met.
- For Assay
- For drug product Assay, the RSD for each analyst is not greater than 2% when six replicates are performed.
- The Batch analysis for assay between the two laboratories should not exceed 2% RSD.
- For drug substance, the individual results from each laboratory should agree within ± 2% of the overall mean of the two laboratories.”
- For immediate release products:
- The mean drug release for each analyst in the receiving Laboratory is within ±5% of the Originating laboratory value.
- The comparison of RSD for the 12 individual test results should be defined on a product basis using an evaluation of existing data.
- If the specification requires the generation of dissolution profile it should be consistent with that generated in the Originating laboratory.
- The acceptance criteria of ±5% are considered acceptable based on the variability inherent in the test and was the acceptance criteria defined in both legacy companies.
- For modified release products:
- The dissolution profiles are similar and the F2 (similarity factor) is between 50 and 100.
- The mean difference between profiles at any time point does not exceed 15% released.
- For immediate release products:
5.8 For all the other tests the acceptance criteria shall be defined and agreed by both the labs based on the nature of the methodology while approving the protocol.
5.9 Guidelines like WHO, ICH, and any prevalent guidelines / regulations shall be followed for defining the acceptance criteria.
- The numbering system for the protocol shall be as follows PRO/MT/XXXX/YYY
5.10 The numbering system for the protocol shall be as follows PRO/MT/XXXX/YYY:
- The first three characters defined as protocol
- The fourth character is slash
- The fifth and sixth character is method transfer
- The seventh character is slash
- 8th to 11th characters are the first 4 letters of the product.
- 12th character is slash
- 13th to 15th characters are the serial number of the method transfer.
|Standard Operating Procedure
|Analytical Development Laboratory
|High Performance Liquid Chromatography
|Protocol for Analytical Method Transfer
8.0 SOP REFERENCES
END OF THE SOP
Annex. No. 01 Protocol for Analytical Method Transfer