To delineate analytical method transfer of developed validated analytical methods for qualifying a laboratory (Receiving unit- Quality control laboratory/another laboratory) to use an analytical procedure that originates in another laboratory (Transferring unit-R&D-Analytical).
This SOP is applicable to all the method transfers made by Transferring Unit (R&D – Analytical) to Receiving unit (QC/other laboratory).
All intended users.
Head, Research and Development – Analytical.
- This SOP Presents the components necessary to complete a successful method transfer by using various types of method transfer.
- Analytical tests:Analytical methods like but not limited to Assay, Related Substances, Dissolution / Drug Release, Residual Solvents etc, for which Analytical Method Validations have been carried out at Transferring unit (R&D – Analytical), shall be included in Method Transfer program.
- Head, QA/QC and Head, R&D- Analytical shall have the rationale for any methods not included (transfer waiver). Additional pharmacopeial tests like identification, moisture content/LOD, pH and optical rotation/specific optical rotation and any other test as applicable in individual monograph/specification shall be considered during the method transfer.
- Method transfer for analytical methods for raw materials shall be carried out based on criticality of the method, as agreed by Head, QA/QC Head R&D – Analytical.
- Types of method transfers:
- Comparative testing:
- Indirect transfer/collaborative:
In this type of method transfer, Transferring unit, Scientist (R&D – Analytical) and Receiving unit Chemist/analyst, (QC/other laboratory) shall analyze same batch of sample at their respective locations and the results obtained shall be compared. Transferring unit (R&D – Analytical) shall provide the Receiving unit (QC/other laboratory) with the best procedures, method validation reports, stepwise direction for critical parameters, and certificate of one sample previously analyzed at transferring unit (R&D – Analytical). The Chemist/analyst, receiving unit (QC/other laboratory) shall perform the analysis in triplicate and provide the results to transferring unit (R&D-Analytical).
- Direct transfer:
This type of method transfer shall include the physical demonstration and joint analysis of sample by Transferring unit, Scientist (R&D – Analytical) and the Receiving unit Chemist/analyst, (QC/other laboratory). Scientist, transferring unit (R&D – Analytical) visits the receiving unit (QC/other laboratory) and demonstrates the method by analyzing the sample as per the protocol. After demonstration by the Scientist (R&D – Analytical), the Chemist/analyst, (QC/other laboratory) shall perform the analysis independently.
- Co-Validation Between Two Laboratories or sites
In this type of method transfer the transferring unit shall include receiving unit in inter laboratory co–validation including them as a part of the validation team at the transferring unit or receiving unit and thereby obtaining data for the assessment of reproducibility. The assessment is made using preapproved transfer or validation protocol providing the details of procedure, the samples to be used, and the predetermined acceptance criteria.
- Complete or Partial Method Validation or Revalidation
Revalidation or partial revalidation is another acceptable type of method transfer wherein those characteristics which are anticipated to be affected by transfer are addressed. Following are the characteristics addressed in Revalidation or partial validation:
- Submission to the regulatory agencies of a revised analytical procedure.
- Use of an established general procedure with a new product or raw material.
- Changes in composition of drug product.
- Changes in analytical procedures.
- Omission of Formal Transfer, Transfer Wavier
In this type of method transfer under certain circumstances, the receiving unit is considered to be qualified to use the analytical test procedures without comparison and generation of inter laboratory comparative data. Following are circumstances that may justify transfer wavier:
- The new product composition is comparable to that of an existing product and /or the concentration of active ingredient is similar to that of an existing product and is analyzed by procedures with which the receiving unit already has experience.
- The analytical procedure being transferred is described in the Pharmacopoeia, and is unchanged. Verification should be applied in this case.
- The analytical procedure transferred is the same as or very similar to a procedure already in use.
- The personnel in charge of the development, validation or routine analysis of the product at the transferring unit are moved to the receiving unit.
Note: If eligible for transfer waiver, the receiving unit should document it with appropriate justification.
- Analytical parameters like precision by
both R&D and QC experiment shall be carried out during the analytical
method transfer. For assay analysis, one set of linearity (from 80% to 120%)
and specificity experiment (Placebo interference) shall be carried out by the
QC chemist/analyst in specified range as per the protocol. Head QA/QC and Head
R&D analytical mutually decide on additional parameter based on the
complexity of the method. In case of Related Substance test, the available
impurities shall be spiked to show the specificity.
- R&D – Analytical in consultation with R&D – Pharma shall initiate the process by informing QC laboratory at the manufacturing location well in advance of the proposed exhibit batch/production batch.
- Before carrying out the method transfer, Head, QA/QC and Head, R&D – Analytical shall set in place an approved protocol. The protocol shall either be prepared on the basis of type of transfer as mutually decided by Head, R&D – Analytical and Head, QA/QC.
- R&D – Analytical shall inform/provide plant, a list of special chemicals, reagents, working standards, GC/HPLC columns required to QC laboratory.
- Protocol shall be initiated by the scientist, R&D – Analytical.
- Preparation of protocol:
- Protocol shall be specific to the product and method. Protocol shall contain the Objective, Scope, Responsibility of transferring and receiving unit, product name, method reference, transferring location name, transfer type, working standard and other chemicals details, column details, sample batch no. and precautions to be taken during the analysis/handling.
- For regulated market, the protocol for analytical method transfer (AMT) shall be numbered as AMT/YY/DNNN/RR, where AMT refers to Analytical Method Transfer for regulated market; this is common for all AMT protocols, YY refers for the year, DNNN refers to (D stands for- Dosage Form, NNN stands for– Product Serial Number), RR refers to the revision number. For AMT prepared first time RR is 00, on revision it increase in ascending order.
- For domestic market, the protocol for Analytical Method Transfer (AMT) shall be numbered as DMT/YY/DNNN/RR, where DMT refers to Analytical Method Transfer for domestic market; this is common for all DMT protocols, YY refers for the year, DNNN refers to (D stands for- Dosage Form, NNN stands for– Product Serial Number), RR refers to the revision number. For DMT prepared first time RR is 00, on revision it increase in ascending order.
- Protocol shall be prepared by the scientist or designee, R&D – Analytical and independently reviewed by another scientist or designee. The same shall be approved by Head, R&D – Analytical or designee and forwarded it for the approval of Head, QA/QC or designee.
- After approval of the protocol the method transfer activity shall be initiated.
- Training during method transfer: Scientist or designee, R&D – Analytical shall provide necessary trainings to the Chemist/analyst, QC to make him understand the method complexity and provide him for the practical tips necessary for the analysis by the method. This shall be documented.
- During the method transfer all the details
of analysis shall be written in the laboratory note book issued at R&D.
Details of instrument usage shall be written in the instrument logbook of
- The results of chemist/analyst-QC shall be reviewed by the scientist or designee, R&D – Analytical for accuracy. Similarly the results of Scientist or designee, R&D – Analytical shall reviewed by the Chemist/analyst-QC.
- All the data of method transfer shall be reviewed by Head QC and approved by Head Quality.
- All the original raw data, chromatograms shall be retained at the QC. However a copy of the method transfer report shall be maintained at the R&D – Analytical.
- Reporting of method transfer results shall be as per format.
- The data shall be authorized by Head Quality or the person designated by them. The data shall be screened to note outliers and then subjected to collaborative evaluation.
- After meeting the acceptance criteria of method transfer, method transfer certificate shall be signed by Head QA.
- If the acceptance criteria not met, R&D – Analytical shall analyze the data to look for any ambiguity (e.g. failure in dissolution due to filled content variation/ weight variation). If any ambiguity observed, method can then be transferred with proper justification. If no such ambiguity is found, perform the reanalysis of analytical method transfer at receiving unit.
- For failure in case of direct method transfer, a fresh batch/ aliquot of sample shall be taken for reanalysis. Repeat analysis shall be performed in duplicate and average of the two results shall be reported.
- If the method does not
meet the acceptance criteria even after the repeat analysis, the data shall be
submitted. The follow-up action
shall be decided by the Head, R&D – Analytical.
- Investigation report shall be filled along with the transfer certificate.
- Reference (S)
USP 38 <1224> Transfer of Analytical Procedures
SOP : Standard Operating Procedure
No. : Number
R & D : Research and Development
HPLC : High pressure liquid chromatography
GC : Gas Chromatography
QC : Quality Control
QA : Quality Assurance