Analytical Method Transfer | USP chapter 1224

Procedure:

Definition:

All the relevant format for Method Transfer provided at the end of article: 

Method transfer is defined as the documented process that qualifies a laboratory (the receiving unit) to use an analytical test procedure that originated in another laboratory (the transferring unit), thus ensuring that the receiving unit has the procedural knowledge and ability to perform the transferred analytical procedure as intended.

·       This SOP presents the components necessary to complete a successful method transfer by means of comparative testing method.

·       Analytical method for assay, related substances, residual solvent etc. which are complex in nature, and for which analytical method has already been developed at Analytical Research Development, shall be included in the method transfer program. Head QCD and Head ARD shall have the rationale to exclude any method from the current scope of analytical method transfer.

·       Analytical method transfer protocol shall be initiated by the Head / Designee ARD.

·       Head QC and Head ARD shall set in place, a pre-approved protocol before start of the transfer exercise. Analytical Research Development shall inform/provide plant/QCD, the list of chemicals, reagents, working standards, instruments required for the method transfer exercise.

·       Method transfer shall include, practical demonstration and joint/comparative analysis of sample by ARD-Analyst and QC- Analyst. ARD- Analyst demonstrates the method by analysing the sample as per the protocol at the QC laboratory. After demonstration by the ARD- Analyst, QC- Analyst shall perform the analysis independently as per the MOA given by the ARD.

Preparation of protocol:

·       Protocol shall be specific to the product and method of analysis. Protocol shall contain the information relating to product name, method detail/description, transferring laboratory location and name, transfer type, working standard and other chemicals details, column details, batch numbers of samples and standards, test parameters and precautions to be taken during the analysis/handling.

·       Protocol shall be prepared by the Executive/ Designee ARD. Same shall be authorized by Head ARD and Head QC.

·       After approval of the protocol the method transfer activity shall be initiated.

Method Transfer:

·       Training during method transfer: Executive/ Designee ARD shall provide necessary training to the concern QCD- person and complete understanding about the method complexity and necessary skills required to perform the analysis as per the referred method. 

·       During the method transfer, all the details of analysis shall be written in the routine

analysis format. Details of instrument usage shall be written in the respective instrument usage logbook.

·       The result of QC & ARD Analyst shall be reviewed by the QC-In charge for accuracy and precision. Similarly, the result of ARD-Analyst shall be reviewed by the ARD Head /Designee ARD.

·       All the data of method transfer shall be verified by the Head QCD & Head ARD.

·       All the original raw data, chromatograms shall be retained at the QCD. However, a copy of all the records shall be maintained at the ARD laboratory.

·        This format for analytical method validation can be altered as per the requirement.

·        The data shall be evaluated by the Head-ARD and Head-QC 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 jointly signed by the Head-ARD and Head-QC.

Acceptance criteria limit:

·       If the limit of assay is NLT 90 % - NMT 110 % then % RSD for both the chemist should be NMT 5 %.

·       If the limit of assay is NLT 90 % then % RSD for both the chemist should be NMT  6 %.

·       For Related Substances % RSD for both the chemist should be NMT 5 %.

Handling of Method Transfer Failure

·       If the acceptance criteria are not met, Analytical Research Development shall          

analyse the data to look for any ambiguity. The method can be transferred with  

proper justification. If no such ambiguity is found, reanalysis shall be initiated at QC.

·       For failure in case of direct method transfer, a fresh batch of sample shall be   taken           

·       for re-analysis.

·       If the method does not meet the acceptance criteria even after the repeat analysis, the data shall be submitted as in Format (Given Below): The follow-up action shall be decided by Head, ARD. Investigation report as given in Format and shall be filled with the transfer certificate.

·       Investigation shall be carried out for failure as per the SOP of Root and Cause 

and report shall be prepared as per appropriate Format No.

            Note: Table can be viewed better in Desktop View

                  

ANNEXURE-I ANALYTICAL METHOD TRANSFER PROTOCOL Protocol No.                            : ­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­­______________________________ Name of Product                      :  ______________________________ Strength                                  :  ______________________________                                                           :  ______________________________                                                            :  ______________________________                                                            : _______________________________ Location of QC/ARD                 :  _______________________________ Method Transfer Type             :  ______________________________           1.         Method Reference (STP No.): __________________________ (Method attached). 2.         Method Validation Report No.: _________________________  3.         Sample Analysis:             Assay (Duplicate analysis) 4.         Reference Standards / Working standards (Name & B. No.): a.            b.           c.            d.                                 e.                        f.                       g.                       h.                        i.                        j.   5.         Sample Name and B. No.: 6.         Chemicals Required:                                        Column Specification                                                 _______________________________   7.         Precautions to be taken during sample handling/ preparation/ analysis:           ----------------------------------------------------------------------------------------------------------------------------------------- ----------------------------------------------------------------------------------------------------------------------------------------- --------------------------------------------------------------------------------------------------------------------------------------- 8.         Analyst Name: a)                   Analytical Development Chemist           :   QC Chemist     b)                   Analytical Development Chemist           :   QC Chemist                 c)                   Analytical Development Chemist           :   QC Chemist     d)                   Analytical Development Chemist           :   QC Chemist                 e)                   Analytical Development Chemist           :   QC Chemist     9.           Acceptance Criteria:   10.  Training on following has been provided to the QC Chemist (To be filled by the Analytical Development Officer/ Executive):        11.  Any deviation from the guideline given in SOP or method (Before start the method transfer): 12.  Deviation in acceptance criteria after repeat analysis.

REPORTING OF RESULTS OF METHOD TRANSFER Results of Assay Method Transfer     R & D Analyst QC Chemist Analyst Name             Instrument ID No.             Column ID No.             Date of Analysis                 Assay (% w/w)                                     %RSD               Acceptance Criteria:   Results of Dissolution Method Transfer     Analytical Development Chemist (I) QC Chemist (II) Analyst Name     Dissolution Apparatus No.     Instrument ID No.     Column ID No.     Date of Analysis       S. No. % Drug Release minutes/Hrs. minutes/Hrs. minutes/Hrs. minutes/Hrs. I II I II I II I II 1.                 2.                 3.                 4.                 5.                 6.                 Mean                 SD                 % RSD                   Acceptance Criteria:   Results of Related Substances Method Transfer     Analytical Development Analyst (I) QC Chemist (II) Analyst Name     Instrument ID No.     Column ID No.     Date of Analysis       S. No. % Impurity (w/w)/ % of Impurity Impurity Name       I 11 Single Highest Individual     Total Impurity     Known impurity (if any)     Known Impurity (If any)     Other Secondary impurity                   I 11 % RSD      % RSD     % RSD     % RSD     % RSD              Acceptance Criteria: Results of Residual solvents method transfer     Analytical Development Analyst (I) QC Chemist (II) Analyst Name         Instrument ID No.         Column ID No.         Date of Analysis         S. No. Content of Solvent in ppm Solvent Name       I II 1.     2.     3.                                 4 .       I II 1.     2.     3.                                 4.       Acceptance Criteria: