gbc-007 process validation.doc (英文)(doc 31页).doc

PROCTER i e store at a special temperature until tested test within 5 minutes of taking sample etc f Analyses for Each Sample Note which test s must be performed for each sample taken Be sure to note any special instructions i e number of replications samples which need to be sent to PDD for analysis or to an outside lab etc g Analytical and Microbiological Methods All analytical and microbiological methods used to test finished product batches for conformance to the validation criteria which includes finished product release criteria must be PD validated site verified and performed by qualified analysts using qualified equipment The following situations are also acceptable 1 Having any qualified plant or PD analyst s using qualified plant equipment to perform each method 2 Having samples sent to PD Analytical for analysis to be performed by qualified analyst s or 3 Having a validated outside laboratory perform certain method s H ACCEPTANCE CRITERIA 1 For Each Sample and Test Performed list in the Sampling Analysis Plan Matrix the requirements that must be met for all samples taken Each sample and required test must have acceptance criteria specified Acceptance criteria outside the requirements listed below must be justified in the Performance Qualification protocol The acceptance criteria need to include the following a All products within specification limits for all samples and all analyses actives pH viscosity color flavor etc b Within Batch Variation For active assay measurements and other ingredients or parameters that affect product efficacy the standard criteria for within batch variation homogeneity is for the Relative Standard Deviation RSD of the within batch samples to be 5 or less The 5 RSD criteria applies to all make stock and intermediates containing active ingredients If the packaging process subjects the product to conditions likely to affect the homogeneous distribution or availability of the active ingredient then the 5 RSD requirement must also be verified for packaged product Additionally all active assay results must be within 90 110 of target If any other limits are chosen a justification of the scientific rationale must be documented in the protocol The RSD of the analytical method should be considered when establishing acceptance criteria c Between Batch Variation For active assay measurements and other ingredients or parameters that affect product efficacy the standard criteria is for the relative standard deviation RSD of all between batch samples to be 5 or less Again the RSD of the analytical method should be considered in setting this acceptance criteria Note For both between batch i e to be shipped to the trade to be scrapped etc Explicitly state in this section the product release criteria If applicable state in this section the release criteria for shipment of bulk product i e from a manufacturing site to contract manufacturing site J SIGNATURES See Responsibilities Section for appropriate approval signatures Submitted by name date for the Team By signing below we indicate that we have reviewed the protocol and have found it to be sufficient to demonstrate the performance of the process against appropriate acceptance criteria Name Title DateName Title Date Performance Qualification Report The following sections are to be addressed in the development of a PQ report PERFORMANCE QUALIFICATION REPORT Validation Protocol Number XXXX A CONCLUSIONS State here the conclusion regarding the validation of the process based on the results of the validation batches Explain the reasoning that would support a successful or not successful conclusion regarding this validation B DISCUSSION 1 Compliance with the Performance Qualification Protocol Make reference to the protocol and indicate whether it was followed completely or not Clearly explain and document any deviations made from the protocol Where there are deviations from the protocol the Performance Qualification Report should contain a recommendation as to the impact of this deviation on the validation 2 Results versus Success Criteria Use this section to briefly summarize the information and to discuss any result s that are not obvious in the table It is helpful to provide a summary of key data at this point C SIGNATURES See Responsibilities Section for appropriate approval signatures Submitted by name date for the Team By signing below we indicate that this process is validated because it has met all of the acceptance criteria spelled out in the pre approved protocol Name Title DateName Title Date E APPENDIX 1 Performance Qualification Protocol 2 Performance Qualification Results Summary Table 3 Completed Batch Records or reference batch record numbers and location 4 Installation Operational Qualification Report Instant Run Process Validation IRPV IRPV is conducted to support release of a single batch or lot of product IRPV s are used to demonstrate that product manufactured individually or on a one time basis yields a finished product meeting all of its finished product and in process specifications and quality attributes IRPV can only validate the batch in question not the process or equipment used to make the product The use of an IRPV may be acceptable in situations such as the following Production of 1 batch of product to produce sales samples well prior to start of commercial production Production of 1 batch of product for test market where the decision regarding broad scale commercialization has not been made Production for one time studies where the intent is to verify conditions prior to full process validation Production of very low volume products where only 1 to 2 batches per year are produced Production of batch as one time offer typical examples are cosmetic shade change offers or promotion samples in one season where only one batch is required to be produced IRPV s are not intended for test market or national production where 3 or more batches are expected to be required to supply a one year test market IRPV s are not intended for meeting shortages in production supply The decision to use an IRPV will be made by the Plant QA Manager in consultation with GBU QA and PD for product intended for commercial distribution IRPV s in manufacturing facilities require a protocol and report to support release of product The protocol and report should follow the format for prospective process validations In situations where IRPV s are used evaluation of data testing and sampling are expected to be more extensive than during routine production where more reliance is placed on prospective validation Instead data evaluation testing and acceptance criteria should be comparable to that of the first batch of a full prospective validation Acceptance criteria must be based on sound technical rational Consideration must be given to whether the IRPV requires a confirmatory stability study Establishment of acceptance criteria should consider historical product and process performance An IRPV may be used as one of the batches for a prospective validation For the full validation where an IRPV batch is used as part of the full validation between batch variation must be analyzed across the IRPV batch and the other validation batches Note The justification or rationale for performing an IRPV instead of PQ must be documented in the IRPV Protocol ATTACHMENTS DEFINITIONS Attachment 1 Glossary Attachment 2 IQ OQ Protocol Example Attachment 3 IQ OQ Report Example Attachment 4 PQ Protocol Example Attachment 5 PQ Report Example REFERENCES Worldwide QA Policy 6 Validation and Change Management Worldwide QA CQG 6 Validation of Analytical Methods Worldwide QA CQG 16 Validation Program for R 1 The system was constructed delivered and installed to specifications and 2 3 The system operates as designed 2 SYSTEM DESCRIPTION Provide a description of the purpose and method of operation for the system being qualified Discussion Where possible attach a flow sheet or create a basic sketch to clearly illustrate the system being studied Example The Binder Mix System provides a mixture of treated water and citric acid to the Schugi agglomerator for atomization in the mixing chamber The Binder Mix System Consists primarily of a 200 gallon stainless steel mix tank TK 500 with agitator M 600 and a 300 gallon storage tank TK 510 Treated water is added to the mix tank to a predetermined weight cut off then citric acid is manually added to the tank via the loose cover After a period of agitation the mix is transferred to the storage tank for use The mixture is delivered to the Schugi by the Binder Feed Pump P 300 To Schugi Binder Feed Pump P 300 Binder Storage Tank Agitator M 600 Binder Mix Tank TK 500 TK 510 3 TEST ASSUMPTIONS BOUNDARIES Provide a brief narrative to describe base assumptions associated with the qualification Clearly state the boundaries of the system and the operating conditions which the qualification will be evaluate Example The qualification will be limited to the equipment associated with the installation of the new binder liquid mixing system System boundaries The binder mixing system starts just after valve FV 2192 that shuts the Treated Water Supply off to both the Binder Mix Tank TK 500 and the Treated Water Tank TK 510 The system includes the pump and all of the piping and instrumentation to the Binder Solution recycle valve FV 2196 and the Treated Water supply valve FV 710 including the valve Binder Mix System will be tested at centerline operating conditions 6 GPM and across the maximum operating range judged technically feasible 4 8 GPM INSTALLATION QUALIFICATION Installation Qualification involves establishing documented evidence that process equipment and ancillary systems equipment are constructed and installed to meet design intent IQ does not typically include operation of the equipment IQ may only need to be performed once after initial installation Thereafter IQ may not be required for each different process validation All or part of IQ may need to be repeated following major repairs renovations or modifications to the equipment 4 EQUIPMENT LIST i e number of replications samples which need to be sent to PDD for analysis or to an outside lab etc e Special Instructions Disposition of Sample Special Instructions should include where the samples be taken once they re collected For example some might be sent to R i e to be shipped to the trade to be scrapped etc Explicitly state in this section the product release criteria If applicable state in this section the release criteria for shipment of bulk product i e from a manufacturing site to contract manufacturing site Examples Product will be released to the trade upon completion and approval of the Performance Qualification Report demonstrating that all success criteria which includes all finished product specifications have been met If the criteria are not met the product will be subject to other disposition as mutually agreed by the Team Leader and the Plant QA Manager Bulk product will be shipped from the plant to a contract packaging site Bulk product will be released from the plant only after completion and approval of the Performance Qualification Report 9 RESPONSIBILITIES In this section list the people who are responsible executing the various sections spelled out in this Performance Qualification Protocol Example TaskPerson Responsible 1 Label sample containers for each sample called for in the sampling plan 2 Pull samples per sampling plan top of mix tank discharge samples treated water samples 3 Take samples to lab at conclusion of each batch 4 Perform required analysis in Quality lab Log in appropriate lab books on separate page marked XYZ Validation viscosity pH soluble fluoride G Jones G Jones W Jennings R Travis D Parton C Black W Nelson G Brooks 10 APPROVALS Manufacturing Facilities a For new products line extensions and formulation changes Product Development PDD has responsibility to assure process validation is conducted and completed This includes responsibility to ensure that critical processing parameters and acceptable ranges are identified and responsibility to ensure that the required documents are written including the Performance Qualification Protocol and the Performance Qualification Report Product Supply PS has responsibility to write and execute the Installation Qualification IQ and Operation Qualification OQ protocol This includes responsibility to prepare the IQ OQ Report b For existing packing processes making processes utilities facilities and laboratory equipment used in the manufacture of existing products and changes to these systems the plants have lead responsibility to assure process validation is conducted and completed This includes lead responsibility to write the required documents c The Plant QA Manager is responsible to assure validation files exist and are kept current d The Plant QA Manager and Operations Manager or designate will review and approve all IQ OQ and PQ protocols and reports e The appropriate PDD Section Head or designate will review and approve all PQ protocols and reports for new initiatives Example Submitted by name date for the Team By signing below we indicate that we have reviewed the protocol and have found it to be sufficient to demonstrate the performance of the process against appropriate acceptance criteria Name Title DateName Title Date Name Title DateName Title Date Attachment 5 PERFORMANCE QUALIFICATION SUMMARY REPORT 1 CONCLUSIONS State here the conclusion regarding the validation of the process based on the results of the validation batches Explain the reasoning that would support a successful or not successful conclusion regarding this validation Example The process is validated All analyses were performed using validated analytical methods that have been plant verified Documented evidence shows the specifications and procedures employed are sufficient to consistently produce quality product meeting all specifications Product met all predetermined success criteria 2 DISCUSSION a Compliance with the Performance Qualification Protocol Make reference to the protocol and indicate whether it was followed completely or not