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Validation of pharmaceutical process, Analytical Method development Computer system validation, ERP. LIST OF CONTENTS. Process validation Introduction Type of validation Stage of validation Major phase of validation SOP Validation report. Method Validation.
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Analytical Method development
Computer system validation, ERP
Validation should thus be considered in the following situations:
The activities relating to validation studies may be classified into three:
Phase 1: (Pre-validation Qualification Phase)
which covers all activities relating to product research and development, formulation pilot batch studies, scale-up studies, transfer of technology to commercial scale batches, establishing stability conditions and storage, and handling of in-process and finished dosage forms, equipment qualification, installation qualification, master production document, operational qualification and process capacity.
Phase 2: This is the Process Validation Phase. It is designed to verify that all established limits of the critical process parameter are valid and that satisfactory products can be produced even under the worst conditions.
Phase 3: Known as the Validation Maintenance Phase, it requires frequent review of all process related documents, including validation of audit reports, to assure that there have been no changes, deviations, failures and modifications to the production process and that all standard operating procedures (SOPs), including change control procedures, have been followed.
A written report should be available after completion of the validation. If found acceptable, it should be approved and authorized (signed and dated). The report should include at least the following:
1. Compendial Analytical Procedures
When using USP 25/NF 20 analytical procedures, the guidance recommends that information be provided for the following characteristics:
Step 1 : select the validation team & define the roles of each team member
Step 2 : define the techanical & regulatory objectives
Step 3 : select the analytical technique
Step 4 : develop & document the analytical method
Step 5 : select the validation parameters & prepare a validation protocol
Step 6 : perform & document the validation
Step 7 : review the data Vs acceptance criteria set forth in the validation protocol ( A failure may change the validation protocol , back to step 5, if necessary)
Step 8 : write the final validation report
Step 9 : ongoing evaluation of the method
Step 10 : revalidation of the method
Defining the technical requirement
Considering the required precision
Considering the required detection limit
Selecting an analytical technique
The analytical method
Using an Exisiting method Modifying or optimizing an Developing a new analytical
Existing method method
Demonstrating method feasibility
Developing system suitability
Documenting the analytical method
Reference Standard Qualification
Qualification of a sourced Qualification of a synthesized reference
Reference standard material Standard material
Figure : The validation process from method development to method validation
LINEARITY - of an analytical procedure is its ability (within a given range) to obtain test results which are directly proportional to the concentration (amount) of analyte in the sample.
DETERMINATION- Linearity should be evaluated by visual inspection of a plot of signals as a function of analyte concentration or content.
Note:- For the establishment of linearity, a minimum of five concentrations is recommended.
RANGE - of an analytical procedure is the interval between the upper and lower concentration (amounts) of analyte in the sample (including these concentrations) for which it has been demonstrated that the analytical procedure has a suitable level of precision, accuracy and linearity.
The specified range is normally derived from linearity studies and depends on the intended application of the procedure.
ACCURACY -of an analytical method is the closeness of test results obtained by that method to the true value.
This definition incorporate both precision & specificity.
Accuracy is giving the laboratory & clinician the right answer, & describing the conc. Of analyte that actually present.
Note:- Accuracy should be assessed using a minimum of 9 determinations over a minimum of 3 concentration levels covering the specified range.
PRECISION- the reproducibility of replicate analyses at different levels of the analyte , within assay & between assay.
Expression of Precision
DETECTION LIMIT of an individual analytical procedure is the lowest amount of analyte in a sample which can be detected but not necessarily quantitated, under the stated experimental conditions.
QUANTITATION LIMITof an individual analytical procedure is the lowest amount of analyte in a sample which can be quantitatively determined with suitable precision and accuracy.
RUGGEDNESS of an analytical method is the degree of reproducibility of test results obtained by the analysis of the same samples under a variety of conditions, such as different laboratories different analyst, different instruments, different lots of reagent, different elapsed assay times, different assay temperatures, different days, etc.
ROBUSTNESS - of an analytical procedure is a measure of its capacity to remain unaffected by small, but deliberate variations in method parameters and provides an indication of its reliability during normal usage.
SYSTEM SUITABILITY TESTING - is an integral part of many analytical procedures. The tests are based on the concept that the equipment, electronics, analytical operations and samples to be analyzed constitute an integral system that can be evaluated as such.
List of contents -
To discuss validation of computerized systems including:
performance monitoring, change control, programme and data security, calibration and maintenance, personnel training, emergency recovery and periodic re-evaluation
In place, stating:
(Fluctuations in the electrical supply can influence computer systems and power supply failure can result in loss of memory).
GMP requirements for computer systems:
Independent verification and release for use by a second authorized person
2. Supply chain management
5. Human resources
6. Customer relationship management
7. Data services
8. Access control
J. Ermer and J. H. McB. Miller
Therapeutics Products Programme. Process Validation: Aseptic Processes for Pharmaceuticals. http://www.hcsc.gc.ca/ hpbdgps/ therapeutic; downloaded March 30, 2001.