|Product Name :|
|Generic Name :||
Terbutaline Sulphate, Ambroxol HCl, Guaiphenesin and Menthol Syrup
|Type of Validation :||Concurrent Validation|
|Reason for Validation :|
|Batch Size :|
TABLE OF CONTENTS
|S. No.||Subject||Page No.|
|8.||Batches selected for validation study|
|10.||List of raw material for formulation:|
|11.||Manufacturing Process flow chart|
|12.||Equipments Used For Process|
|13.||Qualification status of equipment’s|
|15.||Critical process parameters:|
|16.||Sampling, test parameters, acceptance criteria|
|17.||Certificate of analysis|
|18.||Mixing time validation|
|19.||Machine set up & filling & sealing checks|
|20.||Stability study Sample|
|22.||Change control / revalidation criteria|
|24.||Evaluation of the Results|
|26.||Summary and Conclusion|
|To demonstrate that the manufacturing process of Terbutaline Sulphate, Ambroxol HCl, Guaiphenesin and Menthol Syrup Syrup has been consistently producing the product, that meets its predetermined specifications and quality attributes.|
|Three consecutive batches of the Terbutaline Sulphate, Ambroxol HCl, Guaiphenesin and Menthol Syrup Syrup have been manufactured according to the method of manufacture to re-confirm the standard manufacturing process parameters.|
|4.||VALIDATION TEAM :|
|A representative from following Departments:
· Quality Assurance
· Quality Control
|During execution of 3 consecutive batches of the product as per the Batch Manufacturing Record, sampling at critical stages was done as per the protocol. Results of all parameters have to be compiled in this report.
|8.||BATCHES SELECTED FOR VALIDATION STUDY:
|10.||LIST OF RAW MATERIAL FOR FORMULATION:
RAW MATERIALS FOR BATCH SIZE: 1000 Ltr.
|*The Quantity of API may vary depending on potency / Assay & %LOD /Water/ Moisture content.
** The Quantity of Purified water may vary according to API.
|11.||MANUFACTURING PROCESS FLOW CHART: –
Equipment Critical Process Process Variables Tests
|12.||EQUIPMENTS USED FOR PROCESS:
|13.||QUALIFICATION STATUS OF EQUIPMENTS
|Raw Material weight verification:
The balance calibration & their record found well within the set acceptance. The weight of all the ingredients was verified as per bill of material given in batch manufacturing record & found satisfactory.
|Mixing of the Terbutaline Sulphate, Ambroxol HCl, Guaiphenesin and Menthol Syrup Syrup with the specified ingredients has been done for 30, 40 & 50 minutes in manufacturing tank. Samples have been taken from 02 different locations (from Top and Bottom) for testing as per details given in the process validation protocol. The content of assay of Terbutaline Sulphate, Ambroxol HCl, Guaiphenesin and Menthol Syrup Syrup after 30-50 minute of mixing found well within the acceptance limit (90.0 to 110.0 % of labeled amount).|
|Filling and Sealing:|
|Samples were collected & tested from filling and sealing machine as per frequency set in the protocol. During filling and sealing, all the parameter found well within the acceptance criteria at a speed of 50 and 150 BPM. All the parameter e.g. average net volume, uniformity of filled volume, pH, leak test were performed on the samples taken at initial, middle & end of filling and sealing process and found consistent & well within the limit prescribed in the in-process specification of filling and sealing stage. The content of assay of Terbutaline Sulphate, Ambroxol HCl, Guaiphenesin and Menthol Syrup Syrup found well within the acceptance criteria (90-110% of the labeled amount respectively) at 50 & 150 BPM and at initial, middle and end of the filling and sealing process.|
|For The Process Parameter:
|For Analytical Parameter:
|During manufacturing & packing process temperature & relative humidity have been checked & found as per environment requirement.|
|15.||CRITICAL PROCESS PARAMETERS:
|16.||SAMPLING, TEST PARAMETERS, ACCEPTANCE CIRTERIA:
|17.||CERTIFICATE OF ANALYSIS:|
|Certificate of analysis for under process validation study below the table maintained
|18.||MIXING TIME VALIDATION:
|19.||MACHINE SET UP & FILLING & SEALING CHECKS:
BOTTLE FILLING AND SEALING M/C ID:
|BOTTLE FILLING AND SEALING M/C:
|20.||STABILITY STUDY SAMPLES:
Three Consecutive validated batches of Terbutaline Sulphate, Ambroxol HCl, Guaiphenesin and Menthol Syrup Syrup shall be subjected for Stability Study at following conditions:
2. Long Time stability study at condition 30 + 20 C, RH 75% + 5% for period of 3, 6, 9, 12, 18, 24, months. MLT Performed 0, 3, 6, 9, 12, 18, 24 months. Sample qty.-Require 10 bottle for each station.
|The process validation study of Terbutaline Sulphate, Ambroxol HCl, Guaiphenesin and Menthol Syrup Syrup shall be carried out on three Consecutive commercial batches following parameters shall be considered as acceptance criteria for process validation study|
|These batches shall be manufactured & complied as per Master Production and Control records.|
|The equipment utilized for the manufacturing and processing of these batches shall be as per list of qualified equipment’s mentioned in Master Production and Control Record.|
|The raw material used for manufacturing process shall be produced from approved vendors only and shall be approved by Quality Control.|
|The critical process parameters of the process shall be evaluated with respect to quality attributes of the products|
|Sampling for in-process control samples is to be carried as per established sampling plan.|
|Critical in-process control shall be evaluated with respect to the laid down specifications.
Finished drug product of these Batches shall be analyzed and meet as per Pre determined specification & it shall be in compliance with the same.
|22.||CHANGE CONTROL / REVALIDATION CRITERIA:|
|The manufacturing process for the Terbutaline Sulphate, Ambroxol HCl, Guaiphenesin and Menthol Syrup Syrup shall be revalidated when there is change in following parameters.
1. Change in facilities or plant.
2. Change or replacement in a critical piece of equipment.
3. Change in source of active pharmaceutical ingredient.
4. Change in batch size.
5. Sequential batches that fail to meet product and process specification on the basis of trend analysis data of one year.
|The implementation of these changes shall be carried out through change control system.|
In case of any deviation(s) are observed they shall be noted down in the deviation report immediately. The deviation shall be noted in succession throughout the process along with the corrective action.
|24.||EVALUATION OF THE RESULTS:|
|After review, the results shall be evaluated for achievement of the acceptance criteria. In case of any deviation, effect of deviation shall be evaluated on the process and quality of the product.|
The yield after filling and sealing was ……………% and it was well within the acceptance criteria (NLT 98.0%).
|26.||Summary & Conclusion: