TABLE OF CONTENTS
- Protocol pre-approval
- Objective
- Scope
- Reference
- Site of Study
- Responsibility
- Materials and instruments
- Cleaning Procedure
- Experimental Design
- Acceptance Criteria
- Result
- Conclusion
- Validation Methodology
- Calculation
- Cleaning Validation Datasheet
- Determination of Traces of Alpha Lipoic Acid
- Determination of Traces of Teepol
- Cleaning Validation Report
PROTOCOL PRE- APPROVAL
INITIATED BY:
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REVIEWED BY:
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Executive QA |
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QC Manager |
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APPROVED & AUTHORISED BY:
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DESIGNATION |
SIGNATURE |
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Head- QA |
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OBJECTIVE
To provide the documentary evidence to ensure that the procedure used for the cleaning of sampling accessories is effective.
SCOPE
This validation study is performed on the sampling accessories which are used during routine sampling of raw material.
REFERENCE
SOP Coding and cleaning of sampling device.
SITE OF STUDY
Quality Control Laboratory
RESPONSIBILITY
Quality Assurance:
- Review, Approval and Compilation of the Cleaning Validation Protocol for Correctness, Completeness and Technical Excellence.
- Monitoring of validation Activity.
Quality Control
- Co-ordination with Quality assurance to execute the protocols.
- Preparation ,Review of Cleaning validation Protocol, testing and Execution.
DEFINITION
Sampling Accessories: The accessories which are used to withdraw the material e.g spatula, scoop, liquid sampling device, solid sampling device, chopper
ALSO READ: Cleaning Validation Protocol
MATERIALS AND INSTRUMENTS
- Instruments : UV Visible Spectrophotometer and HPLC
- Cleaning agent : Teepol
CLEANING AND STORAGE PROCEDURE
Cleaning of sampling accessories as follows:-
- Wash all the sampling accessories in tap water.
- Rub the inner and outer surface of of sampling device using liquid soap ( 2%Teepol) with plastic brush
- Rinse the sampling accessories in running tap water.
- Wipe inner and outer surface of sampling device using lint free cloth moist in 70% isopropyl alcohol
- Affix a label on polyethylene bag containing sampling device.
- The sampling device used for microbial testing to be cleaned as per above procedure and then sterilize at 1210C, 15lbs for 30 minute
TYPES OF SAMPLING ACCESSORIES
Sampling accessories used for Sampling
EXPERIMENTAL DESIGN
- Select the labeled sampling device as mentioned for the sampling of Alpha Lipoic Acid.
- Isolate the sampling device in sealed polythene bag immediately after sampling.
- Monitor the movement of the selected sampling device during washing, take care to maintain its identity throughout the cleaning.
- Clean the respective sampling device as per routine cleaning procedure mentioned in SOP and dry the same.
- Analyze the rinse sample as per mentioned in method details and report the observations in the cleaning validation data sheet.
- Rinse the volumetric flask with 10 ml of water and determine traces of Teepol.
ACCEPTANCE CRITERIA
Finding of the study should be below detectable limit as specified in the method details.
RESULT
- Observation and results to be recorded in the respective cleaning validation data sheet.
- Summarize the finding of the study to draw inference.
CONCLUSION
Based on the interpretation of the results in cleaning validation summary, draw the conclusion for the effectiveness of the cleaning procedure used.
VALIDATION METHODOLOGY
A. Determination of traces of Alpha Lipoic Acid
Chromatographic Conditions:
- Column: A Stainless steel column 250mm X 4.6mm(5µ),C18
- Flow rate: 1.2 ml/min
- Detector: 215nm
- Injection Volume: 20μl
- Diluent: Mobile phase
- Blank Injection: 1 run (Diluent)
- Standard injection: 5 run
- Sample injection: 2 run
Preparation of mobile phase:
Buffer Preparation: Dissolve 340 mg Potassium dihydrogen phosphate in 500ml Distilled water.
Preparation of Mobile Phase: Buffer: Methanol: Acetonitrile = 230:290:45
Adjust the PH 3.0 to 3.1
Preparation of Standard solution:
Weigh and transfer accurately about 25mg Alpha Lipoic Acid WS into 25ml volumetric flask. Add 10 ml of diluent and sonicate for 10 minutes. Make up the volume up to 25ml with mobile phase. Further dilute 1ml of this solution to 100 ml with mobile phase.
Preparation of Sample solution:
Add 10ml of diluent with the help of pipette in the cleaned accessories. Swirl the device determine content . Determine the content in rinse sample collected.
CALCULATION
Average area of sample ✕ Standard wt ✕ 1 ✕ Purity ✕ 1000
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Average area of standard ✕ 25 ✕ 100 ✕ 100
Limit of Detection
Alpha Lipoic Acid = 0.1 ppm
B. Determination of Traces of cleaning agent (Teepol)
Preparation Of Standard (Teepol):
Weigh 100mg of Teepol in a 100ml volumetric flask, dissolve and dilute to the volume with water. Dilute 10ml of this solution to 100ml with water. Further dilute 7.0 ml of this solution to 50 ml with water.
Sample Preparation:
Add 10 ml of water with the help of pipette in the cleaned sampling device. Swirl the device and determine content in rinse sample collected.
Calculation:
Measure the absorbance of Teepol solution at 223 nm of the sample solution using water as blank.
Traces of Teepol (ppm):
Sample absorbance ✕ Standard weight (mg) ✕ 10 ✕ 7.0 ✕ 1000
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Standard absorbance ✕ 100 ✕ 100 ✕ 50
Limit of Detection: 2.0ppm
Tags
Validation
