Protocol for Glassware Cleaning Validation

TABLE OF CONTENT

1. Protocol Pre-Approval
2. Objective
3. Scope
4. Responsibility
5. Training
6. Pre-Requisites
7. Description of Method
8. Details of Glassware Cleaning Validation
9. Type of Analysis: BY UV
10. Acceptance Criteria
11. Summary
12. Conclusion
13. Abbreviation
14. Deviation/OOS/Changes (If Any)
15. Revision History

1. PROTOCOL PRE APPROVAL

Preparation and Approval of this Glassware cleaning validation document will be joint responsibility of the following functional area.

Any modification in this document shall be documented and approved.

Prepared By:
Department Name	Name of Person	Designation	Sign and Date
Quality Control

Reviewed By:
Department Name	Name of Person	Designation	Sign and Date
Quality Control
Microbial Lab
Quality Assurance

Approved By:
Department Name	Name of Person	Designation	Sign and Date
Head- QA

 

2. OBJECTIVE

To perform Glassware Cleaning Validation provides documentary evidence that the method used for Glassware Cleaning Validation of said product full fill the regulatory & compendia requirement. This protocol presents and discusses the result obtained in the Validation study.

3. SCOPE

This document is applicable for the Glassware Cleaning Validation of UV Method which is applying at PharmaGuide Ltd.

4. RESPONSIBILITY

4.1. Quality Control

• To perform the analysis in the Verification and evaluate the data as per protocol.
• To prepare the protocol and review all data evaluated as per protocol.
• To provide technical support, review the protocol and ensure that all parameter performed as per protocol

4.2. Quality Assurance head / designee

• Approval of Glassware Cleaning Validation protocol and report.
• Training of Glassware Cleaning Validation
• Monitor of Glassware Cleaning Validation activities

5. TRAINING

Training is imparted for all personnel involved in Glassware cleaning validation

This training shall be attached along with Glassware cleaning validation Protocol/Report.

6. PRE-REQUISITES

Following parameters shall be checked before carrying out Glassware Cleaning Validation:

Sr. No.	Parameters	Confirmation
1.	The basic SOPs on Glassware cleaning procedure should be available.
2.	Glassware cleaning validation protocol should be available before starting Validation.
3.	Training shall be given to all concerned department and person involved in activity

7. DESCRIPTION OF METHOD

7.1. Equipment/Instrument required during validation

Sr. No.	Name of Equipment	Calibration Status
		Equipment No.	Calibration on	Calibration Due	Make/Mode
1	UV Spectrophotometer

7.2. Reagents and Chemicals

Sr. No.	Name of Reagent	Grade	Make	Lot No.
1.	Water
2.	pH paper strips
3.	Conical flask

ALSO READ: Cleaning Validation of Sampling Accessories

8. DETAILS OF GLASSWERE CLEANING VALIDATION

8.1 Chemical cleaning optional methods

• When a piece of glassware is badly contaminated with stopcock grease (except silicone grease), it may be necessary to rinse with acetone once or twice before using one of the methods below. For silicone grease, the acetone can be omitted, and the piece soaked for 30 min in fuming sulfuric acid. Warm decahydronaph- thalene (decalin) also has been suggested as a solvent for silicone grease. In this case, let the piece soak for 2 h, drain, and rinse once or twice with acetone, followed by a water rinse.
• Fill with sulfuric acid-dichromate mixture and let stand. After removal of the mixture, rinse with distilled water at least six times. To make the cleaning mixture, dissolve 60 g to 65 g of sodium- or potassium-dichromate by heating in 30 mL to 35 mL of water, cool and slowly add concentrated sulfuric acid to make one liter of solution. This solution is available from laboratory supply companies. Note: Extreme care should be exercised in handling acidic solutions.
• Scrub with a 1 % to 2 % hot solution of a detergent. Rinse well after brushing. Several suitable, commercial washing compounds are available.
• Fuming sulfuric acid (very hazardous material) is an excellent cleaning agent. Usually, cleaning can be accomplished by use of a comparatively small amount of acid, manipulating the vessel so that the acid contacts the entire surface, and immediately emptying and rinsing

8.2  Preparation of cleaning solutions

• For the cleaning of glassware, those are used for chemical analysis special precautions will take place to avoid any chemical residue in glassware, which may later interfere with the results of chemical analysis.
• Following cleaning solutions were used for cleaning of glassware.

1. 2% Liquid soap solution
2. Measure 20 ml soap solution and add it to container containing 980 ml of purified water and stir it well.
3. Record the solution preparation details in glassware cleaning solution preparation record.

8.3  Cleaning of glassware

• Cleaning of glassware, which has contained hazardous materials, must be solely undertaken by experienced personnel.
• Most new glassware is slightly alkaline in reaction. For precision chemical tests, new glassware should be soaked several hours in acid water (1% solution hydrochloric acid or nitric acid) before washing.
• Wash glassware as quickly as possible after use if it is not possible then the articles should be allowed to soak in water.
• For cleaning of glassware such as bottles, flasks, beakers, test tubes, etc use 2% liquid soap solution. For better results use hot water.
• During the washing all parts of the article should be thoroughly scrubbed with a brush selected for the shape and size of the glassware. Brushes should always be in good condition to avoid any abrasion of the glassware.
• Special types of precipitate material may require removal with nitric acid, aquaregia or fuming sulphuric acid. These are very corrosive substances and should be used only when required.
• Before cleaning of glassware remove the labeling of marker pen with the help of IPA or acetone. For plastic ware do not use acetone for removing marker pen labeling.
• It is imperative that all soap detergent and other cleaning fluids be removed from glassware before use. This is especially important with detergents, slight traces of which will interfere with serological and culture reactions. After cleaning, thoroughly rinse with tap water ensuring that containers are partly filled with water, shaken and emptied several times. Finally rinse with purified water.
• After cleaning dry the glassware in Hot air oven at 600 temperature ± 50.
• Always protect clean glassware from dust by use of temporary closures or by placing in a dust free cabinet.

9. Type of Analysis: BY UV

9.1 Blank Solution Preparation:

• The Purified water as a blank scans for 200nm to 400 nm riding to UV Spectrophotometer.

9.2 Sample Solution Preparation:

• After dry the Glassware cleaning for purified water (rinse sample) scan for 200 nm to 400 nm riding to UV Spectrophotometer.
• The glassware cleaning sample absorbance not more than blank sample absorbance.

9.3 Procedure:

• Switch on the main power supply After getting the initialization of instrument About 15 minutes, instrument Triple beep sound.
• Than Press enter and again sound of tree beep, Open the software on system UV-Visible analyst display on the system screen.
• Display system status, close click on file menu, click new and select fixed point measurement for single wavelength and multiple wavelengths.
• Click on file menu, click new and select Wavelength scan measurement for scanning.
• For scan click wavelength scan measurement fill up the blank medium in booth cuvette and click z for both cuvette matching.
• Then fill sample in sample cuvette and click red arrow.

ALSO READ: SOP for Calibration of Volumetric Glassware

9.4 pH Checks Procedure:

• Take the glassware of residual solvent checks.
• Add to it 0.04 % bromothymol blue solution and observe for color reaction.
• If the color observed as green means that acidity is present in the glassware.
• If the color observed as blue means that alkalinity is present in the glassware.
• If the color observed as blue-green means that pH is neutral, and use this glassware in routine.
• Some washing solutions are difficult to remove completely, so it is necessary to test clean glassware for an alkaline or acid residue.
• Add a few drops of 0.04 % bromothymol blue and observe the color reaction of the Bromo Thymol Blue.
• It gives blue-green colour between pH-6.5 to 7.3.
• It gives yellow colour below pH 6.5 and blue colour above pH 7.3.
• Preparation of 0.04 % bromothymol blue solution: Add 16 ml 0.01 N NaOH to 0.1 g bromothymol blue and dilute to 250 ml with distilled water.
• Acceptance criteria: Acidity and Alkalinity should be absent.
• Frequency : Monthly

9.5 Burette and Pipette cleaning Validation:

• This procedure is applicable to cleaning validation of pipettes and burettes.
• Keep the burette in burette stand, and tight the rubber cork screw by rotating it anticlockwise.
• Add the water in burette up to zero marking.
• Unscrew the rubber cork screw by rotating it clockwise, and allow to dropping of water in any two of general glassware had previously checked for acidity and alkalinity.
• Add in one glassware 2-3 drops of methyl red indicator.
• If water becomes red, it seems that acidity is present in the burette.
• If water remains colorless, deep the pipette in that water and suck the water using pipette bulb, if acidity is present in the pipette then it turns in red color.
• It seems that acidity is present in the pipette.
• Add in another glassware 2-3 drops of Phenolphthalein indicator.
• If water becomes pink, it seems that alkalinity is present in the burette.
• If water remains colorless, deep the pipette in that water and suck the water using pipette bulb, if alkalinity is present in the pipette then it turns in pink color.
• Acceptance criteria: Acidity and Alkalinity should be absent.
• Frequency : Monthly

9.6 HPLC & GC vials cleaning:

• This procedure is applicable to cleaning validation of vials.
• Take a clean and dried vial, and check it for residual solvent test as per mentioned in above step.
• Add the water in vial and transfer the water in previously checked container.
• Perform the acidity and alkalinity checks as per mentioned in above step.
• Acceptance criteria: Acidity and Alkalinity should be absent.
• Frequency : Monthly

10. ACCEPTANCE CRITERIA

Sr. No.	Title	Acceptance Criteria	Observation
1	ABSORBANCE	The glassware cleaning sample absorbance not more than blank sample absorbance.

• Frequency: Annually
• If prewashed, presterilized plasticware is used, test it for inhibitory residues
• Change in the washing procedure or the washing agent.

11. SUMMARY

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12. CONCLUSION

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13. ABBREVIATION

CEHT : Cleaned equipment Hold Time

MOC : Material of Construction

SOP : Standard operating procedure

CAPA : Corrective Action Preventive Action

SS : Stainless steel

GL : Glass Lined

hrs : Hours

QA : Quality Assurance

QC : Quality Control

cfu : Colony Forming unit

NMT : Not More Than

OOS : Out Of Specification

14. DEVIATION / OOS / CHANGES

Any deviation, OOS or changes that may occur during the process, shall be investigated and Referred in the report.

15. REVISION HISTORY

Nil

ALSO READ: SOP for Cleaning of Glassware used in Chemical & Instrumental Analysis