Cleaning Validation Protocol [PDF]

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VEGA LIFE SCIENCES PVT. LTD Pashamylaram, Patancheru, Sangareddy Dist, TS, INDIA. Cleaning Process Validation Protocol 1.0

PRODUCT NAME: 1, 3 - DICYCLOHEXYL CARBODIIMIDE Protocol No.: CV/P/DCC-19001 Effective Date: Stage Code: DCC Page No.: 1 of 6 Department: QA

Objective: 1.1 The objective is to provide a high degree of assurance that the cleaning procedure for the set of equipment used during product change over from 1, 3-Dicyclohexyl Carbodiimide (DCC) to any other product to check the effectiveness cleaning and to control of carryover of previous product 1, 3-Dicyclohexyl Carbodiimide (DCC) to the prospective products. 1.2 To evaluate the effectiveness of the steps used to clean the set of equipment and to establish the limits based on the results obtained from validation cycles.

2.0

Scope: The validation covers the cleaning procedure for the set of equipment used during product change over from 1, 3-Dicyclohexyl Carbodiimide (DCC) to any other product at Vega Life Sciences Pvt Ltd.

3.0

Responsibilities: 3.1 QA is responsible for preparation of Cleaning Validation Protocol. 3.2 Production is responsible for carryout of cleaning as per established procedure. Also responsible for review of protocol. 3.3 QC is responsible for collection of sample and testing of sample. Also responsible for review of protocol.

4.0

Number of cycles and selection of equipment: 4.1 Three validation cycles (both rinse and swab) shall be considered for the completion of the equipment cleaning validation. The equipment shall be cleaned as per procedure mentioned in “Equipment Cleaning Record” after completion of 1, 3-Dicyclohexyl Carbodiimide (DCC) batches execution for product changeover. The details of set of equipment is furnished below table-1

Prepared by

Checked by

Approved by

Ch. Ravi Babu Executive - Production

M.Aditya Varna Plant Head

P. Venkateswara Rao Manager - Quality

Sign & Date Name Designation

VEGA LIFE SCIENCES PVT. LTD Pashamylaram, Patancheru, Sangareddy Dist, TS, INDIA. Cleaning Process Validation Protocol

PRODUCT NAME: 1, 3 - DICYCLOHEXYL CARBODIIMIDE Protocol No.: CV/P/DCC-19001 Effective Date: Stage Code: DCC Page No.: 2 of 6 Department: QA

S. No. Equipment No.

5.0

1 2 3 4 Procedure:

Capacity

SSR-105 SSR-108 SSR-110 SSR-107

MOC Stainless Steel Stainless Steel Stainless Steel MS+GL/Propeller

Volume of solvent used for final rinse (L) 10 10 10 10

5.1 Cleaning Validation numbering system is as follows: CV/PC/@-YYNNN Where: CV

- Cleaning Validation

PC

- Protocol

@

- Product Code / Stage

YY

- Last two numerical figure of calendar year

NNN

- Sequential number starts from 001,002 and so on......

Note: PC will replace ‘R’ for report.

5.2 Equipment cleaning procedure: 5.2.1 All the equipment involved in 1, 3-Dicyclohexyl Carbodiimide (DCC) manufacturing shall be cleaned as per “Equipment Cleaning Records”. The respective equipment cleaning record details are furnished below. 5.2.1.1 Stainless steel reactor cleaning record: ECR/SSR/001-00 Effective date: 01.12.2019

Prepared by

Checked by

Approved by

Ch. Ravi Babu Executive - Production

M.Aditya Varna Plant Head

P. Venkateswara Rao Manager - Quality

Sign & Date Name Designation

VEGA LIFE SCIENCES PVT. LTD Pashamylaram, Patancheru, Sangareddy Dist, TS, INDIA. Cleaning Process Validation Protocol

PRODUCT NAME: 1, 3 - DICYCLOHEXYL CARBODIIMIDE Protocol No.: CV/P/DCC-19001 Effective Date: Stage Code: DCC Page No.: 3 of 6 Department: QA

Note:  The cleaning for each of the equipment involved for cleaning validation shall be executed as per the instructions provided in the “Equipment Cleaning Records”.  Based on the results obtained from the three cycles (both rinse and swab), the capability and effectiveness of cleaning procedures shall be reviewed. 5.3 Sampling procedure: 5.3.1 Swab sample shall be collected according to Annexure-1 before rinse sample by QC. 5.3.2 Swab area will be 10 x 10 cm in vertical and horizontal method by using swab sticks. The area will be quantified by using suitable measuring tool free from contamination. Swab residues will be dissolved in 10 ml Methanol and shall be measured by UV. 5.3.3 QC shall collect the rinse sample into a cleaned sample bottle after physical verification of equipment by quality assurance. 5.3.4 QC shall ensure the container label. 5.3.5 QC shall be analysed the samples as per the validated testing procedure. 5.3.6 Samples shall be carried out from production to QC under closed conditions. 5.4 Swab and Rinse sampling for equipment: 5.4.1 10 x 10 cm area of swab sample to be collected. 5.4.2 Test sample shall be collected from final rinse of 10 L. 6.0

Analytical method of analysis: 6.1

Both swab and rinse samples shall be analyzed by UV method.

6.2

Procedure for determination of wavelength: Scan the 100 ppm1, 3-Dicyclohexyl Carbodiimide (DCC)

standard solution

from 200 to 400nm and observe the wavelength maximum absorbance of the sample. Prepared by

Checked by

Approved by

Ch. Ravi Babu Executive - Production

M.Aditya Varna Plant Head

P. Venkateswara Rao Manager - Quality

Sign & Date Name Designation

VEGA LIFE SCIENCES PVT. LTD Pashamylaram, Patancheru, Sangareddy Dist, TS, INDIA. Cleaning Process Validation Protocol 6.3

PRODUCT NAME: 1, 3 - DICYCLOHEXYL CARBODIIMIDE Protocol No.: CV/P/DCC-19001 Effective Date: Stage Code: DCC Page No.: 4 of 6 Department: QA

Solution Preparation (100ppm): Weigh and transfer accurately 10mg of 1, 3-Dicyclohexyl Carbodiimide (DCC) working standard into a 100.0ml clean and dry volumetric flask, add about 25ml of water and sonicate to dissolve. Makeup to the volume to the mark with Water. Transfer and dilute the above stock solution with water as per the following table-2. Table-2

01

Stock solution

1.0

100.0

Resulting concentration of solution (ppm) 1

02

Stock solution

2.0

100.0

2

03

Stock solution

5.0

100.0

5

04 05 06

Stock solution Stock solution Stock solution

1.0 2.0 3.0

10.0 10.0 10.0

10 20 30

S. No.

Name of the solution transferred

Transferred volume (mL)

Diluted volume (mL)

Limit: Not more than 100ppm (0.01%) 7.0

Selection of solvent: Selection criteria of solvent for cleaning shall be based on the solubility (water followed by methanol) pattern of 1, 3-Dicyclohexyl Carbodiimide (DCC)

.

The

quantity of rinse volume shall be noted in the respective cleaning records. Swab sample location will be followed as per Annexure-1. 8.0

Data to be compiled: Upon execution of validation cycles and analysis of samples, complete the following data. 8.1

Quantity of Methanol used.

8.2

Fresh Methanol to be used (commercial) for final rinse.

8.3

Tabulate the data and analyze the data in comparison with the prescribed criteria and specifications. Prepared by

Checked by

Approved by

Ch. Ravi Babu Executive - Production

M.Aditya Varna Plant Head

P. Venkateswara Rao Manager - Quality

Sign & Date Name Designation

VEGA LIFE SCIENCES PVT. LTD Pashamylaram, Patancheru, Sangareddy Dist, TS, INDIA. Cleaning Process Validation Protocol 9.0

PRODUCT NAME: 1, 3 - DICYCLOHEXYL CARBODIIMIDE Protocol No.: CV/P/DCC-19001 Effective Date: Stage Code: DCC Page No.: 5 of 6 Department: QA

Acceptance Criteria: 9.1

Trained personnel shall be performed the validation study.

9.2

The results of the individual equipment should be less than the specified value.

9.3

Analyse the rinse samples individually for description and content of total residue as per the procedure. S. No.

Test

Acceptance criteria

1.

UV

Not more than 100ppm (both swab & rinse samples)

10.0 Review of documents: The following documents to be reviewed to ensure the activities are carried out according to requirement. 10.1 Executed cleaning records during product change over 10.2 Test methods 10.3 Analysis records 10.4 Training records 11.0 Steps to be taken in case of failures: In-case there are assignable causes such as deviations due to operating personnel, equipment problem, then the next cycle shall be considered for validation in place of deviated batch. In-case the result variation is due to random cases i.e. no assignable cause is found, then validation shall be repeated with three other cycles with modified cleaning procedure. 12.0 Validation and Conclusions: Upon completion of cleaning validation, compile the data and prepare a validation report by tabulating all the results and observations made during the validation study. The cleaning validation report shows that product changeover cleaning process has satisfied all the Quality attributes acceptance criteria, then it shall be concluded that

Prepared by

Checked by

Approved by

Ch. Ravi Babu Executive - Production

M.Aditya Varna Plant Head

P. Venkateswara Rao Manager - Quality

Sign & Date Name Designation

VEGA LIFE SCIENCES PVT. LTD Pashamylaram, Patancheru, Sangareddy Dist, TS, INDIA. Cleaning Process Validation Protocol

PRODUCT NAME: 1, 3 - DICYCLOHEXYL CARBODIIMIDE Protocol No.: CV/P/DCC-19001 Effective Date: Stage Code: DCC Page No.: 6 of 6 Department: QA

cleaning procedure for the product 1, 3-Dicyclohexyl Carbodiimide (DCC) to other product is found to be effective. Based on the results obtained from three validation cycles during product changeover from 1, 3-Dicyclohexyl Carbodiimide (DCC)

to any other product, prepare the

validation report and comment on the efficacy of the cleaning method used and establish the limits for routine monitoring of equipment cleaning during product changeover. Finally, conclude whether this method is valid for regular cleaning of the equipment during product changeover from 1, 3-Dicyclohexyl Carbodiimide (DCC) to any other product. Once validation study is completed, the cleaning procedure and testing method shall be verified for suitability and any changes required, same shall be addressed through change control to the cleaning procedure or any associated procedures. Deviations shall be documented, investigated, evaluated before concluding the cleaning validation study report.

Prepared by

Checked by

Approved by

Ch. Ravi Babu Executive - Production

M.Aditya Varna Plant Head

P. Venkateswara Rao Manager - Quality

Sign & Date Name Designation