Department: Page 1 of 11

Quality Assurance
Protocol No.: Revision No. 00
QA/PRT/PTH/082
Protocol for PT (HPLC)
Effective Date: Replaces:
Not Applicable
Doc. Ref. No.
Next Review Date:
QC/SOP/AQR/068A

kAPPROVAL

We have reviewed the “Protocol for Proficiency Testing of “HPLC <621>” and found it
acceptable.

Sr. No. Verification Team Responsibilities Signature Date

1. Lead QA-Lab Operation Preparation of Protocol

(QMS)

2. Chief Manager QC Review of Protocol

3. Manager QA (O&C) Approval of Protocol

Director Quality
4. Operations & Regulatory Authorization of Protocol
Affairs

Confidential Information – Remington Pharmaceutical Industries (Pvt) Ltd.

Not to be reproduced/disclosed without prior written approval
Department: Page 2 of 11
Quality Assurance
Protocol No.: Revision No. 00
QA/PRT/PTH/082
Protocol for PT (HPLC)
Effective Date: Replaces:
Not Applicable
Doc. Ref. No.
Next Review Date:
QC/SOP/AQR/068A

INDEX:

1.0 Purpose

2.0 Scope

3.0 Reference Document

4.0 Responsibilities

5.0 Procedure

6.0 Testing Plan & Result Evaluation

7.0 PT Report

8.0 Deviation

9.0 Change Control

10.0 Documentation

11.0 Summary of Results & Conclusion

12.0 Abbreviation

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Department: Page 3 of 11
Quality Assurance
Protocol No.: Revision No. 00
QA/PRT/PTH/082
Protocol for PT (HPLC)
Effective Date: Replaces:
Not Applicable
Doc. Ref. No.
Next Review Date:
QC/SOP/AQR/068A

1.0 Purpose

The purpose of this protocol for PT is to elaborate the procedure for the testing and
reporting of Proficiency testing sample of “HPLC <621>” received from “Sigma
Aldrich” Merck against Round QT-0027656.

2.0 Scope

This protocol is valid for QC Department of Remington Pharmaceutical Industries

(Pvt) Ltd.

3.0 Reference Document

3.1 Proficiency testing is being carried out against Packet instructions for round:
QT-0027656 received from sigma Aldrich (Merck)

3.2 ISO/IEC 17025 General requirements for the competence of testing and
calibration laboratories

4.0 Responsibilities

4.1 Lead QA-Lab Operations will be responsible to prepare protocol for PT and
to generate the report.

4.2 Manager QC/Designee will be responsible to review protocol and report. He

/ she is also responsible to review and handle any deviation observed during
Analysis.

4.3 Chief Manager QC/Designee will be responsible to review the protocol and
report to confirm that the analysis is performed as per requirement and
reportable.

4.4 Manager QA (O&C)/Designee will be responsible to approve this protocol

and report. He/She is also responsible to handle and approve any deviation
observed during execution.

4.5 Director Quality Operations and Regulatory Affairs is responsible for the
authorization of this protocol and execution.

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Department: Page 4 of 11
Quality Assurance
Protocol No.: Revision No. 00
QA/PRT/PTH/082
Protocol for PT (HPLC)
Effective Date: Replaces:
Not Applicable
Doc. Ref. No.
Next Review Date:
QC/SOP/AQR/068A

5.0 Procedure:

5.1 Calibration & Qualification of Equipment

All the equipment which will be used for analysis must be calibrated and
qualified prior the start of Verification process. The detail will be provided in
the Table 1.

Table 1 Calibration and Qualification of Equipment

Calibration/ Next Calibration/

Sr. Verified by
Equipment Model Origin Qualification Qualification date
# (Sign/date)
Date

5.2 Calibration of Glass Apparatus

The glass apparatus which will be used must be calibrated. The detail will be
provided in the Table 2.

Table 2 Calibration of Glassware

Glass Apparatus Apparatus I.D Origin Calibration Verified by

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Department: Page 5 of 11
Quality Assurance
Protocol No.: Revision No. 00
QA/PRT/PTH/082
Protocol for PT (HPLC)
Effective Date: Replaces:
Not Applicable
Doc. Ref. No.
Next Review Date:
QC/SOP/AQR/068A

Date (Sign/date)

5.3 Chemicals / Reagents / Buffers

The detail of the chemicals, reagents and buffers which will be used for will
be provided in the Table 3.

Table 3 Characteristics of Chemicals and Reagents/Buffers

Name of Chemicals/ Batch Number/Lot Manufacturer Verified by

Reagent/ Buffers No. Name (Sign/date)

5.4 Qualified Analysts Detail

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Quality Assurance
Protocol No.: Revision No. 00
QA/PRT/PTH/082
Protocol for PT (HPLC)
Effective Date: Replaces:
Not Applicable
Doc. Ref. No.
Next Review Date:
QC/SOP/AQR/068A

Analysts, who will be responsible for performing analysis of sample for PT

should be appropriately qualified and trained. The detail of the
corresponding qualified personnel will be provided in the Table 4.

Table 4 Qualification and Training Record of Personnel

Verified by
Analyst Joining Date Designation Training Date
(Sign/date)

5.5 Method of Analysis

General Directions

1. Preparation of Mobile phase

a) Dissolve 1.64g of anhydrous sodium acetate in 2L of water (Sol. A)

b) Transfer 1910mL of soln. A to a 2L volumetric flask, add 50mL of acetonitrile

and 40mL of tetrahydrofuran and mix.

c) Adjust to pH 4.5, mix, filter and degas.

2. Preparation of test solutions

a) Test solution 1: Transfer 40mg of caffeine sample 1 to a 200mL volumetric

flask and dissolve in about 50mL of mobile phase (sonicate if necessary),
dilute to volume with mobile phase and mix.

b) Test solution 2: Transfer 40mg of caffeine sample 2 to a 200mL volumetric

flask and dissolve in about 50mL of mobile phase (sonicate of necessary),
dilute to volume with mobile phase and mix.

3. Perform the liquid chromatography according to the USP caffeine monograph

related compounds, or the SOP for HPLC analysis of caffeine impurity analysis.

4. Identify which caffeine sample passes according to the caffeine monograph (NMT
0.1% impurities)

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Department: Page 7 of 11
Quality Assurance
Protocol No.: Revision No. 00
QA/PRT/PTH/082
Protocol for PT (HPLC)
Effective Date: Replaces:
Not Applicable
Doc. Ref. No.
Next Review Date:
QC/SOP/AQR/068A

Note: Identify which caffeine sample is passing (Data= 1 or 2)

6.0 Testing Plan and Result Evaluation

Testing Date Analyst Equipment Equipment Results

Name ID

7.0 PT report

___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________

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Department: Page 8 of 11
Quality Assurance
Protocol No.: Revision No. 00
QA/PRT/PTH/082
Protocol for PT (HPLC)
Effective Date: Replaces:
Not Applicable
Doc. Ref. No.
Next Review Date:
QC/SOP/AQR/068A

___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________

8.0 Deviation

Description of deviation:
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________

Justification for Acceptance:

___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________

Impact on operations, function and process:

___________________________________________________________
___________________________________________________________

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Department: Page 9 of 11
Quality Assurance
Protocol No.: Revision No. 00
QA/PRT/PTH/082
Protocol for PT (HPLC)
Effective Date: Replaces:
Not Applicable
Doc. Ref. No.
Next Review Date:
QC/SOP/AQR/068A

___________________________________________________________
___________________________________________________________

9.0 Change Control

Proposed
By
Sr. Change Control
Description of Change Control
No. Number
(Sign &
Date)

10.0 Documentation

___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________

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Department: Page 10 of 11
Quality Assurance
Protocol No.: Revision No. 00
QA/PRT/PTH/082
Protocol for PT (HPLC)
Effective Date: Replaces:
Not Applicable
Doc. Ref. No.
Next Review Date:
QC/SOP/AQR/068A

11.0 Summary of Results and Conclusion

___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________
___________________________________________________________

12.0 Abbreviation

SR. No. Terms/words/statement Meaning/description

s

1 QC Quality Control

2 QA Quality Assurance

3 O&C Operations and Compliance

4 PT Proficiency Testing

13.0 Post Approval

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Department: Page 11 of 11
Quality Assurance
Protocol No.: Revision No. 00
QA/PRT/PTH/082
Protocol for PT (HPLC)
Effective Date: Replaces:
Not Applicable
Doc. Ref. No.
Next Review Date:
QC/SOP/AQR/068A

The Proficiency testing activities has been carried out as per protocol and results
are reviewed and approved for implementation.

Reviewed By _____________________________ Date: _____________

Manager QC /Designee

Reviewed By _____________________________ Date: _____________

Chief Manager QC /Designee

Approved By _____________________________ Date: _____________

Manager QA (O&C)

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