PHARMADEVILS

QUALITY ASSURANCE DEPARTMENT

HOLD TIME STUDY PROTOCOL CUM REPORT OF RAW MATERIAL

HOLD TIME STUDY PROTOCOL CUM REPORT OF

RAW MATERIAL
 PHARMADEVILS
QUALITY ASSURANCE DEPARTMENT

HOLD TIME STUDY PROTOCOL CUM REPORT OF RAW MATERIAL

CONTENTS
S.No. Title of sections Page No.
1 Pre-approval Protocol 3

2 Objective 4

3 Scope 4

4 Responsibility 4

5 Validation Team training details 5

6 Verification of Instruments for calibration 5

7 Reference of standard operating procedure/ Documents 6

8 Validated Analytical Methods of intermediates for estimation of 6

activeingredient
9 Raw Material storage condition 6

10 Hold time study Procedure 6-7

11 Sampling size, plan, frequency and Result/ observation 7-10

12 Acceptance Criteria 11

13 Details of deviation/ Non- compliance/ OOS 11

14 Risk management study 11

15 Summary of the study activity 12

16 Recommendation 12

17 Attachments 13-15

18 Abbreviations 16

19 Review and Post approval 17

 PHARMADEVILS
QUALITY ASSURANCE DEPARTMENT

HOLD TIME STUDY PROTOCOL CUM REPORT OF RAW MATERIAL

1.0 Pre-approval Protocol:

This document has been developed and the individuals listed below have reviewed the
document and agree with its content and with their signature grant approval for its execution.

Functional area Name Designation Signature Date

PREPARED BY

Validation QA

REVIEWED BY

Production Head

Quality Control Head

Warehouse Head

Engineering Head

Quality Assurance

APPROVED BY

QA Head

Plant Head
 PHARMADEVILS
QUALITY ASSURANCE DEPARTMENT

HOLD TIME STUDY PROTOCOL CUM REPORT OF RAW MATERIAL

2.0 OBJECTIVE:
Objective of hold time study is to establish the storage time of raw material with documented evidence.

3.0 SCOPE:
This protocol is applicable for hold time study of raw material used in manufacturing activity.

4.0 RESPONSIBILITY:
QUALITY ASSURANCE:
- Preparation, Execution & reviewing the protocol.
- Collection of the samples as specified in protocol.
- Reviewing the QC result and draw conclusion.
QUALITY CONTROL:
- Reviewing of hold time study protocol.
- Analyzing the hold time study samples as per this protocol and reporting the result.
PRODUCTION:
- Reviewing of hold time study protocol.
- To intimate the collection of sample of hold time study after completion of dispensing.
WAREHOUSE:
- Reviewing of hold time study protocol.
- To dispense the raw material required for hold time study.
ENGINEERING:
- Reviewing of hold time study protocol.
- Maintaining the required environmental condition of the storage area.
 PHARMADEVILS
QUALITY ASSURANCE DEPARTMENT

HOLD TIME STUDY PROTOCOL CUM REPORT OF RAW MATERIAL

5.0 VALIDATION TEAM TRAINING DETAILS:

Availability of training status and training record of all personnel involved in the validation /
assessment exercise should be recorded.

DEPARTMENT NAME TRAINING STATUS SIGNATURE

Quality Assurance

Quality Control

Production

Warehouse

Engineering

6.0 VERIFICATION OF INSTRUMENTS FOR CALIBRATION:

Calibration Calibration Checked by
S.No. Instrument Name Instrument Code
done on due on Sign/Date
1 Weighing Balance
 PHARMADEVILS
QUALITY ASSURANCE DEPARTMENT

HOLD TIME STUDY PROTOCOL CUM REPORT OF RAW MATERIAL

7.0 REFERENCE OF STANDARD OPERATING PROCEDURE/ DOCUMENTS:

S.No. SOP/ Document Name SOP/ Doc. No.
1 SOP for Hold time study of products at different stages
SOP for Microbiological analysis of raw material, finish product and
2
Stability samples
3 SOP for Incident Reporting and Investigation

4 SOP for Deviation

5 SOP for Quality Risk Management

6 SOP for Handling of out of specification (OOS) results

8.0 Reference Analytical Method Validation protocol number/ QC Specification no. to be recorded.

Test Analytical Method Validation Protocol Checked by

No. / QC specification number (Sign/ Date)

Microbiological analysis

9.0 Raw Material Storage Condition:

9.1 Store the sample dispensed raw material in fresh polybag at a temperature NMT 250C and
Relative humidity NMT 60%.
9.2 Store the sample of dispensed raw material (moisture sensitive) in fresh polybag at a temperature
0
NMT 25 C and Relative humidity NMT 40%.
9.2 Store the light sensitive materials in black polybag.

10.0 HOLD TIME STUDY PROCEDURE:

10.1 Selection of Raw material: Raw material shall be selected based on its nature and scientific
rationale.

10.2 Dispensed Raw Material Details:

The raw materials used in the manufacturing of the batches selected for Hold Time Study shall be
tested, analyzed and approved before use in the production as per their respective approved
specifications. Details of the raw material shall be recorded in the report as shown below in the table.
 PHARMADEVILS
QUALITY ASSURANCE DEPARTMENT

HOLD TIME STUDY PROTOCOL CUM REPORT OF RAW MATERIAL

10.2 SAMPLING SIZE, PLAN AND FREQUENCY:

Hold time study samples of raw materials shall be collected as per below mentioned quantity:
Sampling Plan for Dispensed Raw Material Hold Time Study
S.No. Storage Time Test Parameters Quantity of Acceptance
Sample Criteria
1 Initial (0) a) Appearance 20 gm for every
b) Microbial test storage time
QC Test
2 5th Day a) Appearance
b) Microbial test Total quantity:
3 10th Day a) Appearance
b) Microbial test 60 gm

11.0 Result/ Observation:

Test Parameters of Raw Material

Raw Material Details Time Appearance Microbial Test

(Day)
Vendor Interval
Name Item Code A.R. No.
Name
Initial (0)

5th Day

10th Day

Initial (0)

5th Day

10th Day

Initial (0)

5th Day

10th Day

Initial (0)

5th Day

10th Day
 PHARMADEVILS
QUALITY ASSURANCE DEPARTMENT

HOLD TIME STUDY PROTOCOL CUM REPORT OF RAW MATERIAL

Test Parameters of Raw Material

Raw Material Details Time Appearance Microbial Test

(Day)
Vendor Interval
Name Item Code A.R. No.
Name
Initial (0)

5th Day

10th Day

Initial (0)

5th Day

10th Day

Initial (0)

5th Day

10th Day

Initial (0)

5th Day

10th Day

Initial (0)

5th Day

10th Day

Initial (0)

5th Day

10th Day

Initial (0)
 PHARMADEVILS
QUALITY ASSURANCE DEPARTMENT

HOLD TIME STUDY PROTOCOL CUM REPORT OF RAW MATERIAL

Test Parameters of Raw Material

Raw Material Details Time Appearance Microbial Test

(Day)
Vendor Interval
Name Item Code A.R. No.
Name
Initial (0)

5th Day

10th Day

5th Day

10th Day

Initial (0)

5th Day

10th Day

Initial (0)

5th Day

10th Day

Initial (0)

5th Day

10th Day

Initial (0)

5th Day

10th Day

Initial (0)

5th Day
 PHARMADEVILS
QUALITY ASSURANCE DEPARTMENT

HOLD TIME STUDY PROTOCOL CUM REPORT OF RAW MATERIAL

Test Parameters of Raw Material

Raw Material Details Time Appearance Microbial Test

(Day)
Vendor Interval
Name Item Code A.R. No.
Name
Initial (0)

5th Day

10th Day

10th Day

As per QC Specification No.:

Limit _______________________________

_______________________________

12.0 Acceptance criteria:

Acceptance criteria for each raw material shall be as per the respective Quality Control specification for
individual raw material.

13.0 Details of Deviation / Non Compliance / OOS:

14.0 Risk management study (if any):

15.0 Summary of the study activity:

16.0 Recommendation:
 PHARMADEVILS
QUALITY ASSURANCE DEPARTMENT

HOLD TIME STUDY PROTOCOL CUM REPORT OF RAW MATERIAL

17.0 Attachments:

Attachment No. Title of Attachment

 PHARMADEVILS
QUALITY ASSURANCE DEPARTMENT

HOLD TIME STUDY PROTOCOL CUM REPORT OF RAW MATERIAL

18.0 Abbreviations:
SOP: Standard operating procedure
OOS: Out of specification
QC: Quality Control
QA: Quality Assurance
No.: Number
Qty.: Quantity
Sr. No.: Serial number
g: Gram
 PHARMADEVILS
QUALITY ASSURANCE DEPARTMENT

HOLD TIME STUDY PROTOCOL CUM REPORT OF RAW MATERIAL

19.0 Review and Post approval:

Functional area Name Designation Signature Date

PERFORMED BY

Validation QA

Quality Control

Production

Warehouse

Engineering

Quality Assurance

APPROVED BY

QA Head

Plant Head