REPORT FOR HOLD TIME STUDY OF DISPENSED RAW MATERIAL

Protocol No.: PRO/MIC/QC/002/2003 Location : Kandla Page No.: 1 of 11

REPORT ON
HOLD TIME STUDY

OF

DISPENSED RAW MATERIAL

Location Kandla

Ref. Protocol No. PRO/MIC/QC/002/2003

Technical Manufacturing Document T 302 (Q9) (01) 01

Reference No.

Report contains pages 11

 REPORT FOR HOLD TIME STUDY OF DISPENSED RAW MATERIAL

Protocol No.: PRO/MIC/QC/002/2003 Location : Kandla Page No.: 2 of 11

TABLE OF CONTENT

Sr.
Subject Page No.
No.
1.0 Report Approval Sheet 3
2.0 Objective 4
3.0 Scope 4
4.0 Validation Team 4
5.0 Responsibility 4
6.0 Procedure 5
7.0 Acceptance criteria 5
8.0 Annexure 1 6-10
9.0 Summary, Conclusion & Approval Report 11
 REPORT FOR HOLD TIME STUDY OF DISPENSED RAW MATERIAL

Protocol No.: PRO/MIC/QC/002/2003 Location : Kandla Page No.: 3 of 11

1.0 REPORT APPROVAL SHEET:

Prepared By Checked By Approved By

Signature

Name Miti Dave Pushpa Nair Pradeep Kumar

Date 23-10-2003 23-10-2003 23-10-2003
Department Microbiologist Quality Control Quality Assurance
Head Head
 REPORT FOR HOLD TIME STUDY OF DISPENSED RAW MATERIAL

Protocol No.: PRO/MIC/QC/002/2003 Location : Kandla Page No.: 4 of 11

2.0 OBJECTIVE :

The objective of this report is to establish the holding period for dispensed raw material
of a batch with respect to the quality of the raw material.

3.0 SCOPE :

The report describes the responsibility, procedure for hold time study of the dispensed
raw material, acceptance criteria, summary & approval report.

4.0 VALIDATION TEAM :

A representative from each of the following departments:

Microbiologist

Production Officer

I.P.Q.A Officer

5.0 RESPONSIBILITY :

Personnel
Microbiologist
Quality Control Head
Quality Assurance Head
Responsibility
To study the bio burden load in the product according to the
laid down procedure and to prepare the report for the batch
under study.
To check the report.
To review & approve the report.
 REPORT FOR HOLD TIME STUDY OF DISPENSED RAW MATERIAL

Protocol No.: PRO/MIC/QC/002/2003 Location : Kandla Page No.: 5 of 11

6.0 PROCEDURE :

1. Dispense the batch of Oral Suspension for hold time study of dispensed material.

2. Select the ingredient which is maximum susceptible towards the microbial growth for the
hold time study.
3. Collect samples of the selected ingredient for microbial analysis as per the sampling
plan.
Sampling Plan
Stage Identified Sample Quantity Frequency Tests to be
Sampling performed
Points
After Each 20g from each Every Day for study Microbial
dispensing Container container period of 8 days. Analysis
After Drying Each 20g from each -- Microbial
container container Analysis
4. Perform microbial analysis of the test samples as per SOP No. GLP/CQD/05/96/15/KDL
5. Record the results in Annexure 1.

7.0 ACCEPTANCE CRITERIA:

Microbial Limits :-

-- Total Bacterial Count : Not more than 1000 CFU/gm

-- Total Fungal Count : Not more than 100 CFU/gm
-- Pathogens ( E.coli, Salmonella typhi) : Absent
 REPORT FOR HOLD TIME STUDY OF DISPENSED RAW MATERIAL

Protocol No.: PRO/MIC/QC/002/2003 Location : Kandla Page No.: 6 of 11

ANNEXURE 1

Product under study : Amoxicillin 250 mg/5ml Oral suspension BP

Batch No. : Q93010Z
Raw Material : Sucrose Pharma Grade
A.R No. : 12300325
CONTAINER No. : 1
Date of Date of Total Total Pathogens
inoculation observation Bacterial Fungal
Count (TBC) Count (TFC)
Initial 10/10/03 15/10/03 30 CFU/g Less than 10 Absent
CFU/g
4th Holding Day 13/10/03 18/10/03 10 CFU/ g Less than 10 Absent
CFU/g
5th Holding Day 14/10/03 20/10/03 40 CFU/g Less than 10 Absent
CFU/g
6th Holding Day 15/10/03 20/10/03 50 CFU/g Less than 10 Absent
CFU/g
7th Holding Day 16/10/03 21/10/03 60 CFU/g Less than 10 Absent
CFU/g
8th Holding Day 17/10/03 22/10/03 80 CFU/g 10 CFU/g Absent
After Drying 17/10/03 22/10/03 10 CFU/g Less than 10 Absent
CFU/g

Microbial Limits :-

-- Total Bacterial Count : Not more than 1000 CFU/gm

-- Total Fungal Count : Not more than 100 CFU/gm
-- Pathogens ( E.coli, Salmonella typhi) : Absent

_____________ _____________
Microbiologist Q.C Executive
 REPORT FOR HOLD TIME STUDY OF DISPENSED RAW MATERIAL

Protocol No.: PRO/MIC/QC/002/2003 Location : Kandla Page No.: 7 of 11

Product under study : Amoxicillin 250 mg/5ml Oral suspension BP

Batch No. : Q93010Z
Raw Material : Sucrose Pharma Grade
A.R No. : 12300325
CONTAINER No. : 2
Date of Date of Total Total Pathogens
inoculation observation Bacterial Fungal
Count (TBC) Count (TFC)
Initial 10/10/03 15/10/03 20 CFU/g Less than 10 Absent
CFU/g
4th Holding Day 13/10/03 18/10/03 10 CFU/ g Less than 10 Absent
CFU/g
5th Holding Day 14/10/03 20/10/03 90 CFU/g Less than 10 Absent
CFU/g
6th Holding Day 15/10/03 20/10/03 120 CFU/g Less than 10 Absent
CFU/g
7th Holding Day 16/10/03 21/10/03 80 CFU/g Less than 10 Absent
CFU/g
8th Holding Day 17/10/03 22/10/03 80 CFU/g Lees than 10 Absent
CFU/g
After Drying 17/10/03 22/10/03 10 CFU/g Less than 10 Absent
CFU/g

Microbial Limits :-

-- Total Bacterial Count : Not more than 1000 CFU/gm

-- Total Fungal Count : Not more than 100 CFU/gm
-- Pathogens ( E.coli, Salmonella typhi) : Absent

_____________ _____________
Microbiologist Q.C Executive
 REPORT FOR HOLD TIME STUDY OF DISPENSED RAW MATERIAL

Protocol No.: PRO/MIC/QC/002/2003 Location : Kandla Page No.: 8 of 11

Product under study : Amoxicillin 250 mg/5ml Oral suspension BP

Batch No. : Q93010Z
Raw Material : Sucrose Pharma Grade
A.R No. : 12300325
CONTAINER No. : 3
Date of Date of Total Total Pathogens
inoculation observation Bacterial Fungal
Count (TBC) Count (TFC)
Initial 10/10/03 15/10/03 40 CFU/g Less than 10 Absent
CFU/g
4th Holding Day 13/10/03 18/10/03 20 CFU/ g Less than 10 Absent
CFU/g
5th Holding Day 14/10/03 20/10/03 60 CFU/g Less than 10 Absent
CFU/g
6th Holding Day 15/10/03 20/10/03 80 CFU/g Less than 10 Absent
CFU/g
7th Holding Day 16/10/03 21/10/03 40 CFU/g Less than 10 Absent
CFU/g
8th Holding Day 17/10/03 22/10/03 150 CFU/g Less than 10 Absent
CFU/g
After Drying 17/10/03 22/10/03 20 CFU/g Less than 10 Absent
CFU/g

Microbial Limits :-

-- Total Bacterial Count : Not more than 1000 CFU/gm

-- Total Fungal Count : Not more than 100 CFU/gm
-- Pathogens ( E.coli, Salmonella typhi) : Absent

_____________ _____________
Microbiologist Q.C Executive
 REPORT FOR HOLD TIME STUDY OF DISPENSED RAW MATERIAL

Protocol No.: PRO/MIC/QC/002/2003 Location : Kandla Page No.: 9 of 11

Product under study : Amoxicillin 250 mg/5ml Oral suspension BP

Batch No. : Q93010Z
Raw Material : Sucrose Pharma Grade BP
A.R No. : 12300325
CONTAINER No. : 4
Date of Date of Total Total Pathogens
inoculation observation Bacterial Fungal
Count (TBC) Count (TFC)
Initial 10/10/03 15/10/03 40 CFU/g Less than 10 Absent
CFU/g
4th Holding Day 13/10/03 18/10/03 10 CFU/ g Less than 10 Absent
CFU/g
5th Holding Day 14/10/03 20/10/03 100 CFU/g Less than 10 Absent
CFU/g
6th Holding Day 15/10/03 20/10/03 50 CFU/g Less than 10 Absent
CFU/g
7th Holding Day 16/10/03 21/10/03 80 CFU/g Less than 10 Absent
CFU/g
8th Holding Day 17/10/03 22/10/03 90 CFU/g Less than 10 Absent
CFU/g
After Drying 17/10/03 22/10/03 Less than 10 Less than 10 Absent
CFU/g CFU/g

Microbial Limits :-

-- Total Bacterial Count : Not more than 1000 CFU/gm

-- Total Fungal Count : Not more than 100 CFU/gm
-- Pathogens ( E.coli, Salmonella typhi) : Absent

_____________ _____________
Microbiologist Q.C Executive
 REPORT FOR HOLD TIME STUDY OF DISPENSED RAW MATERIAL

Protocol No.: PRO/MIC/QC/002/2003 Location : Kandla Page No.: 10 of 11

Product under study : Amoxicillin 250 mg/5ml Oral suspension BP

Batch No. : Q93010Z
Raw Material : Sucrose Pharma grade BP
A.R No. : 12300325
CONTAINER No. : 5
Date of Date of Total Total Pathogens
inoculation observation Bacterial Fungal
Count (TBC) Count (TFC)
Initial 10/10/03 15/10/03 30 CFU/g Less than 10 Absent
CFU/g
4th Holding Day 13/10/03 18/10/03 20 CFU/ g Less than 10 Absent
CFU/g
5th Holding Day 14/10/03 20/10/03 50 CFU/g 10 CFU/g Absent
6th Holding Day 15/10/03 20/10/03 50 CFU/g 10 CFU/g Absent
7th Holding Day 16/10/03 21/10/03 50 CFU/g 30 CFU/g Absent
8th Holding Day 17/10/03 22/10/03 70 CFU/g 10 CFU/g Absent
After Drying 17/10/03 22/10/03 30 CFU/g Less than 10 Absent
CFU/g

Microbial Limits :-

-- Total Bacterial Count : Not more than 1000 CFU/gm

-- Total Fungal Count : Not more than 100 CFU/gm
-- Pathogens ( E.coli, Salmonella typhi) : Absent

_____________ _____________
Microbiologist Q.C Executive

8. SUMMARY, CONCLUSION & APPROVAL REPORT :

 REPORT FOR HOLD TIME STUDY OF DISPENSED RAW MATERIAL

Protocol No.: PRO/MIC/QC/002/2003 Location : Kandla Page No.: 11 of 11

SUMMARY :

The study for establishing the hold time period for dispensed raw material was carried out in
accordance with the procedure in the protocol.

There was no considerable increase in the bacterial & fungal count of sucrose in first three
days of the study.

There was an increase in the bacterial & fungal counts of sucrose after the fourth day of the
study, which however were observed within the acceptable limits.

There was considerable decrease in the microbial count of sucrose analyzed after drying it
on the eighth day of the study.

CONCLUSION :

From the study carried out, hold time period of seven days for dispensed raw material has
been established.

Checked By Approved By

Pushpa Nair Pradeep Kumar

Quality Control Head Quality Assurance Head