ANALYTICAL METHOD VALIDATION REPORT PROTOCOL No.

:
FOR
PRE & PROBIOTIC CAPSULES

PHARMA DEVILS

ANALYTICAL METHOD

VALIDATION REPORT

FOR

PRE & PROBIOTIC CAPSULES

SUPERSEDE REPORT No.

DATE OF VALIDATION

VALIDATION BATCH No.

VALIDATION BATCH SIZE

 ANALYTICAL METHOD VALIDATION REPORT PROTOCOL No.:
FOR
PRE & PROBIOTIC CAPSULES

PHARMA DEVILS

REPORT CONTENTS

S.No. TITLE PAGE No.

1.0 PRE APPROVAL 3
2.0 OBJECTIVE 4
3.0 SCOPE 4
4.0 RESPONSIBILITY 4
5.0 TRAINING RECORDS 5
6.0 INSTRUMENT CALIBRATION VERIFICATION 6
7.0 MATERIALS & INSTRUMENTS DETAILS 7-8
8.0 SPECIFICITY 9
9.0 METHOD PRECISION 10
10.0 INTERMEDIATE PRECISION 11
11.0 LINEARITY & RANGE 13
12.0 ACCURACY/RECOVERY 14
13.0 SUMMARIZED VALIDATION REPORT 18
14.0 ATTACHMENTS 19
15.0 DEVIATION 19
16.0 CONCLUSION 19
17.0 RECOMMENDATION 19
18.0 ABBREVIATIONS 20
19.0 POST APPROVAL 21
 ANALYTICAL METHOD VALIDATION REPORT PROTOCOL No.:
FOR
PRE & PROBIOTIC CAPSULES

PHARMA DEVILS

1.0 REPORT PRE APPROVAL:

INITIATED BY:

DESIGNATION NAME SIGNATURE DATE

OFFICER/EXECUTIVE
(QUALITY CONTROL)

REVIEWED BY:

DESIGNATION NAME SIGNATURE DATE

HEAD
(QUALITY CONTROL)
MANAGER
(QUALITY ASSURANCE)

APPROVED BY:

DESIGNATION NAME SIGNATURE DATE

HEAD
(QUALITY ASSURANCE)
 ANALYTICAL METHOD VALIDATION REPORT PROTOCOL No.:
FOR
PRE & PROBIOTIC CAPSULES

PHARMA DEVILS

2.0 OBJECTIVE:
To compile the data of Analytical Method Validation carried out as per Analytical Method Validation
Protocol (Protocol No. …………….) the Assay test of Pre & Probiotic Capsules is validated and suitable
for testing samples of commercial batches.

3.0 SCOPE:
This Analytical Method Validation Report provides information after compilation of Analytical Method
Validation Data that the applicable for Assay Test of Pre & Probiotic Capsules for Accuracy, Precision,
Specificity, Linearity & Range, Robustness test methods is suitable for testing of samples of commercial
batches.

4.0 RESPONSIBILITY:

The validation group, comprising of a representative from each of the following departments, shall be
responsible for the overall compliance of this report:

DEPARTMENTS RESPONSIBILITIES
 Preparation and Review of Analytical Method Validation Report.
 Execution of Analytical Method Validation Activity as per Protocol
Quality Control
and to compile the data in Analytical Method Validation Report.
 Preparation of Analysis Report and submission to Quality Assurance.

 Preparation, Review and Approval of Analytical Method Validation

Report based on Analytical Method Validation Protocol and Analytical
Quality Assurance Method Validation Data.
 Co-ordination with QC to carryout Analytical Method Validation.
 Monitoring of Analytical Method Validation Activity.
 ANALYTICAL METHOD VALIDATION REPORT PROTOCOL No.:
FOR
PRE & PROBIOTIC CAPSULES

PHARMA DEVILS

ANNEXURE-I

5.0 TRAINING RECORDS:

S.No. Name of Trainee Department Designation Acceptance Signature

Criteria of Trainee

All personnel
involved in
execution of the
protocol shall be
trained in the
required
procedure and
shall be
documented

Name of the Trainer: ……………………….

Sign & Date:

Inference:
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Reviewed By:
Sign & Date…………………………
 ANALYTICAL METHOD VALIDATION REPORT PROTOCOL No.:
FOR
PRE & PROBIOTIC CAPSULES

PHARMA DEVILS

ANNEXURE-II
6.0 INSTRUMENT CALIBRATION VERIFICATION:

S.No. Instrument Name Instrument ID Calibration Calibration Calibration Checked By

No. Status Date Due Date (Sign & Date)
QC

Inference:
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Reviewed By:
Sign & Date…………………………
 ANALYTICAL METHOD VALIDATION REPORT PROTOCOL No.:
FOR
PRE & PROBIOTIC CAPSULES

PHARMA DEVILS

ANNEXURE-III

7.0 MATERIALS AND INSTRUMENTS DETAILS:

7.1 PRODUCT DETAILS:

 Product Name :

 Batch No. :

 Batch Size :

 Mfg. Date :

 STP No. :

DETAILS OF MATERIALS USED:

S.No. Name of Media/ Chemical Manufacturer Lot No./Batch No. Grade

 ANALYTICAL METHOD VALIDATION REPORT PROTOCOL No.:
FOR
PRE & PROBIOTIC CAPSULES

PHARMA DEVILS

DETAILS OF INSTRUMENTS/EQUIPMENT USED:

S.No. Instrument Make Model Functional & Identification No. Condition

Name Performance
requirements

DETAILS OF FILTER/CENTIRFUGE USED FOR VALIDATION:

S.No. Name Size B. No./Lot No. Make

Checked By: Verified By:

Officer/Executive-QC Manager-QC
Sign & Date……………………….. Sign & Date……………….

Inference:
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Sign & Date…………………
 ANALYTICAL METHOD VALIDATION REPORT PROTOCOL No.:
FOR
PRE & PROBIOTIC CAPSULES

PHARMA DEVILS

ANNEXURE-IV
8.0 SPECIFICITY:

Plate No. Content of Content of Clostridia Content of Bacillus Content of Lactic

Streptococcus faecalis butyricum mesentricus acid bacillus
(In millions) (In millions) (In millions) (In millions)
1.

2.

3.

Acceptance Criteria: There should be no interference by the blank and placebo in the determination of the
analyte

Analyzed By: Verified By:

Officer/Executive-QC Manager-QC
Sign & Date……………………….. Sign & Date……………….

Inference:
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Reviewed By:
Sign & Date…………………
 ANALYTICAL METHOD VALIDATION REPORT PROTOCOL No.:
FOR
PRE & PROBIOTIC CAPSULES

PHARMA DEVILS

ANNEXURE-V

9.0 METHOD PRECISION:

S.No. Content of Streptococcus Content of Content of Content of

faecalis Clostridia butyricum Bacillus mesentricus Lactic acid bacillus
(in millions) (in millions) (in millions) (in millions)
1.

2.

3.

4.

5.

6.

Mean

STD.
DEV.
%RSD

Acceptance Criteria: RSD should not be more than 10.0%

Analyzed By: Verified By:

Officer/Executive-QC Manager-QC
Sign & Date………………… Sign & Date…………………

Inference:
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Reviewed By:
Sign & Date…………………
 ANALYTICAL METHOD VALIDATION REPORT PROTOCOL No.:
FOR
PRE & PROBIOTIC CAPSULES

PHARMA DEVILS

ANNEXURE VI
10.0 INTERMEDIATE PRECISION:
PARTICULARS RESULTS
ANALYST-I ANALYST-II
Date of Analysis
Analyst Name
Contents

Lactic acid bacillus

Lactic acid bacillus

Bacillus mesentricus

Bacillus mesentricus
faecalis

faecalis
Streptococcus

Streptococcus
Clostridia butyricum

Clostridia butyricum
(in millions)

1.
2.
3.
4.
5.
6.
Average
STD
RSD
Relative difference
Acceptance Criteria: RSD of assay results obtained for six preparations by second analyst should NMT 10%. The
relative difference between the average results obtained by both analysts should NMT 10%.

Analyzed By: Verified By:

Officer/Executive-QC Manager-QC
Sign & Date………………… Sign & Date……………………

Inference:
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Reviewed By:
Sign & Date……………………
 ANALYTICAL METHOD VALIDATION REPORT PROTOCOL No.:
FOR
PRE & PROBIOTIC CAPSULES

PHARMA DEVILS

ANNEXURE-VII

11.0 LINEARITY & RANGE:

S.No. Concentration Contents Contents

(in millions) (in millions)

Streptococcus

Streptococcus
mesentricus

mesentricus
butyricum

butyricum
Clostridia

Clostridia
Lactic acid

Lactic acid
faecalis

faecalis
bacillus

bacillus
Bacillus

Bacillus
1. 60%

2. 80%

3. 100%

4. 120%

5. 140%

Slope
Intercept
Coefficient of Variance
Acceptance Criteria: Plot of concentration vs No. of colony forming units shall be linear coefficient of
variance shall be close to 1.0

Analyzed By: Verified By:

Officer/Executive-QC Manager-QC
Sign & Date…………………. Sign & Date………………….

Inference:
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Reviewed By:
Sign & Date…………………
 ANALYTICAL METHOD VALIDATION REPORT PROTOCOL No.:
FOR
PRE & PROBIOTIC CAPSULES

PHARMA DEVILS

ANNEXURE-VIII
12.0 ACCURACY/RECOVERY:

12.1 Content of Streptococcus faecalis (in millions)

S.No. S. No. Known amount added in placebo Recovery % Recovery
(wt.in mg) Individual Average
Value Value
1. 1 80 % added of
2 Label Claim

3
2. 1 100 % added of
2 Label Claim

3
3. 1 120 % added of
2 Label Claim
3

Acceptance Criteria: Should be between 90.0% and 110.0%

Analyzed By: Verified By:

Officer/Executive-QC Manager-QC
Sign & Date……………………. Sign & Date……………………..

Inference:
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Reviewed By:
Sign & Date…………………..…
 ANALYTICAL METHOD VALIDATION REPORT PROTOCOL No.:
FOR
PRE & PROBIOTIC CAPSULES

PHARMA DEVILS

12.2 Content of Clostridia butyricum (in millions)

S. No. S. No. Known amount added in placebo Recovery % Recovery
(wt.in mg) Individual Average
Value Value
1. 1 80 % added of
2 Label Claim

3
2. 1 100 % added of
2 Label Claim

3
3. 1 120 % added of
2 Label Claim
3

Acceptance Criteria: Should be between 90.0% and 110.0%

Analyzed By: Verified By:

Officer/Executive-QC Manager-QC
Sign & Date……………………. Sign & Date……………………

Inference:
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Reviewed By:
Sign & Date……………………
 ANALYTICAL METHOD VALIDATION REPORT PROTOCOL No.:
FOR
PRE & PROBIOTIC CAPSULES

PHARMA DEVILS

12.3 Content of Bacillus mesentricus (in millions)

S.No. S.No. Known amount added in placebo Recovery % Recovery

(wt.in mg) Individual Average
Value Value
1. 1 80 % added of
2 Label Claim

3
2. 1 100 % added of
2 Label Claim

3
3. 1 120 % added of
2 Label Claim
3

Acceptance Criteria: Should be between 90.0% and 110.0%

Checked By: Verified By:

Officer/Executive-QC Manager-QC
Sign & Date………………….. Sign & Date………………….

Inference:
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Reviewed By:
Sign & Date…………………
 ANALYTICAL METHOD VALIDATION REPORT PROTOCOL No.:
FOR
PRE & PROBIOTIC CAPSULES

PHARMA DEVILS

12.4 Content of Lactic acid bacillus (in millions):

S.No. S.No. Known amount added in placebo Recovery % Recovery
(wt.in mg) Individual Average
Value Value
1. 1 80 % added of
2 Label Claim

3
2. 1 100 % added of
2 Label Claim

3
3. 1 120 % added of
2 Label Claim
3

Acceptance Criteria: Should be between 90.0% and 110.0%

Analyzed By: Verified By:

Officer/Executive-QC Manager-QC
Sign & Date……………………. Sign & Date…………………….

Inference:
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Reviewed By:
Sign & Date……………….……
 ANALYTICAL METHOD VALIDATION REPORT PROTOCOL No.:
FOR
PRE & PROBIOTIC CAPSULES

PHARMA DEVILS

ANNEXURE-IX

13.0 SUMMARIZED VALIDATION REPORT:

S.No. Validation Acceptance criteria Observation

Parameters
1. Specificity There should be no growth observed in
Placebo
2. Precision
Method Precision RSD: Not more than 10.0%
Intermediate RSD: Not more than 10.0%
precision
Analyst I
Analysis II
Relative difference
3. Linearity Plot of concentration vs. No. of colony
forming units shall be linear coefficient of
variance shall be close to 1.0
4. Accuracy 80% Recovery: Between 90.0% and 110.0%
(Recovery)
Llll 100%
120%

Checked By: Verified By:

Officer/Executive-QC Manager-QC
Sign & Date……………………. Sign & Date…………………….

Inference:
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Reviewed By:
Sign & Date……………………
 ANALYTICAL METHOD VALIDATION REPORT PROTOCOL No.:
FOR
PRE & PROBIOTIC CAPSULES

PHARMA DEVILS

14.0 ATTACHMENTS:
1. Records for all critical parameters with graphical representation where applicable.
2. Raw data generated during the execution of this protocol.

15.0 DEVIATION (IF ANY):

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16.0 CONCLUSION:
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 ANALYTICAL METHOD VALIDATION REPORT PROTOCOL No.:
FOR
PRE & PROBIOTIC CAPSULES

PHARMA DEVILS

17.0 RECOMMENDATION:
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 ANALYTICAL METHOD VALIDATION REPORT PROTOCOL No.:
FOR
PRE & PROBIOTIC CAPSULES

PHARMA DEVILS

18.0 ABBREVIATIONS:
OD : Oral Dosage
Sr. : Senior
Pvt. : Private
Ltd. : Limited
QA : Quality Assurance
cGMP : Current Good Manufacturing Practices
FDA : Food & Drug Administration
LAF : Laminar Air Flow
pH : Potential of Hydrogen
ml : Milliliter
NaCl : Sodium Chloride
AR : Analytical Grade
Gm : Gram
°C : Degree Centigrade
lbs : Pound
cfu : Colony Forming Unit
Wt. : Weight
CO2 : Carbon Dioxide
RSD : Relative Standard Deviation
ICH : International Conference On Harmonization
 ANALYTICAL METHOD VALIDATION REPORT PROTOCOL No.:
FOR
PRE & PROBIOTIC CAPSULES

PHARMA DEVILS

19.0 REPORT POST APPROVAL:

Signing of this report indicates that the Analytical Method Validation for Assay Test of Pre & Probiotic
capsules has been completed as per approved Protocol.

INITIATED BY:

DESIGNATION NAME SIGNATURE DATE

OFFICER/EXECUTIVE
(QUALITY CONTROL)

REVIEWED BY:

DESIGNATION NAME SIGNATURE DATE

HEAD
(QUALITY CONTROL)
MANAGER
(QUALITY ASSURANCE)

APPROVED BY:

DESIGNATION NAME SIGNATURE DATE

HEAD
(QUALITY ASSURANCE)