Analytical Method Validation - Activated Charcoal 300MG Capsule SS

NATURAL WELLNESS BIOTECH (M) SDN BHD
ANALYTICAL METHOD VALIDATION REPORT

ACTIVATED CHARCOAL CAPSULE 300 MG
Prepared by: Nurfarahin Binti Mohd Kassim Date: 11/12/2023
Reviewed by: Ummi Umairah Binti Mohad Sukor Date: 11/12/2023
Document No.:
Page: 01 of 13 Revision No.: 01 Effective Date: 11/12/2023
NW/MV/22/P/002
CONTENTS PAGES
1. APPROVAL 2
2. OBJECTIVE 3
3. SCOPE 3
4. ANALYTICAL TESTING PROCEDURES 3
5. ANALYTICAL METHOD VALIDATION FOR UNIFORMITY OF 4
WEIGHT
6. ANALYTICAL METHOD VALIDATION FOR DISINTEGRATION 9
TIME
7. CONCLUSION 13
8. REFERENCES 14
9. REVISION HISTORY 14

Document No.:
NW/MV/22/P/002
1. APPROVAL
The following approvals indicate that this Analytical Method Validation (AMV) Report
has been reviewed and approved.
Responsible Person Name Signature Date
Prepared by:
NURFARAHIN BINTI
Quality Executive
MOHD KASSIM
Reviewed by:
Research and Development

UMMI UMAIRAH BINTI
Executive
MOHAD SUKOR
Approved by:
Quality Executive NUR EZZATUL ALYA

BINTI ANUAR

Document No.:
NW/MV/22/P/002
2. OBJECTIVE
The method validation objective is to validate the testing procedure for solid as per
compendia - Drug Registration Guidance Document (DRGD), National
Pharmaceutical Regulatory Agency determination for NW Activated Charcoal Capsule
300 mg. This is to ensure that the procedure used for NW Activated Charcoal Capsule
300 mg testing is acceptable in terms of specificity and precision.
3. SCOPE
The validated method is applicable to bulk sample, finished product and stability
product testing used by NATURAL WELLNESS BIOTECH (M) SDN BHD for NW
Activated Charcoal Capsule 300 mg for the registered pack size.
4. ANALYTICAL TESTING PROCEDURE
Refer as per attachment:
NW/QC/APFP/044: ANALYTICAL PROTOCOL ACTIVATED CHARCOAL

CAPSULE 300 MG

Document No.:
NW/MV/22/P/002
5. ANALYTICAL METHOD VALIDATION FOR UNIFORMITY OF WEIGHT
5.1 Specificity
5.1.1 Method Specificity
5.1.1.1 Weigh 20 capsules individually using weighing balance.
5.1.1.2 Individual weight of the capsule to be within the limit of 90 – 110% of the
average weight. (383 mg ± 10.00%)
5.1.1.3 Acceptance criteria
5.1.1.3.1 The deviation of the volume (in mL) of titrant used is not
more than 2% in terms of standard and solution sample,
respectively.
5.1.2 Report of Specificity for Uniformity of Weight
Table 1: Specificity of Uniformity of weight of the sample
No Weight (mg) No Weight (mg)
1 398.2 11 401.5
2 400.8 12 402.9
3 398.2 13 413.1
4 397.4 14 398.5
5 401.7 15 403.2
6 410.2 16 409.5
7 395.6 17 400.1
8 397.3 18 397.0
9 410.5 19 390.0
10 396.1 20 399.5
Average 401.06
STD 5.6
RSD 1.45%

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5.2 Precision
5.2.1 Method Precision

5.2.1.1 Weigh 20 capsules individually using weighing balance.
(Note: 6 (six) sample preparations at 100% test concentration)
5.2.1.2 Individual weight of the capsule to be within the limit of 90 – 110% of the
average weight. (400.00 mg ± 10.00%)
5.2.1.3 Calculate the deviation of replicate titrations and assay contents (in mL/g).

5.2.1.4.1 The RSD of the uniformity of weight is not more than 2%
in all 20 samples.
5.2.1.4.2 The uniformity of weight result in NW Activated Charcoal
Capsule 300 mg is not more than or not less than 10%
from the target weight.

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NW/MV/22/P/002
5.2.2 Report of Precision of for Uniformity of Weight
5.2.3
Table 2: Precision of Uniformity of weight of the sample
No Weight (mg) No Weight (mg)
1 396.5 11 402.0
2 400.9 12 400.7
3 399.4 13 407.0
4 402.7 14 400.2
5 401.5 15 405.0
6 420.6 16 399.9
7 398.7 17 407.5
8 400.0 18 400.9
9 408.2 19 412.2
10 400.1 20 407.4
Average 403.57
STD 5.62
RSD 1.39%
5.2.4 Intermediate Precision

5.2.4.1 Prepare 20 replicate of uniformity of weight by using finished
product and analyses by a different analyst and a same analyst on a
different day.

Document No.:
NW/MV/22/P/002
Table 3: Experimental design for variation study

Condition Analyst Day
Initial 1 1
Different analyst, day 2 2
5.2.4.2 Calculate the RSD and uniformity of weight (in mg).

5.2.4.3.1 The RSD of both result variations for both analyst and
days is not more than 2%.
5.2.5 Report of Intermediate Precision
Table 4: Intermediate Precision (Assay)
First Analyst (Day 1)
1 409.0 11 402.7
2 400.9 12 400.2
3 401.7 13 408.5
4 410.3 14 401.4
5 399.5 15 397.0
6 406.3 16 411.3
7 402.7 17 401.0
8 400.8 18 400.7
9 401.5 19 401.5
10 398.7 20 412.0

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NW/MV/22/P/002
Average 403.4
STD 4.5
RSD 1.11%
Second Analyst (Day 2)
1 410.2 11 411.5
2 408.0 12 412.3
3 401.2 13 414.0
4 399.5 14 406.5
5 400.5 15 400.7
6 399.9 16 412.0
7 412.5 17 400.0
8 400.2 18 399.6
9 399.7 19 407.2
10 400.9 20 410.1
Average 405.3
STD 5.53
RSD 1.36%

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6. ANALYTICAL METHOD VALIDATION FOR DISINTEGRATION TIME
6.1 Specificity
6.1.1 Method Specificity
6.1.1.1 Insert 6 sample into each hole.
6.1.1.2 Put back the disc according to its number back into the hole.
6.1.1.3 If temperatures reach 37°C, can Click [Start].
6.1.1.4 If the capsules solute in water, it indicates that the test finished and
passed within expected time (30 minutes).
6.1.1.5 Record the temperature and time of capsules disintegration shown in

disintegration test apparatus.

6.1.1.6.1 The deviation in the disintegration time is not more than 2%.
6.1.2 Report of Specificity for Disintegration time


Document No.:
NW/MV/22/P/002
Table 5: Specificity of Disintegration time of the sample
No Disintegration time (min)
1 9.55
2 9.80
3 9.43
4 9.50
5 9.60
6 9.24
Average 9.52
STD 0.19
RSD 1.95%
6.2 Precision
6.2.1 Method Precision
6.12.1.1 Insert 6 sample into each hole.
(Note: 6 (six) sample preparations at 100% test concentration)
6.2.1.2 Put back the disc according to its number back into the hole.
6.2.1.3 If temperatures reach 37°C, can Click [Start].
6.2.1.4 If the capsules solute in water, it indicates that the test finished and
passed within expected time (30 minutes).
6.2.1.5 Record the temperature and time of capsules disintegration shown in
disintegration test apparatus.
6.2.1.6 Calculate the deviation of replicate disintegration time (in minutes).
6.2.1.7.1 The deviation in the disintegration time is not more than 2%.
6.2.1.7.1 The RSD of the disintegration time is not more than 2% in all 6
samples.
6.2.1.7.1 The disintegration time result in NW Activated Charcoal
300 mg Capsule is not more than 30 minutes.

Document No.:
NW/MV/22/P/002
6.2.2 Report of Precision for Disintegration time
Table 6: Precision of Disintegration time of the sample
1 9.40
2 9.45
3 9.28
4 9.50
5 9.65
6 9.70
Average 9.50
STD 0.16
RSD 1.65%
6.2.3 Intermediate Precision

6.2.3.1 Prepare 6 replicate of disintegration time by using finished product
and analyses by a different analyst and a same analyst on a different
day.

Document No.:
NW/MV/22/P/002
Table 7: Experimental design for variation study

Condition Analyst Day
Initial 1 1
Different analyst, day 2 2
6.2.3.2 Calculate the RSD and disintegration time (in minute).

6.2.3.3.1 The RSD of both result variations for both analyst and days is
not more than 2%.
6.2.4 Report of Intermediate Precision

Table 8: Intermediate Precision (Assay)
First Analyst (Day 1)
1 9.30
2 9.58
3 9.60
4 9.22
5 9.50
6 9.44
Average 9.44
STD 0.15
RSD 1.62%

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NW/MV/22/P/002
Second Analyst (Day 2)
1 9.50
2 9.70
3 9.55
4 9.37
5 9.59
6 9.48
Average 9.53
STD 0.11
RSD 1.17%
7. CONCLUSION
The lab experiment shows that the analytical test procedures pass all the validation
acceptance criteria. The analytical procedure is considered validated and shall be use
for testing of bulk sample (intermediate product), finished product and stability studies
of NW Activated Charcoal Capsule 300 mg for the registered pack sizes.

Document No.:
NW/MV/22/P/002
8. REFERENCES
ICH Harmonized Tripartite Guideline (November 2005) – Validation of

Analytical Procedures: Text and Methodology Q2 (R1)
Drug Registration Guidance Document (DRGD), National

Pharmaceutical Regulatory Agency, Second Edition, September 2016,
revised July 2020
9. REVISION HISTORY
Revision No. Effective Date Change History

00 07/12/2022 New
01 11/12/2022 Updated

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NATURAL WELLNESS BIOTECH (M) SDN BHD

ANALYTICAL METHOD VALIDATION REPORT

4. ANALYTICAL TESTING PROCEDURES 3

5. ANALYTICAL METHOD VALIDATION FOR UNIFORMITY OF 4

6. ANALYTICAL METHOD VALIDATION FOR DISINTEGRATION 9

ANALYTICAL METHOD VALIDATION REPORT

Responsible Person Name Signature Date

Research and Development

Quality Executive NUR EZZATUL ALYA

ANALYTICAL METHOD VALIDATION REPORT

4. ANALYTICAL TESTING PROCEDURE

Refer as per attachment:

NW/QC/APFP/044: ANALYTICAL PROTOCOL ACTIVATED CHARCOAL

ANALYTICAL METHOD VALIDATION REPORT

5. ANALYTICAL METHOD VALIDATION FOR UNIFORMITY OF WEIGHT

Table 1: Specificity of Uniformity of weight of the sample

No Weight (mg) No Weight (mg)

ANALYTICAL METHOD VALIDATION REPORT

5.2.1 Method Precision

5.2.1.4 Acceptance criteria

ANALYTICAL METHOD VALIDATION REPORT

5.2.2 Report of Precision of for Uniformity of Weight

No Weight (mg) No Weight (mg)

5.2.4 Intermediate Precision

ANALYTICAL METHOD VALIDATION REPORT

Table 3: Experimental design for variation study

5.2.4.2 Calculate the RSD and uniformity of weight (in mg).

5.2.4.3 Acceptance criteria

ANALYTICAL METHOD VALIDATION REPORT

Second Analyst (Day 2)

ANALYTICAL METHOD VALIDATION REPORT

6. ANALYTICAL METHOD VALIDATION FOR DISINTEGRATION TIME

6.1.1.3 If temperatures reach 37°C, can Click [Start].

6.1.1.5 Record the temperature and time of capsules disintegration shown in

6.1.1.6 Acceptance criteria

6.1.2 Report of Specificity for Disintegration time

ANALYTICAL METHOD VALIDATION REPORT

Table 5: Specificity of Disintegration time of the sample

No Disintegration time (min)

ANALYTICAL METHOD VALIDATION REPORT

6.2.2 Report of Precision for Disintegration time

Table 6: Precision of Disintegration time of the sample

No Disintegration time (min)

6.2.3 Intermediate Precision

ANALYTICAL METHOD VALIDATION REPORT

Table 7: Experimental design for variation study

6.2.3.2 Calculate the RSD and disintegration time (in minute).

6.2.3.3 Acceptance criteria

6.2.4 Report of Intermediate Precision

No Disintegration time (min)

ANALYTICAL METHOD VALIDATION REPORT

Second Analyst (Day 2)

No Disintegration time (min)

ANALYTICAL METHOD VALIDATION REPORT

ICH Harmonized Tripartite Guideline (November 2005) – Validation of

Drug Registration Guidance Document (DRGD), National

Revision No. Effective Date Change History

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