PROCESS VALIDATION REPORT

PROCESS VALIDATION REPORT FOR ABC TABLETS PROTOCOL REFERENCE NO.: XYZ Product Name Batch Number ABC TABLETS A ABC TABLETS B ABC TABLETS C

REPORT APPROVAL

	Name	Signature	Date
PREPARED BY (QA CHEMIST)
CHECKED BY (QA OFFICER)
REVIEWED BY (PRODUCTION HEAD-TABLET)
APPROVED BY (QA HEAD)

Sr. No.	Details	Page No.
	PRODUCT DETAILS	04
	ANALYTICAL DATA FOR BATCH NO.: A	05-17
	ANALYTICAL DATA FOR BATCH NO.: B	18-26
	ANALYTICAL DATA FOR BATCH NO.: C	27-35
	SUMMARY AND CONCLUSION	36
	RECOMMENDATION	36
	REVALIDATION	36

1.0	PRODUCT DETAILS:
1.1	Product Name :  ABC
1.2	Label Claim:--
1.3	Description:   ---
1.4	Batch Size:   -- kg

ANALYTICAL DATA FOR ABC BATCH NO.: A

2.0

Analytical data for Batch No.:  A                                                              DATE:

2.1 2.1.1

Dry Mixing : Analytical data at the stage of mixing of active ingredient with Excipients : Mix the sifted Materials with Excipients into bowl of RMG 10, 12 and 15 min at slow speed.  10 samples were withdrawn after 10, 12 and 15 minutes of mixing & tested for following tests. Testing on pooled sample : Acceptance criteria Test name Results Description of sample Complies Testing on unit dose sample for ABC content.      Acceptance criteria: - Assay content: - Not less than --% & Not more than -- % of the labelled amount. RSD:-NMT 2.0% ( At 10 min. – SP1 to SP10 , At 12 min.–SP1 to SP10, At 15 min. – SP1 to SP10) Location Sample ID Mixing for    10 min Sample ID Mixing for 12 min Sample ID Mixing for 15 min Top Left SP1 SP1 SP1 Middle Left SP2 SP2 SP2 Bottom Left SP3 SP3 SP3 Top  Right SP4 SP4 SP4 Middle Right SP5 SP5 SP5 Bottom Right SP6 SP6 SP6 Top Center SP7 SP7 SP7 Middle Center SP8 SP8 SP8 Bottom Center SP9 SP9 SP9 Composite SP10 SP10 SP10 Average Average Average RSD RSD RSD Conclusion: - The results of the assay content for 10, 12 & 15 minutes of dry mixing  shows that -- min. of dry mixing  has lowest RSD than the -- & -- min., hence dry mixing  of -- minutes is validated.

2.0

Analytical data for Batch No.: A                                                    DATE:

2.2 2.2.1 2.2.2 2.2.3

Analytical data for drying process Dried the materials in FBD initially for 30 min with inlet temperature at 60°C. Continue drying till LOD is NMT 3% w/w. Sample withdrawals from Top, Center & Bottom part of the bowl. Drying Time:  60 Min ,  Drying Temperature : 60°C Sampling      points Test name Acceptance Criteria Results Top Right LOD at 105OC on moisture balance NMT 3 % w/w Bottom Right Top Left Bottom Left Center Drying Time:  70 Min ,  Drying Temperature : 60°C Sampling      points Test name Acceptance Criteria Results Top Right LOD at 105OC on moisture balance NMT 3% w/w Bottom Right Top Left Bottom Left Center Drying Time:  80 Min ,  Drying Temperature : 60°C Sampling      points Test name Acceptance Criteria Results Top Right LOD at 105OC on moisture balance NMT 3% w/w Bottom Right Top Left Bottom Left Center Conclusion:  The results of LOD for drying process at -- min, --°C meet the acceptance criteria.

2.0		Analytical data for Batch No.: A                                                                DATE:
2.3 2.3.1		LUBRICATION : Analytical data at the stage of lubrication process : Add lubricants into the granules & mixed in Octagonal blender for total 20 min at slow speed. 10 samples were withdrawn after 10, 15, and 20 minutes of mixing & tested for following tests. Testing on pooled sample : Test name Acceptance criteria Results Description of sample Complies Testing on unit dose sample for ABC  Content: Acceptance criteria: - Assay content: - Not less than --% & Not more than -- % of the labelled amount. RSD:- NMT 2.0% ( At 10 min. – SP1 to SP10 , At 15 min.– SP1 to SP10, At 20 min. – SP1 to SP10) Location Sample ID Mixing for 10 min Sample ID Mixing for 15 min Sample ID Mixing for 20 min Top  Right SP1 SP1 SP1 Middle Right SP2 SP2 SP2 Bottom Right SP3 SP3 SP3 Top Left SP4 SP4 SP4 Middle Left SP5 SP5 SP5 Bottom Left SP6 SP6 SP6 Top Center SP7 SP7 SP7 Middle Center SP8 SP8 SP8 Bottom Center SP9 SP9 SP9 Composite SP10 SP10 SP10 Average Average Average RSD RSD RSD Conclusion: - The results of the assay content for 10, 12 & 15 minutes of lubrication shows that -- min. of lubrication has lowest RSD than the -- & -- min., hence lubrication of -- minutes is validated.
	2.0	Analytical data for Batch No.: A                                                                DATE:
	2.4 2.4.1 2.4.2 2.4.3	Analytical data lubricated granules Sr. No. Test name Min Acceptance criteria Results 1 Bulk density 10 min   For information only Bulk density Tap density Tap density Sr. No. Test name Min Acceptance criteria Results 1 Bulk density 15min     For information Bulk density Tap density Tap density Sr. No. Test name Min Acceptance criteria Results 1 Bulk density 20min   For information Bulk density Tap density Tap density Conclusion:  Results of the stage of lubrication meets the acceptance criteria. Bulk density, Tapped density                         results are for information and record.

2.0

Analytical data for Batch No.: A                                                                DATE:

2.5 2.5.1

COMPRESSION : ( INITIAL STAGE) Analytical data of Compression : Using respective punches & dies compression of lubricated granules is done on 51 station machine at 22 RPM. Analysis of Full, Half & Low Hopper Level sample.                                       Results of physical parameters at  22  RPM Sr. No. Test name Acceptance criteria                                  Test Results Full Hopper  Level Half Hopper  Level Low Hopper  Level R1C1 L1C1 R1C2 L1C2 R1C3 L1C3 1. Description Complies Complies Complies Complies Complies Complies 2. Wt. of 20 tablets 3. Individual wt. of 20 tablets R L R L R        L Wt in gm Wt in gm Wt in gm Wt in gm Wt in gm Wt in gm     4. Uniformity of weight for 20 tablets RSD NMT 2%

2.0	Analytical data for Batch No.: A                                                                DATE:
	Sr. No. Test name Acceptance criteria Test Results Full Hopper Level Half Hopper Level Low Hopper Level R1C1 L1C1 R1C2 L1C2 R1C3 L1C3 5. Résistance to crushing ( Hardness) Avg Min Max 6. Thickness Avg. Min Max 7. Friability NMT 1.0% 8. Disintegration time

2.0

Analytical data for Batch No.: A                                                                DATE:

2.5 2.5.2

COMPRESSION : ( MIDDLE STAGE) Analytical data of Compression : Using respective punches & dies compression of lubricated granules is done on 51 station machine at 26 RPM. Analysis of Full, Half & Low Hopper Level sample. Results of physical parameters at  26  RPM Sr. No. Test name Acceptance criteria                                  Test Results Full Hopper  Level Half Hopper  Level Low Hopper  Level R2C1 L2C1 R2C2 L2C2 R2C3 L2C3 1. Description Complies Complies Complies Complies Complies Complies 2. Wt. of 20 tablets 3. Individual wt. of 20 tablets R L R L R L Wt in gm Wt in gm Wt in gm Wt in gm Wt in gm Wt in gm     4. Uniformity of weight for 20 tablets RSD NMT 2%

2.0	Analytical data for Batch No.: A                                                               DATE:
	Sr. No. Test name Acceptance criteria Test Results Full Hopper Level Half Hopper Level Low Hopper Level R2C1 L2C1 R2C2 L2C2 R2C3 L2C3 5. Résistance to crushing ( Hardness) Avg Min Max 6. Thickness Avg. Min Max 7. Friability NMT 1.0% 8. Disintegration time

2.0

Analytical data for Batch No.: A                                                                DATE:

2.5 2.5.3

COMPRESSION : ( FINAL  STAGE) Analytical data of Compression : Using respective punches & dies compression of lubricated granules is done on 51 station machine at 30 RPM. Analysis of Full, Half & Low Hopper Level sample. Results of physical parameters at  30  RPM Sr. No. Test name Acceptance criteria                                  Test Results Full Hopper  Level Half Hopper  Level Low Hopper  Level R3C1 L3C1 R3C2 L3C2 R3C3 L3C3 1. Description Complies Complies Complies Complies Complies Complies 2. Wt. of 20 tablets 3. Individual wt. of 20 tablets R L R L R L Wt in gm Wt in gm Wt in gm Wt in gm Wt in gm Wt in gm     4. Uniformity of weight for 20 tablets RSD NMT 2%

2.0

Analytical data for Batch No.: A                                                                DATE:

Sr. No. Test name Acceptance criteria Test Results Full Hopper Level Half Hopper Level Low Hopper Level R3C1 L3C1 R3C2 L3C2 R3C3 L3C3 5. Résistance to crushing ( Hardness) Avg Min Max 6. Thickness Avg. Min Max 7. Friability NMT 1.0% 8. Disintegration time Conclusion:          On the basis of above study it has been observed that compression machine speed                                at -- RPM has lowest Average RSD of -- % for Right side and --% for Left side. RSD                                limit is NMT 2%.For the test Uniformity of weight of Tablets are well within the acceptable limit                                -- gm to -- gm, in comparisons with machine Speed at -- & -- RPM.                                Other test result like friability and hardness at -- RPM are also under acceptance criteria.                                Considering all above factors it has been concluded that optimum speed of compression                                machine at -- RPM is validated.

2.0

Analytical data for Batch No.: A                                                                DATE:

2.6

Analytical data for  Packaging : Acceptance criteria:- Appearance:  Proper knurling should be visible, there should be no damage and no cut pockets to the blisters and edges of the blisters should be smooth. Embossing: shall be legible on the blister. Sealing:  All the blisters shall pass leak test. Overprinting:  Overprinting shall be legible and no spreading of ink should be there. Parameters to be studied during blister primary packing validation studies Leak Test : Complies with 5  Blisters (Validation study has been carried out  at 3 different temp. by keeping temp. constant and varying speeds at 3 different levels)            Speed   Temp 70 Blisters per min. 90 Blisters per min. 110 Blisters per min. At  150°C-165°C 1S1 1S2 1S3 At   165°C-180°C 2S1 2S2 2S3 At   180°C-195°C 3S1 3S2 3S3 Conclusion:   From the above test it is concluded that the following sealing temperature and speed are validated. Temperature :  --°C - --°C Speed             :   -- Blisters per min.

2.0	Analytical data for Batch No.: A                                                                DATE:
2.7	Analytical data for Finished Product : Sr. No. Test Specification Observations 1.   Description 2.   Identification  3.   Average Wt. of Tablet 4.   Weight  of 20 Tablets 5.   Uniformity weight of tablets 6.   Disintegration Time 7.   Assay : 8. Microbial Limit Test Pathogens Conclusion: - All the tests performed on finished product of ABC TABLET complies as per specification.

ANALYTICAL DATA FOR ABC TABLET BATCH NO.: B PREPARE DATA FOR BATCH NUMBER B AND C AS SAME AS AVAILABLE IN BATCH NO. A

5.0  SUMMARY AND CONCLUSION: ·          Test result and data generated during the process validation studies of batch shall be complied as process validation report.               ·          Any deviation or change in the process or equipment should be recorded. ·          Production Head-Tablet Dept. shall review the complied validation report. ·          Quality - Head of -- shall authorize the report.                                                                                                                                                                                                 6.0  RECOMMENDATION : The data of validation for three batches reviewed, Process parameters data indicates consistent result for three batches. On the basis of these result  prospective process parameters will be fixed for manufacturing of  ABC TABLET ·          Prospective  Process for Dry Mixing: -      Time:  -- min ·          Prospective Process for Drying: -              Time:  -- min             :Temperature : --ºc ·          Prospective Process for Lubrication: -       Time:   -- min ·          Prospective Process for Compression: -   Speed: -- rpm ·          Prospective  Process for Packing :-           Sealing Temperature  : --°C-°C                                                                    Speed                         :   -- Blisters per min.                                                                     7.0 REVALIDATION : ·          Revalidation will be undertaken if: 1)     Change in equipment: If major change in equipment or facilities which may affect the quality of product. 2)     Change in source of Raw Material. 3)     Major changes in process. 4)     Change in formulation / Average weight.