SOP for Testing and Release Of Product By IPQA at Intermediate Stages

1.0 OBJECTIVE:

The objective of this standard operating procedure (sop) is to lay down the procedure to prepare master copy of analytical worksheet on the basis of TAD, Issuance of worksheet and Testing and Release of product by IPQA at intermediate stages of manufacturing of drug product.

2.0 SCOPE:

The scope of this SOP is to provide the procedure for Testing and Release of product at intermediate stages of manufacturing in in-process Quality Assurance department at [Company name].

3.0 RESPONSIBILITY:

IPQA

• Preparation of master analytical worksheet.

• Request for analytical worksheet for testing, Review and Release of product and attachment of worksheet in Batch Record.

Production:

To co-ordinate IPQA person.

Head QA:

Ensure the compliance of SOP.

Document & Data Controller:

Issuance of Worksheet and management of master worksheet

4.0 PROCEDURE:

4.1 Preparation of Master Worksheet

4.1.1 Worksheets for record of analysis shall be prepared and checked by IPQA Personnel as per the TAD and shall be approved by Head – QA or his designee.

4.1.2 In case of TAD needs to be revised, simultaneously worksheets shall be revised. Old Master worksheet shall be stamp as obsolete.

4.1.3 Any minor mistakes like typographical error etc. is found in worksheet i.e. required for immediate use, the correction shall be made manually by putting sign & date which shall be authorised by Head – QA or his designee in the copies issued for execution.

4.1.4 The same shall be rectified by filling “Request for Document ratification ” Head QA or his designee shall rectify in the original copy.

4.1.5 The corrections made manually shall be incorporated in subsequent revision.

4.2 Issuance of the worksheet

4.2.1 The issue of worksheet for analysis of Granules / Core Tablets / Coated Tablets shall be followed as described below:

4.2.2 The IPQA personnel will raise the requisition for analytical worksheet as per requirement by filling format as per Annexure- V and hand it over to document data controller.

4.2.3 Document Data Controller (QA) shall make the requested photocopy of Record of analysis from the Master Copy.

4.2.4 Documentation Controller (QA) shall enter the product name and batch no. on worksheet with “Blue Color” ink and issue details shall be documented in “Issuance Record of Worksheet for Analysis” in format as per Annexure- IV and each page of worksheet shall be stamped as “QA Issued” in Red color.

4.2.5 Document Data Controller (QA) shall make respective entries in the register as per Annexure- IV and IPQA personnel shall receive the same after signing in the register for “Issuance Record of Worksheet for Analysis” as per Annexure IV.

4.3 Testing & Release

4.3.1 Following instruction to be followed for testing & release of product at intermediate stages.(Granules / Core Tablets / Coated Tablets)

4.3.2 Ensure cleanliness of the testing equipment.

4.3.3 Ensure that the instruments are calibrated and are in working condition.

4.3.4 Sampling shall be done according to current version of sampling SOP.

4.3.5 Send Requisition for issuance of analytical worksheet as per Annexure-V for granules / core tablets / coated tablets to document data controller (QA department) and receive the respective analytical worksheet for analysis.

4.3.6 After verifying the worksheet, IPQA person attached the analytical worksheet with product intimation slip in respective BMR.

4.4 Testing & Release of Granules.

4.4.1 IPQA person analyse the granules as per the current specification and enter the values in controlled analytical worksheet as per Annexure – I.

4.4.2 In case of testing for Validation / Optimisation / Submission batches, Testing shall be performed according to specification and protocol.

4.4.3 After verifying the worksheet by next person in IPQA, approve the Granules for next stage and record the same in respective BMR and sampling detail register by putting sign and date in provided space.

4.4.4 IPQA person will destroy the remaining quantity of granules as per procedure and enter the same in sample destruction record in current version of format.

4.5 Testing & Release of Core Tablets.

4.5.1 IPQA person analyse the core tablets as per the current specification and enter the values in controlled analytical worksheet copy as per Annexure –II.

4.5.2 In case of testing for Validation / Optimisation / Submission batches, Testing shall be performed according to specification and protocol.

4.5.3 After getting the related analytical report from QC department (For test performed in QC) and after getting it verified by QA head or his designee IPQA person will attach the report in respective BMR.

4.5.4 After verifying the analytical worksheet of IPQA (For test performed in IPQA) by next person in IPQA, approve the core tablets for next stage. (Coating / Packing) and record the same in BMR and sampling details register putting sign and date in provided space.

4.5.5 IPQA person will destroy the remaining quantity of core tablets as per procedure and enter the details in sample destruction record of current version of format.

4.6 Testing and Release of Coated Tablets.

4.6.1 IPQA person analyse the Coated tablets as per the current specification and enter the values in controlled analytical worksheet copy as per annexure –III.

4.6.2 In case of testing for Validation / Optimisation / Submission batches, Testing shall be performed according to specification and protocol.

4.6.3 After verifying the analytical worksheet by next person in IPQA, approve the coated tablets for packing and record same in BMR and Sampling detail register putting sign and date in provided space.

4.6.4 Destroy the remaining quantity of coated tablets as per procedure and enter the details in sample destruction record of current version of format.

5.0 ANNEXURE:

Annexure-I: Analytical Work Sheet For Granules

Annexure-II: Analytical Work Sheet For Core Tablets

Annexure-III: Analytical Work Sheet For Coated Tablets

Annexure -IV: Issuance record of worksheet for Analysis

Annexure -V: Request for Issue of Analytical Worksheet

Annexure – I: Analytical Work Sheet for Granules

Product Name:

Date of Analysis:

Batch No.:

Product Code:

Specification No.:

Batch Size:

Mfg. Date:

Exp. Date:

Worksheet Revision No.:

1. Appearance:

Result : Passes / Fails

Analysed By / Date:

Checked By / Date:

2. LOD (Loss on Drying):

Limit :_____________% (w/w)

Instrument ID No.:

Due date for Calibration:

LOD Observed= ________________%

Result: Passes / Fails

Analysed By / Date:

Checked By / Date:

Remarks: The above said product complies / does not complies as per the specification for granules. Hence the product is released / not released for compression.

Analysed By: (Sign / Date)

Verified By: (Sign / Date)

Annexure – II Analytical Work Sheet for Core Tablet

Product Name :

Date of Analysis:

Specification No.:

Product Code:

Batch No.:

Batch Size :

Mfg. Date :

Exp. Date:

Worksheet Revision No.:

1. APPEARANCE:

Result : Passes / Fails

Analysed By / Date:

Checked By / Date:

2. AVERAGE WEIGHT:

Limit:

Balance Id. No.:

Due date of Calibration:

Avg. Wt.=Wt. of 20 Tablets in gm/20

Result : Passes / Fails

Analysed By / Date:

Checked By / Date:

3. UNIFORMITY OF WEIGHT

Limit:

(Weight of the 20 tablets as per the attached printout)

Balance Id. No.:

Due date of Calibration:

Calculation:

Minimum = [Min. Wt. of Tablet(gm)/Avg. Wt. (gm) x100]-100

Maximum = [Max. Wt. of Tablet(gm)/Avg. Wt. (gm) x100]-100

4. Analytical Work Sheet for Core Tablet

Product Name:

Date of Analysis:

Specification No.:

Product Code:

Batch No.:

Batch Size:

Mfg. Date:

Exp. Date:

Worksheet Revision No.:

Result : Passes / Fails

Analysed By / Date ______________

Checked By / Date: _______________

5. DISINTEGRATION:

Limit:

Instrument Id. No.:

Due date of Calibration:

Observation= ________ Min. _______ Sec.

Result: Passes / Fails

Analysed By/ Date:

Checked By/ Date:

6. DIAMETER:

Limit:

Instrument Id. No.:

Due date of Calibration:

Record 10 readings:

Minimum = __________mm

Maximum = __________mm

Result : Passes / Fails

Analysed By / Date:

Checked By / Date:

7. THICKNESS

Limit:

Instrument Id. No.:

Due date of Calibration:

Record 10 readings:

Minimum = __________mm

Maximum = __________mm

Result: Passes / Fails

Analysed By / Date:

Checked By / Date:

8. HARDNESS

Limit:

Instrument Id. No.:

Due date of Calibration:

Record 10 readings:

Minimum = __________mm

Maximum = __________mm

Result : Passes / Fails

Analysed By / Date:

Checked By / Date:

9. FRIABILITY

Limit:

Instrument Id. No.:

Due date of Calibration:

Balance Id. No.:

Due date of Calibration:

Wt. Of tablets Before friabilation : __________ gm

Wt. Of tablets After friabilation : __________ gm

Loss of Wt. After friabilation : __________ gm

% of Loss = Loss of weight after friabilation/ Weight of Tablets before friabilation X 100

Result : Passes / Fails

Analysed By / Date:

Checked By / Date:

10. LOD (Loss on Drying) (105°C, IR Balance, till constant weight)

Limit: _________________%(w/w)

Balance Id. No.: __________

Due date of Calibration :___________

LOD Observed = ________________%(w/w)

Result : Passes / Fails

Analysed By / Date:

Checked By / Date:

Remarks: The above said product complies / does not complies as per the specification for Core Tablets. Hence the product is released / not released for next stage (Coating / Packing).

Analyzed By: (Sign / Date)

Verified By: (Sign / Date)

Annexure – III Analytical Work Sheet for Coated Tablets

Product Name :

Date of Analysis:

Specification No.:

Product Code:

Batch No.:

Batch Size:

Mfg. Date:

Exp. Date:

Worksheet Revision No. :

APPEARANCE:

Result : Passes / Fails

Analysed By / Date ____________ Checked By / Date: ______________

DISINTEGRATION:

Limit: __________________________

Instrument Id. No.: __________

Due date of Calibration :___________

Observation= ________ Min. _______ Sec.

Result: Passes / Fails

Analysed By / Date:

Checked By / Date:

UNIFORMITY OF WEIGHT

Limit: __________________________

(Weight of the 20 tablets as per the attached printout)

Balance Id. No.: __________

Due date of Calibration :___________

Calculation:

Minimum =[ Min. Wt. of Tablet(gm)Avg. Wt. (gm) x100]-100

Maximum =[Max. Wt. of Tablet(gm)Avg. Wt. (gm) x100]-100

Product Name:

Date of Analysis:

Specification No.:

Product Code:

Batch No.:

Batch Size:

Mfg. Date:

Exp. Date:

Worksheet Revision No.:

Result : Passes / Fails

Analysed By / Date:

Checked By / Date:

Remarks: The above said product complies / does not complies as per the specification for Coated Tablets. Hence the product is released / not released for packing.

Analyzed By: (Sign / Date)

Verified By: (Sign / Date)

Annexure – IV Issuance Record of Worksheet for Analysis

Issue Date

Product Name

Batch No.

Issued By / Date

Received By / Date

Remarks

Annexure – V Request for Issue of Analytical Worksheet

From: IPQA

To: Document Data Controller (QA)