Testing and Release of In process samples, Semi Finished Products and Finished Product

By / Quality control / QC, SOP /

SOP for Finished Product Release | Finished Product Testing Procedure | SOP for Release of Finished Products |

  • SOP for Release of In process samples, Semi Finished and Finished Products covers below points:
    • Testing of in-process samples and semi finished products
    • Release of in-process samples and semi finished products
    • Testing and release by Single Pharmacopeia as per requirement
    • Testing and release of finished product (Packed product)
    • Handling of remain sample after testing
      • Finished product dispose / destruction procedure
      • In-process samples dispose / destruction procedure
    • Handling and analysis of Rinse samples (Residual samples)
    • Flow Chart for Finished Product Analysis
1.0 OBJECTIVE :
  • To lay down the procedure for testing and release of in-process samples, semi finished products and finished products.
2.0 SCOPE :
  • This SOP is applicable for testing and release of in-process samples; semi finished products and finished products in quality control department
3.0 RESPONSIBILITY :
  • The QC Staff shall be responsible for:
    • Testing and release of in-process sample
    • Testing and release of semi-finished product
    • Testing and release of finished product
    • Handling of remain sample after testing
    • Maintenance of related documents
  • The Head QC shall be responsible for:
    • Ensuring adherence and compliance to SOP
    • Verification of Documents
    • Accountability
4.0 ACCOUNTABILITY:
  • Concern Department Head and Head QA shall be accountable for this SOP
5.0 PROCEDURE :

5.1 Testing and release of In-process samples, semi finished products and finished products.

  • Sampling of in-process samples, semi finished products and finished products (Packed product) shall be conducted by IPQA person after completion of activity. (Sampling of Intermediate and Finished Product SOP)
  • Test order shall be created in system by production chemist.
  • IPQA chemist shall collect the samples and product intimation slip (test request) with sign of production chemist.
  • IPQA chemist shall submit the sample along with the test request to finished product section head.
  • Test order number shall be mentioned on test request. The same test order number shall be considered as certificate number of the product.

5.2 Testing of in-process samples and semi finished products:

  • Finished product section head shall enter details of product in finished product entry log book.
  • Test data sheet of in-process testing and finished product shall be issued by the document cell of QC department.
  • Finished product section head shall assign chemist and microbiologist for analysis.
  • The sample shall be hand overed to assigned chemist / microbiologist with test order and test data sheet.
  • Mean while, test order shall be released in system.
  • The status of test order shall be shown as “Value recording”.
  • Chemical and instrument analysis shall be conducted in the quality control department in respective section. Microbiological analysis shall be conducted in the microbiology lab.

5.3 Release of in-process samples and semi finished products:

  • After completion of the total analysis, Quality control chemist shall report to finished product section head with filled test data sheet.
  • Finished product section head shall review the complete document.
  • Value recording of test order of product shall be carried out by the analyst in ERP system.
  • After completion of value recording, the status of the same test order shall be shown as “Testing finished”.
  • Finished product section head shall verify the COA in system against the raw data and ensure that Inspection results shall be shown as “Items are ok”.
  • The test order shall be finished by the finished product section head.
  • The status of test order shall be shown as “Finished”.
  • The reviewed documents along with analytical raw data shall be submitted to Manager – QC for approval.
  • Manager – QC shall review the documents and approve by taking test decision in system.
  • Certificate of Analysis (COA) will be taken from ERP system as Electronic Signature. (Without having manual signature).
  • Certificate of Analysis and Release Slip shall be taken by ERP system.
  • The approved document of semi finished product and in-process testing sample with complied raw data shall be submitted to concerned Quality Assurance officer.
  • Concerned Quality Assurance officer shall review the documents.
  • Semi finished product shall be released based on the release limits (with stringent limit).
  • All injectable shall be released after completion of sterility test (14 days) along with other test.
  • All tablets and capsules shall be released after completion of microbial test (5 days.) along with other test.

5.4 Testing and release by Single Pharmacopeia as per requirement:

  • Semi finished product shall be tested as per the approved specification.
  • The analysis of the batch of the product by single pharmacopeia shall be decided by the production planning team.
  • Request for analysis by single pharmacopeia if required shall be sent QA by production planning team as per format of Declaration for batch analysis requirement, Annexure No.: 07
  • The same declaration form shall be approved by Head-QA or his/her designee.
  • The approved declaration form shall be issued to production department with Batch manufacturing record at the time of issuance by QA.
  • The same declaration form shall be handed over to QA with ERP created test request of the same batch by production department.
  • The test property set of respective tests which are not required to analyze as per declaration form will be deleting by an authorized QA person.
  • The modification by deleting test property set shall be done in test order level only.
  • The declaration form and ERP created test request with sample will be submitted to QC by QA.
  • QC will analyze of this particular batch as per declaration form and release as per point No. 5.2 and 5.3.

5.5 Testing and release of finished product (Packed product):

  • After receiving the packed product with test request and sample, finished product section head shall enter details of product in finished product entry log book.
  • Finished product section head shall assign chemist for analysis.
  • The sample shall be tested for identification or other test such as pH, water content, Average weight etc. as per specification.
  • Observation shall be entered in Annexure No. 06.
  • Value recording of test order of product shall be carried out by the analyst in ERP system.
  • After completion of value recording, the status of the same test order shall be shown as “Testing finished”.
  • Finished product section head shall verify the COA in system against the raw data and ensure that Inspection results shall be shown as “Items are ok”.
  • The test order shall be finished by the finished product section head.
  • The status of test order shall be shown as “Finished”.
  • The reviewed document along with analytical raw data will be submitted to Quality Assurance Manager or his designee for approval.
  • Manager – QA or his designee shall review the documents and approve by taking test decision in system.
  • Certificate of Analysis (COA) will be taken from ERP system as Electronic Signature. (Without having manual signature).
  • Certificate of Analysis and Release Slip shall be taken by ERP system.
  • Finished product (Packed product) shall be released based on the shelf life limit.
  • The test order shall be released, value recording, testing finished and approved in ERP system.
  • Certificate of Analysis, Release Slip and Approved label / Rejected label shall be taken by ERP system.      

5.6 Handling of remain sample after testing:

  • The remaining in-process samples, semi finished products & finished product have to be disposed off after testing.
  • Dispose off should be done under supervision of responsible person
  • This procedure is written as a policy to be strictly followed.
  • Samples that may be left after analysis:
    • Finished products – Injectable preparation – Cytostatic and general
    • Finished products – Tablet/Capsule – Cytostatic.
    • In-process sample (Semi finished product) – Injectable preparation – Cytostatic and general.
    • In-process sample (Semi finished product) – Tablet/Capsule – Cytostatic.
  • In-process samples/Finished product – Injectable preparation – cytostatics product:
  • In-process samples/finished packs excess left after testing to be disposed off as:
    • For ampoules: Break the ampoule and the content is drained into bucket/bin. Empty ampoules are kept in other bucket/bin containing 4-6 % sodium hypochlorite solution.
    • For vials (liquid): Open the Vial using de-sealer and the content is drained into bucket/bin. Empty vials and plugs are kept in other bucket/bin containing 4-6 % sodium hypochlorite solution.
    • For vials (dry powder): Open the Vial using de-sealer and the powder is added to water in bucket/bin. Empty vials and plugs are kept in other bucket/bin containing 4-6 % sodium hypochlorite solution.
    • Empty vials/ampoules are kept with 4-6 % sodium hypochlorite solution for half an hour for deactivation of cytostatics product.
    • Wash the vials/ampoules with water and dispose off by breaking manually or using ampoules crushing machine in small pieces.
    • Add sufficient quantity of 4-6 % sodium hypochlorite solution to the content collected for deactivation of cytostatics product. Mix and keep it for 30 minutes.
    • After 30 minutes, the solution is diluted out with water and hand over to EHS department for discarding.
  • In-process samples/Finished product – Tablet/Capsule – Cytostatic product:
  • In-process samples/finished packs excess left after testing to be disposed off as:
    • In-process samples/finished packs excess left after testing are transferred into a bucket/bin containing water, stir vigorously.
    • Add sufficient quantity of 4-6 % sodium hypochlorite solution to the content collected for deactivation of cytostatics product. Mix and keep it for 30 minutes.
    • After 30 minutes, the solution is diluted out with water and hand over to EHS department for discarding.
    • Empty bags/containers are kept into bucket/bin containing 4-6 % sodium hypochlorite solution. Dip bags/containers completely and allow to deactivate for about 30 minutes. Drain the solution into another bin. Wash bags/containers with water. Washed bags/containers are disposed off in a manner prescribed by local council.
  • In-process samples/Finished product – Injectable preparation – General:
  • In-process samples/finished packs excess left after testing to be disposed off as:
    • For ampoules: Break the ampoule and the content is drained into bucket/bin.
    • For vials (liquid): Open the Vial using de-sealer and the content is drained into bucket/bin.
    • For vials (dry powder): Open the Vial using de-sealer and the powder is added to water in bucket/bin.
    • Vials/ampoules are disposed off by breaking manually or using ampoules crushing machine in small pieces.
    • The content is diluted out with water, drain it and then flush with excess of water.

5.7 Handling and analysis of Rinse samples (Residual samples):

  • Rinse samples will be collected after cleaning of the equipments which were used for manufacturing of the products.
  • Rinse sample request shall be created by IPQA.
  • IPQA chemist shall submit the rinse samples to QC department.
  • Section head shall verify the rinse samples against intimation slip of rinse sample analysis and hand over the samples to the analyst for analysis.
  • Analyst shall verify the samples against intimation slip of rinse sample analysis and analyze by using UV spectrophotometer.
  • Rinse samples will be examined in the range of 200 nm to 400 nm in UV spectrophotometer.
  • The absorbance shall be compared with blank absorbance in the same range.
  • Water will be examined in the range of 200nm to 400nm as a blank run.
  • The absorbance of the rinse samples should be equivalent with absorbance blank.
  • If rinse samples chromatograms will be complied the acceptance criteria, QC analyst shall update comply remarks and request send for approval to authorized QC senior person.
  • The authorized QC senior person shall verify and the same intimation of rinse sample analysis shall be approved.
  • IPQA person shall check, whether the intimation of rinse sample analysis is approved or not for further activity.
 6.0 ABBREVIATIONS:
SOPStandard Operating Procedure
QAQuality Assurance
QCQuality Control
NO.Number
DeptDepartment
COACertificate of Analysis
ERPEnterprises Resource Plan
TDSTest Data Sheet
MHRAMedicines and Healthcare Products Regulatory Agency
PIC/SPharmaceutical Inspection Convention and Pharmaceutical Inspection Co-operation Scheme
OOSOut of Specification
MLTMicrobial limit test

7.0 ANNEXURES:
  Annex. No.Title
01In-process control sample entry log book
02Finished product entry log book
03Destruction Log of Sample Left After Testing
04Flow Chart for Finished Product Analysis
05Checklist For Finished Product Analysis Completion
06Finished Product (Packed Product) Analytical Record
07Declaration for Batch analysis requirement

8.0 SOP REFERENCES
  • Orange Guideline MHRA – Rules and Guidance for Pharmaceutical Manufacturers and Distributors – 2007.
  • PIC/s –Guide to Good Manufacturing Practice for Medicinal Products – 15 January 2009.

END OF THE SOP

ANNEXURES :

Annex. No. 01 In-process control sample entry log book

Annex. No. 02 Finished product entry log book

Annex. No. 03 Destruction Log of Sample Left After Testing

Annex. No. 04 Flow Chart for Finished Product Analysis

Annex. No. 05 Checklist For Finished Product Analysis Completion

Annex. No. 06 Finished Product (Packed Product) Analytical Record

Annex. No. 07 Declaration for Batch analysis requirement