Lead time for sample analysis and approval

1.0 OBJECTIVE

                 To lay down the procedure for testing, approval and releasing of in-process samples

2.0            SCOPE

                 This procedure is applicable to all in-process samples for all products manufactured.

3.0 RESPONSIBILITIES

                 Executive – QA

                 Executive – QC 

                 Team Leader – QC

4.0 DISTRIBUTION

Master copy             : Quality Assurance Department

Controlled copy – 1: Quality Control Department

5.0 PROCEDURE:     

As general rule the manufacturing stages in the manufacture of various dosage forms are as follows:

5.1 Tablets

• Granules
• Bulk/Blend
• Compressed Tablets (semi finished, can be considered as Final dosage form before  primary packing if uncoated)
• Coated Tablets (Semi finished can be considered as final  dosage form before primary packing)

5.2 Capsules

• Bulk/Blend
• Filled Capsules (final dosage form before primary packing)

5.3 Liquids

• Bulk
• Filled container or filled bottles (Final Dosage form)
• Ointment / Creams / Gels
• Bulk
• Filled Tube or filled containers (Final dosage form)

5.4 Dry Suspensions

• Granules
• Bulk/Blend
• Filled bottles (Final Dosage Form)
• In-process samples can be defined as the samples from each manufacturing stage in manufacturing of dosage form, which are not in the final pack.
• QA Notification will be generated by production department and delivered to QC by QA. Normally a QA notification will request for test as required in the BPR.  In some cases specific in-process test procedure exists.
• The QA – Executive will check the details in the notification against the BPR and acknowledge receipt of the notification with signature and date.
• Samples will be sampled by the QA – Executive as given in QA SOP “Sampling Procedure for In-Process, Bulk, Granules, finishes Materials of Tablets, Capsule, Syrup, Ointment and injection”.
• The notification and samples are then handed over to the QC – Executive and details are entered, signed and dated at the time of receiving in the in-process samples logbook by QC.
• The samples and notification are then placed in the respective place provided for the purpose in the QC laboratory.
• The QC – Incharge/designee will allot the samples to the analyst.  The QC analyst will necessarily check and compare between the details of the sample label and the QA notification. If there is any difference, shall intimate to the QC in charge for corrective action. 
• The acceptance criteria are given in the BPR for the product.
• Unless otherwise specified in the individual specification and test procedure of in –process for the concern material, test are required to be performed .
• During review of the documents refer the approved specification and test procedures for the release of products.
• The analyst will document the raw data in the Analyst data sheet.
• The analyst will then hand over the compiled document with the Analytical data sheet to the F/P in charge for checking. The compiled document will consist of:
• QA Notification: –
• In the space under QC report the analyst will document the required data with acceptance criteria.
• The analyst will sign under analyst along with date.
• All work sheets, calculation data and chromatograms, dissolutions printouts etc will be attached with analytical data sheet.
• A summary sheet for the results must be prepared.
• The analyst will sign and date all the pages of the document.
• The QC – Manager / designee will check and approve the notification in the “approved by” section and date.
• The QC analyst will prepare the labels in ERP software as applicable with stage of   sample. Like:
• Approved for Compression.
• Approved for Coating.
• Approved for Filling and Packing.
• Approved for Packing.
• Approved for Filling
• The white copy of the notification is given to QA to be handed over to production and is to attach to the BPR. 
• The yellow copy of the notification along with attached analytical documents is handed retained for QC to be filed.
• All out of specifications results should be treated as given as in QA SOP (investigation procedure of out of specification results).
• In case of an Out of Specification results, a copy of the OOS report should be attached with the notification while submitting to QA.
• Rejection of any in-process item is to be handled .
• In case the batch is not released for any particular reason, the cause and further action is decided by the respective in charge/designee in consultation with the Head – QC and Head – QA for the final decision.
• The non-compliance and the corrective action are written in the remarks column of the notification. The analytical documents are handed over to QA for further action.
• In-process samples and test(s) required.

5.5 Final Bulk

• Description.
• Foreign Particles.
• Water Content/LOD (if required)
• Assay (as per Test Procedure for finished product except that the weight of sample taken should be equivalent to the weight of one dosage form).
• Bulk and tapped density (if required).
• Sieve analysis (if required).

5.6 Uncoated Tablets.

• Description.
• Foreign particles.
• Assay.
• Dissolution (If applicable).
• Disintegration (as required).
• Physical parameters (like Hardness, Thickness,Friability etc.)

5.7 The testing of bulk solutions, oral suspension, creams, Ointments and gels before filling will be:

• Description.
• Clarity (where applicable)
• Homogeneity
• pH
• Foreign matter
• Assay

• Grittiness for ointments creams and gels.

5.8     LEAD TIME FOR TESTING OF SAMPLE FOR BULK, SEMI-FINISH AND FINISH

• The bulk and semi-finish sample well be released within 5 days from the receiving date.

• And finish sample will be released within 15 days from the receiving date.

5.9     LEAD TIME FOR TESTING OF RAW MATERIAL

• Raw material which are analyzed in-house Lab released within 7days from the date of sampling.
• Raw material, which are analyzed outside Lab, released within 20 days from the date  of sampling.
• The Raw material, which have to polymorphic test. By XRD in specification released within 50 days from the date of sampling.

5.10    LEAD TIME FOR TESTING OF PACKING MATERIAL

• Time line for sample analysis and release should be 10 days from the date of sampling.

.0            ABBREVIATIONS

QC   – Quality Control

BPR – Batch Production Record