Drug Product (Finished, Stability) Sampling Procedure

Standard Operating Procedure (SOP) for the sampling/collection of trial, in-process, Finished product, micro, hold time, validation, control, and stability sample.

SOP for Drug Product Sampling

1.0   PURPOSE:

    • To define the procedure for the sampling of trial, in-process, finish, micro, hold time, validation, control, and stability sample.

2.0   SCOPE:

    • This SOP is applicable for the collection of trial, in-process, finish, micro, hold time, validation, control, and stability sample, manufactured at the pharmaceutical drug manufacturing plant.

3.0   REFERENCES:

    • SOP for Control Sample Management. <SOP>
    • Handling of Product Hold Time. <SOP>
    • SOP for Sampling procedure for withdrawal of Stability samples. <SOP>

4.0   RESPONSIBILITY – SAMPLING PROCEDURE:

    • Production Department:

    • To intimate QA person for the sampling of drug products.
    • To ensure simultaneous entries in the sampling log register.
    • Quality Assurance:

    • To collect samples as per SOP.
    • Quality Assurance Head:
    • To provide training to the concern before the implementation of SOP.
    • Ensure the implementation of SOP.
    • To review and approve the SOP.

5.0   ABBREVIATIONS – SAMPLING PROCEDURE:

    • AQL: Acceptable Quality Level
    • Wt. : Average Weight
    • QA: Quality Assurance
    • QC: Quality Control
    • SOP: Standard Operating Procedure
    • DEFINITION:
    • Sample: Sample is concerned with the selection of a subset of individuals from within a statistical population/batch to represent characteristics of the whole population/batch.
    • Sampling: The procedure of random collection of samples from a defined location.
    • Sampling rod: Device through which sampling to be done.

7.0   PROCEDURE OF SAMPLING:

    • General Sampling Procedure

    • On completion of granulation (Blending/compression/coating/capsulation operation, concerning section’s production person, shall intimate QA through duly filled sampling log register (Annexure-1) and analysis intimation slip (Annexure-2) for sampling of drug products.
    • The QA person shall verify the analysis intimation slip against BMR for the correctness of all the details provided.
    • After verification of the details, the QA person shall fill the analysis intimation slip and prepare the sample for analysis/analysis for in-process label (Annexure-3) for the sample container.
    • The QA person shall do a sampling of the drug product as per the below-mentioned procedure and shall keep the sample in a duly labelled sample container.
    • The sample container shall be kept in self-sealing transparent polyethylene bags.
    • In the case of light-sensitive products, sample container shall be kept in self-sealing black polyethylene bags.
    • In the case of a moisture-sensitive product sample, the QA person shall keep a silica gel bag between the polyethylene bag and the sample container.
    • Sample intimation numbering shall be done as XXX/YY/NNNN,
    • Where
      • XXX denotes manufacturing section code
      • YY denotes the current year
      • NNN denotes of sample intimation number.
Manufacturing Section Section Code
Granulation GRN
Compression COM
Coating COT
Capsule CAP
Packing PKG
Sex Hormone SHD
    • The sampling of Trial, in-process, Finished, Hold time, Validation, Micro, Control, and Stability Sample:

    • Samples of blend shall be withdrawn from each drum and a composite sample shall be prepared.
    • Samples of each drum shall be mixed together to get a composite sample.
    • The pooled sample shall be withdrawn in equal quantity from each selected container as per the AQL procedure for uncoated tablets and capsules.
    • Each collected tablet/capsule shall be checked for quality attribute specified as per AQL.
    • In the case of coated tablets, once the coating is completed (% weight gain is ensured), sampling shall be done from four corners and centre of bed from the coating pan.
    • In case tablets are unloaded from the coating pan, sampling can be done from each selected containers as per AQL procedure.
    • If the coating of a batch is done in more than one lot, samples of each lot shall be mixed together to get a composite sample.
    • In the case of control sample/stability sample sampling, finished tablets/capsules shall be collected from the initial, middle, and end cycle.
    • Validation and hold time samples to be collected as per the given protocol.
    • In case if, hold time exceeds of granules/ uncoated tablet/coated tablet/capsule as per BMR, then sampling to be done from each drum in equal quantity.
    • The stability sample shall be collected as per the stability test request form given to QC.
    • The quantity of sample required, at a different stage of operation is mention below:
    • Quantity for Sampling :

Stage of operation Quantity of Sample required
Trial Finish Micro Hold time Validation Control Stability
Blend 50 g 100 g 20 g 50g or as per protocol As  per protocol NA  

 

 

 

As per stability test request form

Uncoated Tablets 20 tablets Av.Wt.≤200mg 200 tablets 20 g 50 tablets  as per protocol As  per protocol 200 tablets
Av.Wt.˃ 200mg 100 tablets
Coated Tablets 20 tablets 100 tablets 20 g 50 tablets  or as per protocol As  per protocol 200 tablets
Capsules 20 capsules 100  capsules 20 g 50  capsules  or as per protocol As per protocol 200  capsules
Bottle Filling As per blend As  per protocol 200 g
Sachet Filling As per blend As per protocol 24 sachets
  • Note: Sample quantity to be collected as per the above table or it may vary as per product specification.

8.0   ANNEXURES FOR DRUG PRODUCT SAMPLING:

Annexure-1: Sampling Log Register

Sample      Intimation No.

Date Stage of operation Type of sample Product Name

Batch No./ Lot No.

 

Intimation prepared by Production Sign/Date

Received by QA Sign/Date

Received by QC Sign/Date

Annexure-2: Analysis of Intimation Slip

(To be filled by Production)
Product   Batch No.  
Generic Name  
Mfg. Date   Exp. Date  
Stage of Operation   Batch size Kg Units
   
BMR Record No.   Quantity  
Type of sample Trial Finished Micro Validation Hold time Other
(To be filled by QA)
Sample Intimation No.  
Av. wt.:  
Test Required   
Remarks  
Requested By

Production

Sign and Date

Sampled By QA

Sign and Date

Sampled Received By QC

Sign and Date

(To be filled by QC)
Allocated A.R. No.   Specification Code  
Remark/ Other details     
Sample Complies/ Does not comply
Analyzed By/Reported By

Sign/Date

  Reviewed By

Sign/Date

 
Put “NA” where details not required.

Annexure-3: Sample for Analysis

 SAMPLE FOR ANALYSIS

Product Name:………………………………………………………………….

Batch No:………………………….Batch Size:………………………………

Mfg. Date:…………………………Exp. Date:……………………………….

Stage:………………………………..No. of Container:…………………….

Sampled Qty………………………Sampled By/Date:…………………..

Annexure-4: Sample for In-Process Label

SAMPLE FOR IN-PROCESS

 Product Name:………………………………

Batch No:………………………………………

Machine Side:………………………………..

Sampled By/Date:…………………………..

 

 

pharmabeginers

Janki Singh is experienced in Pharmaceuticals, author and founder of Pharma Beginners, an ultimate pharmaceutical blogging platform. Email: [email protected]

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