1.Objective :  

To lay down procedure for handling of Control Sample. Also known as Retention Sample or Reserved Sample.

2. Scope :

This procedure is applicable for sampling, storage, issuance and destruction of Control Sample of Key Raw material, Intermediate, Packing material, drug substance and drug product.

3. Responsibility:

QC & QA

4. Definitions:

Control Sample:  A sample of batch of starting material, packaging material, drug substance or drug product which is stored in a simulated pack for the purpose of potential future evaluation during the shelf life of the batch concerned.

5. Procedure:

      5.1 Control Sample Collection

a) Collection of Raw Material Samples & Intermediates:

  • Responsible QC person shall collect the raw material sample &/or Key Starting material (KSM), intermediates as per the defined sampling procedure.
  • Control sample details of material shall be entered into the Control Sample register & Hand over to QA.
  • QA shall store control sample in Control Sample Room as per their defined condition.
  • Control sample is not required for Excipients, Solvents, Liquids, Hazardous material such as Acids, Alkali, Corrosive, and Toxic Materials etc.

b) Collection of APIs & Drug Product:

  • Responsible QA person shall collect the Finished Product sample as per SOP.
  • Control sample details shall be entered in control sample register.
  • QA person shall store the control sample in control sample storage area as per their defined conditions.
  • Each control sample shall have “Control Sample Label “.

c) Collection of Packaging Materials :

  • There shall be approved list of packaging materials for which controls samples shall be taken.
  • Sampling shall be done by QC as per procedure defined in SOP.
  • Packing material control sample shall be retained in Control Sample Room.
  • Four years retention period shall be applicable for Primary Packaging Materials.

5.2 Quantity of Control Sample:

Sufficient quantities should be retained to conduct at least Two Full Compendial analysis or when there is no pharmacopoeial monograph, two full specification analysis.

5.3 Storage of Control Samples:

  • Control samples should be stored in the same packaging system (simulated) in which the Drug Substance or Drug Product is stored or in one that that is equivalent to or more protective than the marketed packaging system.
  • The control sample shall be stored at recommended storage condition as per material or in case of Ambient Condition, store them at temperature NMT 25°C.
  • Store the control sample of cold chain products between 2°C to 8° C.
  • Record the minimum and maximum temperature of control sample room on working days and in case of discrepancy observed inform to department head and engineering department for rectification.
  • The control samples retention period is

For Finished product, one year after expiry date of the batch assigned by the manufacturer or for three years after distribution of the batch whichever is longer.

For APIs with retest dates, control samples should be retained for three years after the batch is completely distributed by the manufacturer.

For Raw Material &/Or KSM , One year

  • In case of Exhibit Batches, storage period shall be up to the regulatory approval.
  • Control samples shall be kept in properly arranged manner for easy traceability.

5.4 Issuance of Control Samples:

  • Holding of control samples is for the purpose of potential future evaluation, for investigation of the quality of the batches & not for the future stability testing or routine analysis purposes.
  • After issuance of required quantity of Control Sample, remaining quantity shall be re-sealed immediately.
  • Control sample shall be issued to concerned person/ department on receipt of requisition approved by quality head /QA head and details are enter in to the control sample issuance register , reconciliation shall be done and record shall be updated.

5.5 Numbering System for Control Sample Room:

  • Number rack individually like A1, A2, A3 etc.
  • Each rack is further divided into rows as R1, R2, R3 etc.
  • B5R2 stands for B-5 rack & second raw

5.6 Physical Verification of Control Sample:

  • Every 10th batch of each finished product (Drug product) shall be selected for Physical verification or minimum 10% of total batches manufactured during that year till its expiry.
  • Any physical excursions shall be evaluated & investigated.

5.7 Destruction of Control Sample:

  • Control samples shall be destroyed after its defined storage period (retention period) on monthly basis as per their defined SOP.
  • The control samples with pending investigation of market complaint shall not be destroyed.
  • QA shall document the destruction details in the column provided in the control sample register with respect to specific Batch No.