Retention sample or Control samples management sop

1.0 OBJECTIVE :

To lay down a procedure for Control Sample collection, retention, verification and destruction.

2.0 SCOPE :

This procedure is applicable for control sample management.

3.0 RESPONSIBILITY :

IPQA Chemist or above:

To collect and handover control samples of finished product to QC Department.

QC Chemist or above:

To collect control sample and store in control sample room,

Maintain the record of control sample,

Issue of control sample for various purposes,

Destruction of control samples.

4.0 ACCOUNTABILITY:

Quality Control Head

5.0 PROCEDURE :

5.1 Definition:

Control sample are retained to fulfill two purpose; Firstly to provide a sample for analytical testing and secondly to provide specimen of the fully finished product.

Control Samples may therefore fall into two categories,

Reference Samples : A sample of a batch of starting material or finished product which is stored for the purpose of being analysed should the need arise during the shelf life of concerned.

Retention Samples: A sample of fully packaged unit from a batch of finished product. It Is stored for identification purpose. For examples, presentation, packaging, labeling patient information leaflet, batch number, expiry date should the need arise during shelf life of the batch.

For finished packed, in many instance the reference and retention samples will be presented identically, i.e., as fully packaged units. In such circumstances, reference and retention samples may be regarded as interchangeable.

5.2 Requirements :

Raw material(Active and Inactive) :

The control samples of all raw materials (Active and Inactive) except solvent is retained for the period of Six Month after its expiry date.

Finished product :

The control sample of all the batches manufactured by company should be kept for the period of one year after its expiry date.

5.3 Collection and Retention of Raw Material Control Samples :

QC Representative while sampling raw material for analysis shall also draw additional quantity of raw material as per SOP.

The quantity as per specification of individual raw material (for two complete analysis except microbiological analysis) shall be kept as control sample.

After approval of material, enter the details in Raw material control sample register.

Keep control sample of Raw material in the LDPE bag and keep this LDPE bag in a HDPE container with screw cap.

Affix label of ‘CONTROL SAMPLE’ printed with black ink having all details on the Container.

5.4 Collection and Retention of Finished Product Control Sample:

Packing department in-charge, shall instruct to QA department for product to be packed.

IPQA Representative shall pick up and accumulate samples for control sample from online packing of product covering the entire process for packing.

Control sample will be withdrawn from accumulated samples as per defined quantity of control sample.

The withdrawn samples will be labeled or stamped as ‘Control Sample’.

Remaining accumulated sample will be returned to packing department.

For this entire activity, packing department will assist the IPQA Representative.

IPQA Representative shall bring samples to QC Department and make necessary entries in logbook/BMR to allow the proper reconciliation.

Control sample to be collected in adequate quantities so as to perform analysis in duplicate (except microbiological analysis), if required.

Authorised QC Representative will record the detail of Control Samples of finished product in a Finished Product Control Sample Register.

Affix label with stamp “CONTROL SAMPLE – NOT TO BE SOLD” Printed with Red Coloured Ink on each secondary pack of control sample.

In case of bulk packing, affix the same label directly on jar/bottle.

Preserve the sample in its same or simulated container in which the product is actually marketed.

5.5 Storage of control samples:

Store the control samples of Raw Material & Finished Product at appropriate storage conditions, in area separately marked as “Control Sample “ .

The room is kept in Locked condition with keys available with Quality Control Head or his/her Designee.

Record the temperature and humidity of control sample room twice a day.

Keep all control sample of raw material in labeled corrugated boxes according to month and year.

Keep all control sample of finished product in labeled corrugated boxes according to month and year.

Arrange the corrugated boxes in such a way that the label on the boxes is easily readable.

5.6 Issuance of control sample:

Control sample shall be issued for the following purpose:

For market complaint investigation.

For product study.

For regulatory requirement/ Statutory requirement.

On request of marketing agency.

For physical verification

Control sample should be issued based on the availability of control sample.

Issuance of control sample shall be decided and approved by Head QC and Head-Quality.

5.7 Verification of control samples:

QC Chemist shall check the finished product control samples randomly for physical observations only.

Frequency for verification/observation of each product shall be on yearly basis.

Physical verification of control sample should be scheduled immediately after receiving of control sample and then after every year as per frequency.

Observation of physical appearance shall be recorded in control sample register.

The control sample shall be kept along with control sample of the same batch after physical verification.

Any abnormality observed in physical appearance with respect to the initial observation shall be informed immediately to the head QC.

Head QC of his/her designee shall fill report’ for the said observation to Head QA.

Head production, Head QC and Head QA shall be jointly responsible to investigate the matter.

A joint discussion shall be held to resolve the matter in order to overcome the problem with future batches.

Any non conformance identified with product stability shall be brought to the notice of Head Technical/Directors.

Head QA shall be responsible to take action against the observed abnormality.

5.8 Destruction of control samples:

Remove the expired batches according to date of destruction from each corrugated boxes on first week of every month for destruction.

Destruction should be done under the supervision of a responsible person from IPQA.

Record the destruction details in control sample register.

Remove unit from outer cartons, inner cartons and individual cartons as the case may be.

Tear outer cartons, inner cartons, and individual cartons so as to make small pieces, and ensure that all the printed packing material has left its identity and cannot be used.

Deblister / defoil tablets and capsules. Empty the jar / bottle.

Segregate samples of tablet, capsules and raw materials.

Dip the units having label in tub containing water so as to loosen labels.

Remove the labels as tear them in to small pieces ensuring that all the printed packing material lost its identity and it cannot be reused.

Raw material in liquid form is diluted and flushed with plenty of tap water.

Raw material in solid form is added in sufficient quantity of solvent in which material is dissolved as per solubility and flushed with plenty of water.

Capsules are removed from strip/ blister and the content is added in sufficient quantity of water and transfer for disposal.

Tablets are removed from strip/ blister/ container and crushed, the crushed powder is added in sufficient quantity of water and transfer for disposal.

6.0 Abbreviations:

Abbreviation Expanded form

QC Quality Control

IPQA In-process Quality Assurance

mfg. date Manufacturing Date

exp. Date Expiry Date

HDPE High-Density Polyethylene

LDPE Low-Density Polyethylene

BMR Batch Manufacturing Record

7.0 Annexures:

Annex. No. Title

01 Finished Product Control Sample Register