make aware Pharma manufacturing personnel

1. SAMPLING, TESTING AND
RELEASE / REJECTION OF
RAW MATERIALS
Presented by
Malangsha
shkrahul42@gmail.com
1
SAMPLING, TESTING AND
RELEASE / REJECTION OF
RAW MATERIALS
Presented by
Malangsha
shkrahul42@gmail.com

2. Quality control shall receive "Material Received Report (MRR) from
Warehouse as an intimation for raw material sampling.
Upon receipt, sampling Executive shall verify the details on the
MRR and supplier COA.
Sampling Executive shall enter the details in the Raw Material
Inward Record as per the MRR and assigns an Analytical Reference
Number as per SOP.
Sampling I analysis priority shall be decided upon the requirement of
material and production plan, in case of multi MRR receipt.
Executive-QC shall prepare the required number of labels (i.e.,
"Sample for analysis" and"Sampled") as defined in the below sampling
plan.
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Quality control shall receive "Material Received Report (MRR) from
Warehouse as an intimation for raw material sampling.
Upon receipt, sampling Executive shall verify the details on the
MRR and supplier COA.
Sampling Executive shall enter the details in the Raw Material
Inward Record as per the MRR and assigns an Analytical Reference
Number as per SOP.
Sampling I analysis priority shall be decided upon the requirement of
material and production plan, in case of multi MRR receipt.
Executive-QC shall prepare the required number of labels (i.e.,
"Sample for analysis" and"Sampled") as defined in the below sampling
plan.

3. Sampling plan
1 to 5 All
6 to 10 6
11 to 20 7
21 to 56 8
More than 56 --./n+ 1*
If the decimal in --./n value is less than 5, it shall be rounded to the
lowest value, if it is more than or equal to 5, it shall be rounded to
the highest value.
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Sampling plan
1 to 5 All
6 to 10 6
11 to 20 7
21 to 56 8
More than 56 --./n+ 1*
If the decimal in --./n value is less than 5, it shall be rounded to the
lowest value, if it is more than or equal to 5, it shall be rounded to
the highest value.

4. Note: For the new vendor first three consignments of starting
raw materials, composite sample shall be prepared from all
the containers (100% sampling), irrespective of the sampling
plan.
Executive-QC shall carry self-sealed polyethylene bags,
glass bottles, cleaned sampling devices (such as SS Scoop,
thief sampler/glass sampler), prepared labels and sampling
record to proceed for sampling.
 Sampling Executive shall verify the physical condition,
consignment details and "Under Test" label of the containers
against MRR.
In case of discrepancy the same shall be recorded and
immediately informed to warehouse in charge for rectification.
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Note: For the new vendor first three consignments of starting
raw materials, composite sample shall be prepared from all
the containers (100% sampling), irrespective of the sampling
plan.
Executive-QC shall carry self-sealed polyethylene bags,
glass bottles, cleaned sampling devices (such as SS Scoop,
thief sampler/glass sampler), prepared labels and sampling
record to proceed for sampling.
 Sampling Executive shall verify the physical condition,
consignment details and "Under Test" label of the containers
against MRR.
In case of discrepancy the same shall be recorded and
immediately informed to warehouse in charge for rectification.

5. Executive-QC shall randomly select the containers for
sampling and instruct the warehouse personnel to shift the same
containers to sampling booth.
Executive-QC shall wear the safety devices and
proceeds for sampling of selected containers one by one in
the sampling booth.
Sampling Executive shall check the physical appearance of
the material and mix the contents thoroughly within the container
by sampling devices (SS scoops/Thief sampler for solids or glass
sampler for liquids) and collects the sample in self sealed bags
(for solids) and glass bottles (for liquids). 5
Executive-QC shall randomly select the containers for
sampling and instruct the warehouse personnel to shift the same
containers to sampling booth.
Executive-QC shall wear the safety devices and
proceeds for sampling of selected containers one by one in
the sampling booth.
Sampling Executive shall check the physical appearance of
the material and mix the contents thoroughly within the container
by sampling devices (SS scoops/Thief sampler for solids or glass
sampler for liquids) and collects the sample in self sealed bags
(for solids) and glass bottles (for liquids).

6. Post sampling, container shall be sealed or closed immediately
and "Sampled" labels shall be affix on the containers adjacent
to under test Labels.
 Sampling Executive shall take equal quantity from each
container and collect composite sample .
 If the physical appearance of the material is varying from
container to container and specification as well, sampling
activity shall be discontinued and informed to Head-QC.
 In such case Head-QC along with QA representative
shall approach ware house and verifies the physical
appearance of the material.
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Post sampling, container shall be sealed or closed immediately
and "Sampled" labels shall be affix on the containers adjacent
to under test Labels.
 Sampling Executive shall take equal quantity from each
container and collect composite sample .
 If the physical appearance of the material is varying from
container to container and specification as well, sampling
activity shall be discontinued and informed to Head-QC.
 In such case Head-QC along with QA representative
shall approach ware house and verifies the physical
appearance of the material.

7. If the material is confirmed failing in physical appearance,
consignment shall be rejected without OOS investigation.
If the physical appearance of the material in all the containers
is similar and complying, all the samples shall be collected
compositely.
 All observations of sampling shall be recorded in "Raw
material sampling record"
Sampled containers shall be shifted to their original place
immediately.
Details of sampling shall be entered into the sampling booth
usage and cleaning record of warehouse. 7
If the material is confirmed failing in physical appearance,
consignment shall be rejected without OOS investigation.
If the physical appearance of the material in all the containers
is similar and complying, all the samples shall be collected
compositely.
 All observations of sampling shall be recorded in "Raw
material sampling record"
Sampled containers shall be shifted to their original place
immediately.
Details of sampling shall be entered into the sampling booth
usage and cleaning record of warehouse.

8. Collected composite sample shall be brought to QC and
divided into 3 parts in sample distribution area.
One part shall be preserved as retention sample (for starting
raw material only) and other two parts shall be used for
complete analysis (at wet and Instrumentation labs)
The QC Analyst shall test the samples as per respective
standard test procedures.
 If the sample meets the individual specification, material
shall be approved and retention sample shall be logged.
Incase sample does not meet the specification OOS shall be
raised and investigation shall be carried out.
25.0 Based on the investigation status of the material shall be
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Collected composite sample shall be brought to QC and
divided into 3 parts in sample distribution area.
One part shall be preserved as retention sample (for starting
raw material only) and other two parts shall be used for
complete analysis (at wet and Instrumentation labs)
The QC Analyst shall test the samples as per respective
standard test procedures.
 If the sample meets the individual specification, material
shall be approved and retention sample shall be logged.
Incase sample does not meet the specification OOS shall be
raised and investigation shall be carried out.
25.0 Based on the investigation status of the material shall be

9. Liquid raw materials (in tankers) sampling sequence:
Sampling Executive shall take prepared sample labels, Glass
bottles, sampling checklist, Glass sampler and proceeds for
sampling.
Sampling Executive shall verify the compartment wise Seal
Naive intact and "Under test labels" before sampling.
 Sampling Executive shall break the compartment seals and
open the lids one by one.
Sampling Executive shall rinse the sampler thrice with the
material and collect the samples from the top of each compartment
compositely into a glass bottle, if the physical appearance is
similar in all compartments.
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Liquid raw materials (in tankers) sampling sequence:
Sampling Executive shall take prepared sample labels, Glass
bottles, sampling checklist, Glass sampler and proceeds for
sampling.
Sampling Executive shall verify the compartment wise Seal
Naive intact and "Under test labels" before sampling.
 Sampling Executive shall break the compartment seals and
open the lids one by one.
Sampling Executive shall rinse the sampler thrice with the
material and collect the samples from the top of each compartment
compositely into a glass bottle, if the physical appearance is
similar in all compartments.

10. Sampling Executive shall open the bottom valves and drain
about 5 to 10 liters of the liquid into buckets. Then samples shall
be collected from bottom of each compartment compositely into a
glass bottle, if the physical appearance is similar in all
compartments.
Post sampling, compartments shall be sealed or closed
immediately and "Sampled" labels shall be affix on the tanker
adjacent to under test Label.
If the physical appearance of the material is varying from
container to container and specification as well, sampling activity
shall be discontinued and informed to Head-QC.
10
Sampling Executive shall open the bottom valves and drain
about 5 to 10 liters of the liquid into buckets. Then samples shall
be collected from bottom of each compartment compositely into a
glass bottle, if the physical appearance is similar in all
compartments.
Post sampling, compartments shall be sealed or closed
immediately and "Sampled" labels shall be affix on the tanker
adjacent to under test Label.
If the physical appearance of the material is varying from
container to container and specification as well, sampling activity
shall be discontinued and informed to Head-QC.

11. ln such case Head-QC along with QA representative shall
personally verify the physical appearance of the material. If the
material is confirmed failing in physical appearance, consignment
shall be rejected without OOS investigation.
 If the physical appearance of the material in top / bottom portion
is similar and complying, a composite sample shall be prepared and
brought to QC for analysis.
The QC Analyst shall test the samples as per respective standard
test procedures.
If the sample meets the individual specification, material shall be
approved and tanker material shall be unloaded into bulk storage
tank.
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ln such case Head-QC along with QA representative shall
personally verify the physical appearance of the material. If the
material is confirmed failing in physical appearance, consignment
shall be rejected without OOS investigation.
 If the physical appearance of the material in top / bottom portion
is similar and complying, a composite sample shall be prepared and
brought to QC for analysis.
The QC Analyst shall test the samples as per respective standard
test procedures.
If the sample meets the individual specification, material shall be
approved and tanker material shall be unloaded into bulk storage
tank.

12. Quantity unloaded shall be intimated by warehouse and the
same shall be recorded in the raw material inward! sampling check
list and protocol.
Warehouse shall request a fresh A.R.No. for the composite material
of storage tank once unloading is completed.
Incase sample does not meet the specification OOS shall be
raised and investigation shall be carried out.
Based on the investigation, status of the material shall be decided
accordingly.
Analyst shall perform the analysis as per the product STP and
records the raw data in the. "Raw material test protocol". 12
Quantity unloaded shall be intimated by warehouse and the
same shall be recorded in the raw material inward! sampling check
list and protocol.
Warehouse shall request a fresh A.R.No. for the composite material
of storage tank once unloading is completed.
Incase sample does not meet the specification OOS shall be
raised and investigation shall be carried out.
Based on the investigation, status of the material shall be decided
accordingly.
Analyst shall perform the analysis as per the product STP and
records the raw data in the. "Raw material test protocol".

13.  Analyst shall record instrument usage details in respective
equipment logbooks.
Analyst shall attach the calculations / observations /
chromatograms with the test protocols.
Test wise results shall be compiled in the certificate of analysis
and forwarded to reviewer (section head) for cross verification.
Section head shall review the raw data thoroughly and upon
execution further forwards the report to Head-QC/Deputy for
approval.
In-charge - QC I deputy shall verify the data randomly and
approves the document for release. 13
 Analyst shall record instrument usage details in respective
equipment logbooks.
Analyst shall attach the calculations / observations /
chromatograms with the test protocols.
Test wise results shall be compiled in the certificate of analysis
and forwarded to reviewer (section head) for cross verification.
Section head shall review the raw data thoroughly and upon
execution further forwards the report to Head-QC/Deputy for
approval.
In-charge - QC I deputy shall verify the data randomly and
approves the document for release.

14.  Status label (Approved/Rejected labels) labels shall be prepared
and pasted on the under test labels of the containers.
MRR shall be sent to warehouse with status details along with
certificate of analysis.
 In the case of failure in quality parameters, OOS (Out of
specification) shall be initiated for raw materials.
 Further thorough investigation shall be carried out with document
evidence for OOS materials.
 Based on the investigation recommendation, status of the material
shall be concluded.
The final status of the material shall be recorded in the raw
material inward registers along with date of release.
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 Status label (Approved/Rejected labels) labels shall be prepared
and pasted on the under test labels of the containers.
MRR shall be sent to warehouse with status details along with
certificate of analysis.
 In the case of failure in quality parameters, OOS (Out of
specification) shall be initiated for raw materials.
 Further thorough investigation shall be carried out with document
evidence for OOS materials.
 Based on the investigation recommendation, status of the material
shall be concluded.
The final status of the material shall be recorded in the raw
material inward registers along with date of release.

15. Gases, Hazardous and Toxic raw materials:
 Upon receipt of Gas cylinders/Tankers, Hazardous, Toxic raw
materials sampling Executive shall verify the details on the MRR
and supplier/manufacturer COA.
 Sampling Executive shall enter the details in the Raw Material
Inward register as per the MRR and assigns an Analytical Reference
Number.
Sampling Executive shall approach the consignments and visual
verification shall be done.
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Gases, Hazardous and Toxic raw materials:
 Upon receipt of Gas cylinders/Tankers, Hazardous, Toxic raw
materials sampling Executive shall verify the details on the MRR
and supplier/manufacturer COA.
 Sampling Executive shall enter the details in the Raw Material
Inward register as per the MRR and assigns an Analytical Reference
Number.
Sampling Executive shall approach the consignments and visual
verification shall be done.

16. Sampling shall not be performed for such raw materials and
released as per the vendor certificate of analysis.
In the case of captive consumption material transfers, earlier
tested certificate of analysis shall be considered for release.
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