SOP on Sampling of Raw Material

SOP on Sampling of Raw Material

Objective:

  • To lay down the procedure for sampling of raw material.

Scope:

  • This procedure is applicable for sampling of raw material

Responsibility:

  • Chemist or above

Accountability:

  • Head – Quality Control

Procedure:

Sampling

Sampling of Raw Materials:

  • Raw material sampling shall be initiated after receiving the “GRN” from warehouse.
  • QC personnel shall enter the material details in raw material control register as per Annexure No. 01 and allot A.R. No.
  • QC personnel shall generate labels of “SAMPLED” as per Annexure No.08
  • QC personnel shall generate labels of “UNDER TEST “as per Annexure No. 09 . The no. of ‘UNDER TEST’ labels shall be ‘no. of container(s) + 1’.
  • If number of containers is five then six under test labels shall be taken out and one label will be numbered as 00 of 05, 00 of 05 for specimen label with sampling report as per Annexure No.  and 01 of 05 for container number 01, 02 of 05 for container number 02 and so on.
  • QC personnel shall go to the warehouse along with ‘Sampling Report of Raw Material’ as per Annexure No. 02 , GRN, Sampled labels and Under Test labels.
  • QC personnel shall check the material as per GRN.
  • QC personnel shall have to ensure that “Quarantine” labels are affixed on each unit pack by warehouse department.
  • QC personnel shall enter into the sampling booth as per SOP. and Check the status label “CLEANED AREA” on sampling booth before entering into the sampling booth.
  • Ensure that Differential pressure of the sampling booth is within the limits and record the observations as per Annexure No.03 .

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  • Ensure that temperature and Relative Humidity of the sampling booth is within the limits and record the observations as per Annexure No. 01
  • Manometer of Reverse Laminar Air Flow is to be checked before starting the air flow. The manometer level should be at “zero” position. The RLAF shall be kept on at least before 15 min of start of sampling. Operate the RLAF as per SOP .
  • Record the sampling start time and differential Pressure of the RLAF in sampling operational log book as per Annexure No. 03
  • Sampling of non-sterile solid shall be carried out under RLAF located in sampling area of warehouse. Sampling of liquid materials shall be done in the area dedicated for liquid sampling.
  • Sampling of sterile materials shall be done as per SOP .
  • QC person shall use cleaned and dried Sampling devices. These sampling devices shall be wrapped in aluminum foil with status label “Cleaned and Ready for Use” as per Annexure No. 10
  • QC personnel shall use sampling utensils as follows:
Type of Raw materialUtensilsSample collection container
For liquid sampling from drum / bag / containerS.S. sampling rodGlass bottles
For liquid sampling from bottles.S.S. sampling rodGlass bottles
For sampling of material from solid bulk containers.SS sampling rod / SS spatulaLDPE bag

QC personnel shall open the containers or bags under the sampling booth individually and take out the sample as per sampling plan given .

Sampling Plan:

  • Before taking the container(s) inside, ensure that the container(s) are clean. If any container is found damaged or with broken / tampered seal then the container shall be rejected and the same shall be informed to the In-charge of Warehouse department.
  • Observe visually the appearance of the material for any abnormalities like discoloration, lumps, non-characteristic odour, foreign matter, physical heterogeneity etc.
  • Material of only one batch number shall be sampled at a time. After sampling of each material cleaning shall be done as per SOP .
  • Withdraw the sample from the no. of containers as per the table given below:
Type of MaterialNo. of ContainersType of sample
Inactive√n + 1 of the total container1. Composite Quantity (for analysis &

for retention sample)

2. From each sampled container (for

identification)

Active100 % of total containers1. Composite Quantity (for analysis &

for retention sample)

2. From each container (for

identification)

  • If no. of containers of inactive materials are five or less than five then each individual container shall be sampled.
  • Container number of each container shall be assigned as x/y where x is serial number of container and y is the total number of containers, e.g. 1/10 shall be assigned for first container out of 10 containers.
  • Put the container number on label affixed on sample for identification. Label of ‘SAMPLE FOR IDENTIFICATION’ shall be as per Annexure No.13.
  • QC personnel shall open the containers or bags under the sampling booth and withdraw quantities as per list prepared as per Annexure No.6 for active materials and Annexure No. 07  inactive materials.
  • List for sample quantity of active and inactive raw material shall be prepared and reviewed by QC department and approved by QA department. Quantity to be sampled shall be as per approved list. Document No. shall be assigned to the list as QCSG01/D06-XX for active material and QCSG01/D07-XX for inactive materials, where XX is for version no. List shall be revised, if sample quantity of any material has to change or new material has to be added in the list.
  • Sample shall be collected from top, middle & bottom of the layers from the drums for solid materials and for liquid/solvent, top and bottom portion of the barrel / containers. In case of any abnormalities observed, inform to QA Officer for necessary action.
  • Mix the top, middle and bottom portion of solid raw material in S.S. sampling pan and transfer the required material for identification in LDPE (Low density polyethylene) polybag.
  • In raw materials where microbiological testing is required, sample is to be drawn in a separate glass vial bearing the label “SAMPLE FOR MICROBIAL ANALYSIS” from every sampled container. Label of Sample for Microbial Analysis shall be as per Annexure No.12 .
  • Glass vial and spatula for micro sample should be sterile.
  • Raw materials of specific nature, are to be sampled with care, (where its potency, characters, stability are related with storage conditions, i.e. specific temperature, humidity, light resistant or any such requirements).
  • For composite sample, withdraw appropriate quantity of sample equivalent to the required quantity from individual containers ensuring that approximately equal quantity are drawn from individual containers.
  • Fill the required quantity from composite sample for “RETENTION SAMPLE” as well as for “SAMPLE FOR ANALYSIS”.
  • Label the samples as ‘SAMPLE FOR ANALYSIS’ as per Annexure No.04’RETENTION SAMPLE’’ as per Annexure No.5
  • Properly close the container(s) under RLAF and affix self-adhesive label of “SAMPLED” as per Annexure No.8 .
  • Affix self-adhesive label of “UNDER TEST” as per Annexure No.9  on all containers of that batch.
  • Record all observations in sampling report of raw material as per Annexure No.02

Cleaning of Sampling Devices:

  • Sampling devices shall be washed with running purified water.
  • During washing of the sampling devices, if any residue is visually seen, scrub the sampling devices with lint free cloth and wash it thoroughly with purified water.
  • After removal of all residues from the sampling devices, rinse the sampling devices thoroughly with purified water and finally rinse the sampling devices with Isopropyl alcohol and dry it.
  • After completion of drying, wrap the sampling devices in aluminum foil and put “CLEANED & READY FOR USE” status label as per Annexure No. 10
  • Keep the sampling devices in a designated place.
  • Record the cleaning activity in cleaning and usage log for sampling devices
  • Bring the sampled polybags/ Glass Bottles to Quality Control Laboratory for analysis.
  • List of Annexure / Formats:
  • Raw material Control Register  :  Annexure 1
  • Sampling report of  raw material  : Annexure 2
  • Sampling operational log book  :Annexure 3
  • Label of Sample for Analysis  : Annexure 4
  • Label for Retention Sample : Annexure 5
  • Sampled quantity for raw material (active) : Annexure 6
  • Sampled quantity for raw material (inactive) : Annexure 7
  • Label for ‘Sampled’ : Annexure 8
  • Label for ‘UNDER TEST’ : Annexure 9
  • Label for ‘Cleaned & Ready for Use : Annexure 10
  • Format of Cleaning and usage log book for sampling devices  : Annexure 11
  • Label of Sample for Microbial Analysis : Annexure 12
  • Label for Identification : Annexure 13

References (if any):

Reason for Revision:

  • For better cGMP & cGLP

Abbreviation:

  • SOP     : Standard Operating Procedure
  • QC   : Quality Control
  • QA    : Quality Assurance
  • SG   : Sub general
  • R. No.  : Analytical Report No.
  • GRN     : Goods Receipt Note
  • LDPE   : Low density polyethylene
  • SS sampling device     : Stainless steel sampling device
  • IPA       : Isopropyl Alcohol
  • cGMP   : Current Good Manufacturing Practice
  • cGLP    : Current Good Laboratory Practice

Annexure 1

Raw material Control Register  :  

Sr. No.

Date

Name of Material

Manufacturer / Supplier Name

GRN No. / Date

Batch No. / Lot No.

Mfg. Date

Exp. / Retest Date

Quantity Received

No. of Containers

A. R.  No.

Worksheet No.

Quantity Sampled

Sampled By / Date

Date of Analysis

Date of Completion

Analyzed By

Status

Remarks

Annexure 2

Sampling report of  raw material  : 

Sampling Report of Raw Material
1Name of material / Item code :
2Name of Manufacturer / Supplier :
3GRN No. / Date :                                                         A. R. No.:
4No. of Containers Received :                                     Total Quantity Received :
5Storage Condition : OK / Not OK
7.Quarantine Label :                                    a) Affixed            b) Not affixed
8.Packinga) Drums / Bottles / Corrugated box
b) Fibre Plastic drums with polybag inside
c) PP woven bags with polybag inside / Paper

bag with polybag inside

9.Packing condition:  (OK / Not OK)

(State observations if not satisfactory)

10.Container Label Detail Verification
a) Pharmacopeial Status

(IP / BP / USP / EP / In-house)

b) Manufacturer’s Name
c) Batch No. / Lot No.
d) Batch Size
e) Date of Manufacturing
f)  Date of Expiry / Retest
g) Storage Condition
h) Any other Remarks
11.Physical Appearance
a) Presence of Lumps
b) Any abnormal odour
c) Heterogeneity between same

container / container to container

d) Foreign Matter
e) Any other abnormality
12.No. of Containers Sampled :                                        Sampled Quantity :
13.Manufacturer’s Certificate of Analysis
14.Remarks:
15.Sampled By/Date:

Annexure 3

Sampling operational log book  :

Sr. No.Name of MaterialA.R. No.Date of SamplingRLAF Started atMagnehelic Reading after 15 minsSampling TimeSampling Done ByRemarks
Pre-FilterFine-FilterHepa-FilterStart TimeEnd Time
1 mm-5 mm5 mm-10 mm10 mm-20 mm
     

Annexure 4

Label of Sample for Analysis  : 

Material name / Item Code____________________

GRN No. _____________    A.R. No._______________

Batch/Lot No. ___________ Batch size______________

Mfg. Date____________      Exp./Retest Date_________

Sampled _____________    Sampled by

Quantity                                (Sign/Date)

Annexure 5

Label for Retention Sample : 

Material Name / Item Code____________________

GRN No. _____________    A.R. No._______________

Batch/Lot No. ___________ Batch size_____________

Mfg. Date____________      Exp./Retest Date_________

Sampled _____________    Sampled by

Quantity                                (Sign/Date)

Annexure 6

Sampled quantity for raw material (active) :

Document No. Page No.
Sr. No.MaterialComposite Sample Quantity (chemical + microbial analysis)Sample Quantity for RetentionSample  Quantity for Microbial AnalysisRetest Sample QuantitySample Quantity for Identification (per sampled container)

Annexure 7

Sampled quantity for raw material (inactive) : 

Document No. Page No.
Sr. No.MaterialComposite Sample Quantity (chemical + microbial analysis)Sample Quantity for RetentionSample  Quantity for Microbial AnalysisRetest Sample QuantitySample Quantity for Identification (per sampled container)

Annexure 8

Label for ‘Sampled’ : 

SAMPLED

Sampled by:

(Sign. / Date)

Annexure 9

Label for ‘UNDER TEST’ : 

UNDER TEST

 A.R.No.:                                                   

Container No.:                                      Sign./Date:

Annexure 10

Label for ‘Cleaned & Ready for Use :

CLEANED & READY FOR USE

Sampling utensil               :       

ID No.                                  :

Previous material              :

A.R. No.                              :

Sign                                    :

Date                               :

Annexur 11

Format of Cleaning and usage log book for sampling devices  : 

Sr. No.DateSampling devicesID No.

 

Used for

Material

A.R. No.Cleaning TimeDone ByChecked ByRemarks
Started atCompleted at

Annexure 12

Label of Sample for Microbial Analysis : 

SAMPLE FOR MICROBIAL ANALYSIS

Material Name / Item Code____________________

GRN No. _____________    A.R. No._______________

Batch/Lot No. ___________ Batch size_____________

Mfg. Date____________      Exp./Retest Date_________

Sampled _____________    Sampled by

Quantity                                (Sign/Date)

Annexure 13

Label for Identification : 

SAMPLE FOR IDENTIFICATION

Material Name /Item Code_________________________

GRN No. _____________    Container No._______ ____

Batch/Lot No. ___________ A.R. No._______________

Mfg. Date____________      Batch size_____________

Sampled _____________    Exp./Retest Date_________

Quantity                                Sampled by______________

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About Alice

Alice is the Author and founder of Drugsformulations, she is a pharmaceutical professional having more than 18 years of rich experience in pharmaceutical field. During her career, she works in the quality assurance department with multinational companies i.e Zydus Cadila Ltd, Unichem Laboratories Ltd, Indoco remedies Ltd, Panacea Biotec Ltd, and Nectar life Science Ltd. During his experience, she faces many regulatorily audits i.e. USFDA, MHRA, ANVISA, MCC, TGA, EU –GMP, WHO –Geneva, ISO 9001-2008 and many ROW Regularities Audit i.e.Uganda, Kenya, Tanzania, Zimbabwe. She is currently leading a regulatory pharmaceutical company as a Head Quality. You can join him by Email, Facebook, Google+, Twitter, and YouTube

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