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SOP for Sampling of Raw Material


Standard operating procedure of sampling of Raw Material received in Stores in pharmaceutical industries using square root of containers +1 sampling plan.

1.0  OBJECTIVE

       To lay down procedure of sampling of raw material in order to get a representative sample of the whole lot for analysis.

2.0  SCOPE

       This procedure is applicable for sampling of all raw materials received.

3.0  RESPONSIBILITY

3.1  Doing       Technical Assistant 
3.2  Checking :  Executive/ Manager

4.0  ACCOUNTABILITY

       Head of the Department

5.0  PROCEDURE

5.1  Precaution

5.1.1  Use clean and dry sampling device for sampling kept in clean poly bags from “Ready for use” receptacle.
5.1.2  Use sampling device after mopping with freshly prepared 70% IPA for collecting the sample for microbiological limit test.
5.1.3  Material of only one consignment shall be sampled at a time.
5.1.4  Use different sampling devices for sampling of different materials.
5.1.5   During sampling wear mask, cap, hand gloves and shoe covers (booty).
5.1.6  Carry out the sampling of active and inactive hygroscopic, light sensitive raw material in sampling booth which has sodium lamp & dehumidifier facility.
5.1.7  Switch On the sodium lamp for 5 minutes before sampling the light sensitive material.
5.1.8  Carry out sampling of Inactive material in dedicated sampling booth having identification No: SB01 and active material in sampling booth having identification No.SB02.
5.1.9  Ensure that the manometer reading of sampling laminar airflow unit is between 7 to 15 mm of water before sampling.
5.1.10  All solids as well as liquids materials except solvents are to be sampled in sampling booth.
5.1.11  Sample for microbial testing shall be taken first followed by other sampling.
5.1.12  Make sure that cleaning status on room label is available on  the sampling booth before starting sampling.
5.2  Receive the MATERIAL RECEIVING REPORT in triplicate with sign of store incharge and with physical verification report from the stores and enter the following details in the raw material log register maintained separately in Q.C. dept. for Active and inactive raw material, company wise. 
            Date of Receipt                                                 Supplied By
            A.R. No.                                                          Qty received 
            Batch No.                                                         Mfg Date 
            Name of Material                                              Exp. Date    
            Manufactured By                                              Store Ref. No.
5.3  Assign the work of sampling of the material to the authorized Q.C. chemist. List of authorized person.
5.4  Make sure that material is received from Approved Vendor.

5.5  Sampling container

5.5.1  Select the sample container according to the nature of the material to be sampled on basis of list prepared & updated.
5.5.2  Use clean fresh poly bags for solid materials.
5.5.3  Use clean dry amber glass bottle with screw caps for liquid and transparent stoppered flask for solvents.
5.5.4  Sample all light sensitive solid materials in black polyethylene bag.
5.5.5  Sample all the moisture sensitive materials in air tight container.
5.5.6  Use sterile tubes for sampling the material for microbial test within 24hr. of sterilization.

5.6  Sampling device

5.6.1  Use stainless steel sampling devices specially designed for solid and liquid material.
5.6.2  For solid materials received in drums/container use specially designed stainless steel sampling device by which material can be sampled from different level (Thief sampler).
5.6.3  For liquid and solvents received in drum, use specially designed S.S. drum sampler.
5.6.4  For liquid material received in small container use specially designed small SS liquid sampler (SS scoop)
5.6.5  For solid material received in bags use specially designed SS solid sampler.
5.6.6  Clean and maintain the sampling device as per S.O.P on completion of sampling.

5.7  Sampling preparation

 5.7.1  Check the details on the MATERIAL RECEIVING REPORT and enter the details in computer for UNDER TEST labels as follow.
Name of Material  :
Material code No  :
A.R. No  :
Sampled by  :                                         Date :   
Container No  :     of :
Sampled Qty  :         
5.7.2  Prepare and send the sample withdrawal slip to Raw material store for quantity of material to be sampled.
5.7.3  Ensure that containers are cleaned externally, before bringing the container to be sampled to the sampling area.
5.7.4  Check the details given on the Material Receiving Report with the suppliers label and the label affixed by the stores on all 100 % raw material containers.
5.7.5  Check whether the material falls under Approved vendor list.
5.7.6  If the material is not from approved vendor, then the material is not to be sampled.
5.7.7  Any discrepancy found should be immediately brought to the notice of the store incharge and Q.C. Executive/Manager.

5.8  Damaged containers

5.8.1  Check the physical condition and cleanliness of raw material containers before opening for sampling.
5.8.2  If any container found in damaged condition, intimate Raw material store incharge to make separate MRR.
5.8.3  Damaged containers whose integrity is doubtful should be sampled and tested separately with a separate A.R.No.

5.9  Gowning procedure

5.9.1  Wear fresh gown before entering into sampling area.
5.9.2  Cover the hands with gloves and wear a cap and mask to cover hair and nose respectively.
5.9.3  Cover the footwear with shoe cover .
5.9.4  Use separate apron, nose mask, Hand gloves, cap & shoe covers for sampling of different material.
5.9.4  Mop the hands with 70% IPA and air dry before proceeding for sampling and particularly when samples are to be drawn for Microbiological testing.

5.10  Sampling 

5.10.1  Before proceeding for sampling ensure:
              • Cleaned’ status for the sampling area
              • Availability of ‘Ready for use’ suitable sampling device
              • Removal of all previous raw material containers and used utensils.
5.10.2  Label the sample bag or container properly & keep it ready. Arrange the raw material containers which are to be sampled in sampling booth area.
5.10.3  Note down the differential pressure reading of sampling booth and other respective detail in sampling checklist.
5.10.4  Open the container for sampling one by one.
5.10.5  Observe visually for appearance of the material for any gross abnormalities like decolourization, lumps, non-characteristics odour, foreign matter and physical heterogeneity.
5.10.6  In case of any abnormalities observed, inform to the store incharge and QC executive/Manager.
5.10.7  In case of all active raw materials carry out sampling from all containers in each of supplied batch for performing identification test individually for all the containers as per S.O.P.
 5.10.8  In case all inactive materials carry out sampling from different containers in each of supplied batch according to formula √n+1 e.g. for 10 containers sample from √10+1=4 containers.
 5.10.9  Assign the sampled Container No. as follows. (for active raw material only.)
e.g. If 25 containers are received then give the container no. as 1/25, to 25/25 with Reference to drum number of container sampled.
 5.10.10  Record the individual container no. in Annexure II given by store from which sample is drawn. Leave the space as blank in container number column of Q.C “UNDER TEST” label.
5.10.11  Draw the sample from different levels of the container. (i.e. From Top, Middle & bottom). The weight of the sampled quantity should be as per list prepared
5.10.12  Reseal the container after sampling as under and transfer it to UT area
1  Fibre/Plastic container pack
Shrink the inside poly bag by twisting it sufficiently. Bent it & tie it using plastic seal. Place the lid of container & close it tightly & seal it.
2  Woven and Paper Bag : Close the sampling point with butter paper and seal it properly using BOPP tape.
3  Liquid RM container : Place the lid of container & keep it tightly closed.
5.10.13  Place the used sampling device in container labelled as ‘To be cleaned’ containing a poly  bag.
5.10.14  Transfer the collected sample to QC laboratory under supervision.
5.10.15  For inactive material prepare two composite samples by taking equal quantity of material from the sampled drum. Mix thoroughly with spoon in big polythene bag for retained sample and testing sample.
5.10.16  For active raw material prepare composite sample for every 10 containers of the consignment by taking equal quantity of material from individual sample container. Mix thoroughly with spoon in big plastic bag to make sample for assay test. For complete analysis and retain sample make composite sample by taking equal quantity from all bags.
5.10.17  If specified in the Annexure-I, take the composite sample for microbiological analysis in sterile container.
5.10.18  Ensure the sample containers are closed tightly and labelled properly.
5.10.19  Handover the samples along with MRR, stores physical verification report, sampling checklist and supplier’s COA (IF received) to Q.C. department for analysis.
5.10.20  If the party’s COA is not received, inform to Purchase Department.
5.10.21  Keep the retain sample and sample to be analysed at specified storage condition as per SOP.
5.10.22  Mark ‘SAMPLED’ stamps on containers from which the samples are collected. Cross the original approval label of manufacturer on all the containers.
5.10.23  Affix yellow colour duly filled & signed “UNDER TEST’’ label on each container below  white label of store.
5.10.24  Prepare sampling record of raw material.
5.10.25  Make the entry of sampling done in sampler booth log card with respective details.

6.0  ABBREVIATIONS

6.1  COA = Certificate of Analysis.
6.2  Q.C. = Quality Control
6.3  No. = Number
6.4  Mfg. date = Manufacturing date
6.5  Exp. Date = Expiry date
6.6  MRR = Material Receiving Report
6.7  UT    =  Under Test 
Ankur Choudhary is India's first professional pharmaceutical blogger, author and founder of Pharmaceutical Guidelines, a widely-read pharmaceutical blog since 2008. Sign-up for the free email updates for your daily dose of pharmaceutical tips.
Email: .moc.enilediugamrahp@ofni Need Help: Ask Question


1 Comment so far : Add yours...

Tatva Chintan said...

Amazing post Ankur. You have shared a very informative post on the standard procedures to be followed while sampling pharma raw materials. Would surely share it with our clients at Tatvachintan Pharma Chem. We are a leading raw material supplier for any pharma industry

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