Sop for sampling of Raw Materials.
This Document describes (Standard Operating procedure) Sop for sampling of Raw Materials.
Sop for sampling of Raw Materials.
I. Purpose & Scope:
- The purpose of this SOP is to lay down a procedure for sampling of Raw Materials.
- This procedure is applicable for sampling of Raw Materials received and raw materials falling in re-test schedule
II. Responsibilities:
- All Quality Control and Quality Assurance personnel’s shall be responsible to follow and implement this SOP.
III : Introduction and Procedural Part :
Procedure for sampling of Raw materials :
Precautions while sampling of Raw materials :
- First carry out the sampling of Inactive Raw Materials then Active materials (when active and inactive raw materials are to be sampled at a time) with clean & dry sampling tools. Keep the sampled material in a self-sealing poly bag.
- While carrying out sampling of light sensitive materials ensure that the tube lights of RLAF and respective area are switched off and a sodium lightis switched on. Black polybag shall be used as an outer bag to enclose the sampled material in a plain poly bag.
- While sampling fluffy materials like colloidal silicon dioxide (Aerosil), sodium lauryl sulfate and color; RLAF shall be switched off to avoid spreading/dispersion of the material in the sampling room.
- The raw material stored at 2°C to 8°C shall be stabilizing at room temperature before sampling. This could not be exposed for long time at room temperature.
- Check the environmental conditions of sampling booth; Temperatureshould not be more than 25°C and humidity should not be more than 50% before commencement and after completion of sampling activity.
- If the environment condition i.e. temperature, relative humidity & differentials pressure are not within the limit, do not start sampling of raw materials and inform the Engineering department for corrective action.
- In case of multiple materials sampling of raw materials in a day of active raw materials, the sampling person should come out in the 1st change room discarded the apron, gloves, mask and cap. Wear fresh set of clothes, disinfect the hands & then enter the sampling room.
- After sampling of each consignment, sampling chemist and workmen shall disinfect the hands with 70 % IPA solution kept in the sampling room.
- In case of power failure during sampling activity close the material container as early as possible. Restart the sampling activity after 15 minute of starting of RLAF and record the observations in the log book.
- Use sampling device of appropriate size for one material only, after usage put it in appropriately labeled polybag tied with plastic tie or nylon thread and send for cleaning.
Sampling of Raw materials Methodology :
- After receipt of Goods Receipt Note (GRN) from warehouse QC officer/designee shall enter all relevant details in the raw material inward register.
- QC Manager/ Designee shall verify the details of GRN against approved vendor list and vendor COA as per respective specification and handover the GRN to trained person for sampling of raw materials.
- QC officer generates the A. R.No. (Analytical report number) in sequential manner and plan for sampling of raw materials.
- Sampling person shall prepare the sampling kit & label as per sampling of raw materials requirement. Refer Annexure I for sampling kit.
- QC officer shall follow the procedure for entry and exit in warehouse as well as sampling booth. He/She shall refer the pictorial diagrams affixed in sampling booth for gowning.
- Calculate the approximate sample quantity to be withdrawn from each container by dividing to total sample quantity (Sample for analysis & control sample) by total number of containers.
- QC officer/chemist shall wear proper uniform, footwear in the airlock and disinfect the hands with 70% IPA before entering in sampling room.
- Warehouse personnel shall pass the material in sampling room through airlock. Ensure the next door of airlock is close during transfer of material.
- Verify the details of consignment against GRN and same is recorded on sampling checklistrefer Annexure – II.
- Check and record the details provided in sampling log book as per Annexure –III.
- If any abnormal observation, non conformance, deviation is observed/occurredimmediate report it to QA/QC Head.
- QA/QC Head shall verify the non conformance and shall take immediate actions to proceed further with proper corrective and preventive actions.
- Use clean poly bags for collecting the solid raw material samples. Use clean and dried glass bottles for collecting the liquid raw materials.
- Check and verify for cleanliness of sampling room as per the checklist mentioned in Annexure -IV. If found not cleaned get it cleaned before sampling. Name of the previous sampled material should be taken from the Sampling of raw materials log book.
- Switch on the RLAF at least 15 minutes prior to starting of the sampling of raw materials activity and record the pressure differentials of RLAF after 15 minutes in the sampling log book as per Annexure – III.
- Pressure differential for across HEPA should be in between 8 to 20 mm of water.
- Pressure differential for across pre-filter should be in between 2 to 8 mm of water.
- After stabilize the pressure of RLAF; balance verification shall be done by using standard calibrated weights as per SOP & record shall be maintained.
- Balance verification shall be done as and when required. The validity for verification is for entire day. Re-verification shall be done when balance is switched off.
- Ensure the spirit level of weighing balance after movement of containers.
- Only one cleaned container of a material shall be brought into RLAF. after completion of sampling from one container the same shall be taken outside. Take care that sampled and unsampled containers are not mingled. Next container shall be taken inside the RLAF after the previous container is taken out.
- Ensure the container shall be open under RLAF.
- Use appropriate sampling tools whenever required for sampling of raw materials.
- Use different sampling tools for different materials.
- Follow the specific instruction as indicated on containers (if any) to be sampled.
- Physically damaged container(s) without seal shall be assessed for intactness of innermost packing. Physically damaged container(s) shall be reported to Head QA for information and further necessary actions.
- Take the sample quantity as maintained in the Sample Quantity List as per Annexure –VI
- Carry out sampling of raw materials from the entire containers i.e.100% sampling for all the active materials. The sample drawn from each container shall be used for identification and composite sample use for complete analysis. Make sample composite in RLAF.
- Carry out sampling from the entire containers i.e.100% sampling for all the Excipients. The sample shall be drawn from individual container and make it composite sample in RLAF for complete analysis.
- Use following samples for different type of raw materials
| Big SS rod with small cup | For liquid sampling from drums |
| Glass pipette with Rubber bulb | For liquid sampling from bottles / cans. |
| Sampling Rod / Spatula | For sampling of raw materials from solid bulk containers. |
- Containers/packs which are selected for sampling of raw materials shall be number as follows S/N‘S’ stands for serial number of container selected for sampling. ‘N’ stands for total number of packs/containers, Example-1/10, 2/10, 3/10……..10/10. Container number shall be written on the “SAMPLED LABEL”
- Affix the samples label on container at the right side of Quarantine label. If the space is congested then affix the label wherever space available but it should be near or back side of quarantine label and easily visible.
- Affix the “Under Test Label” on Quarantine label in such a way that only “QUARANTINE” word of Quarantine label shall be hidden.
- Ensure all the containers are properly sealed and transferred to under test area.
- Sampling of raw materials shall be completed within 15 days from the date of GRN receipt.
Sampling of solid Raw materials:
- To take the sample from the container by sampling equipment close the sampling pits by rotating the sampler.
- Insert the sampler/Sampling device inside the container.
- Rotate the sampler to expose the pits.
- Agitate the sampler gently to & fro to fill the pits.
- Rotate the sampler to close the pits & lift the sampler outside the container.
- Hold the sampler in horizontal position on the butter paper & rotate the Sampling device and remove the samples appropriate samples by using cleaned spatula, collect the sample from the top, middle & bottom portions of the container on the butter paper
- Simultaneously close the containers of the material sampled properly, with a plastic seal /nylon thread as appropriate for the inner bag and close the lid of the container.
- In case of any abnormalities observed, inform to QA/QC head for further process.
- Mix the top, middle and bottom samples on the same butter paper to make a homogenous blend using spatula. Transfer the required quantity as per Annexure-VI “Sample Quantity Details” in a transparent poly bags by using a clean and dry spatula for identification test of each container. After transferring the sample for identification test, remaining sample from the butter paper shall be transferred to the poly bag meant for composite sample for analysis &control sample.
- Label the polybag appropriately with the concernedidentification label i.e. ‘samplefor analysis’and ‘Control sample’.
- Collect all the samples in a polybag. Sample for analysis shall be carried and store in designated cabinet in QC. Control sample shall be handover to QA officer for further process of keeping of control samples. Record shall be maintained as per Annexure V.
- Likewise, sample the remaining individual containers and Affixed“SAMPLED” & “UNDER TEST” label to each container.
- Weigh the required quantity from this composite sample for preparing Sample for analysis and control sample.
- Discard the used butter paper in the waste bin.
- Use sampling device of appropriate size for one material only, then after use put it in a polybag with “TO BE CLEANED”.
- Remove the “TO BE CLEANED” label. Wash the sampling tool with potable water under running water for 1 to 3 minutes to flush out the adhered powder.
- Clean the sampling tool using 0.1% teepol solution. (Take approximate 1ml of teepol and dissolve in to 100 mL. quantity of purified water to get 0.1% teepol solution).
- Wash thoroughly with potable water approx 5 liter from inside & outside, finally rinse with purified water.
- Check the surface of the cleaned parts and ensure that they appear clean to the naked eyes. In case if any part appears unclean to the naked eyes, repeat the above procedure
- Dry with a clean and dry lint free cloth.
- Wipe the dried sampling device with 70% IPA.
- Attach “Cleaned” label to clean sampling device and wrap into polybag.
- Store the cleaned sampling devices in the secure cupboard provided in sampling booth.
- The sampling device is to be wiped with 70 % IPA before sampling of raw materials .
Sampling of Liquid/Solvent Raw materials:
From Large containers (above 50 lit)
- Liquids from large containers shall be sampled in the quarantine area.
- Insert the SS tube with small cup in the container and withdraw the sample.
- Simultaneously close the containers properly.
- Put the S.S .Sampling device after use in a polybag and tie with nylon thread appropriately labeled and transfer for cleaning.
- Clean the samplers / sampling device as stated earlier.
From small containers (50 lit /below 50 lit):
- Mix the content of the liquid container well by shaking the container and sample under RLAF.
- Insert the pipette in the container and with the help of the rubber bulb withdraw the sample.
- Take the required quantity of sample and close the container properly.
- Likewise sample the remaining individual containers.
- Mix the liquid quantities from the individual containers well to prepare composite sample in a bottle.
- Label the sample bottles appropriately.
- After sampling label “SAMPLED” & “UNDER TEST” to the Container.
- Samples shall be carried along with GRN, Party COA to Quality Control Department and microbiology department (if any) for analysis.
- Clean the sampler/sampling device as stated earlier.
IV: Annexure:
| Annexure No. | Format Name |
| Annexure – I | Sampling Kit |
| Annexure – II | Sampling checklist |
| Annexure – III | Sampling Log Book |
| Annexure – IV | Sampling area Cleaning Check List |
| Annexure – V | Control Sample Receiving Register |
| Annexure – VI | Template for Sample Quantity Details |
Annexure -I
Sampling Kit
| Sr.No. | Items |
| 1 | Appropriate numberof “under test” labels. |
| 2 | “Sampled” labels. |
| 3 | “Sample for Analysis” label. |
| 4 | “Control sample” label. |
| 5 | Appropriate number of small self sealing poly bags/bigger LDPE bag/glass bottle |
| 6 | Appropriate number of sampling spatula/sampling device/sampling rod |
| 7 | Scissors/ cutters |
| 8. | BOPP Tape |
| 9 | Plastic seal/nylon thread |
Annexure-II
Sampling Check List
Material Name: __________________________ Batch. No.:_____________
Batch no. : ___________________________Date : _____________
| Sr. No. | SAMPLING INSPECTION PARAMETER | OBSERVATION |
| 1 | Physical condition of consignment | Satisfactory/ Not satisfactory |
| 2 | Source of material | Approved vendor/ Not approved |
| 3 | Certificate of analysis from vendor | Received/ Not received |
| 4 | Name of Manufacturer & Supplier | Available / Not available |
| 5 | Cleaning of surrounding area of consignment | Satisfactory/ Not satisfactory |
| 6 | Consignment sealed with uniform sealing from vendor | Yes/ No |
| 7 | Proper consignment label affixed by the vendor | Yes/ No |
| 8 | Proper Quarantine label affixed by warehouse | Yes/ No |
| 9 | Generic / Patent name available on label | Yes/ No |
| 10 | Batch Number | Present / Not Present |
| 11 | Manufacturing Date | Present / Not Present |
| 12 | Expiry Date/ Retest Date/ Reevaluation Date | Present / Not Present |
| 13 | Storage condition | Present / Not Present |
| 14 | Location as Per Standard | AC/ NON AC |
| 15 | Material received at Standard Packing | Yes/ No |
| 16 | Number of Packages | |
| 17 | Colour of material | |
| 18 | Odour of material | |
| 19 | Appearance of material | |
| 20 | Foreign matters if any | |
| 21 | After sampling resealing of boxes done | |
| 22 | Any abnormal observation |
Sampled By: Reviewed By:
Date : Date :
Annexure -III
Sampling Log Book
| Date | RLAF Start Time | Pressure Differential Reading Across HEPA | Pressure Differential Reading Across Prefilter
|
Before Sampling Activity. Limit: Temp. NMT 25oc, Humidity: NMT 50% | Material Name and grade | GRN No. | B.NO
./Lot. No. |
A.R. No | No of Container in Consignment | Container For Sampling | Sampling tool ID No.
(/../…)
|
Balance ID used | Sampling time | After Sampling activity
Limit: Temp.: NMT 25oc, Humidity: NMT 50% |
RLAF Cleaning
(70% IPA) |
Sampling Tools Cleaning (0.1% teepol) | Area cleaning after Sampling | Remarks | ||||||||||||||
| Limit: 8 To 20 mm water | Limit: 2 To 8 mm water
|
Temp. | Humidity | Checked By | From | To | Temp. | Humidity | Checked By | From | To | Done By | Checked By | From | To | Done By | Checked By | From | To | Done By | Checked By | |||||||||||
Annexure –IV
Sampling of Raw materials area cleaning check list
Raw material to be sampled: __________________________________
Batch Number: _____________________________________________
A.R. Number:______________________________________________
Previous raw material sampled: _________________________________
Date: ______________________________________________________
| Sr. No. | Particulars | Cleaning status |
| 1 | Surrounding area of sampling room | Satisfactory /Not satisfactory |
| 2 | Over gowning room | Satisfactory /Not satisfactory |
| 3 | Sampling device | Satisfactory /Not satisfactory |
| 4 | Sampling room | Satisfactory /Not satisfactory |
| 5 | SS stool kept under RLAF | Satisfactory /Not satisfactory |
| 6 | RLAF | Satisfactory /Not satisfactory |
| 7 | Analytical Balance | Satisfactory /Not satisfactory |
Checked By: Verified By:
Sign/ Date: Sign/ Date:
Annexure – V
Control sample receiving register
| Date | Name of Material | Batch. No. | A.R. No. | Control Sample Quantity | Received by
Sign / Date |
Remark |
Annexure VI
Template for sample quantity details.
| Sr.
No. |
Name of Raw material | Quantity from individual container for identification | Quantity sample for Chemical Analysis
(NLT) |
Quantity sample for Microbial Analysis
(NLT) |
Quantity for
Control sample (NLT) |
| Prepared By | Reviewed By | Approved By | |
| Sign & Date | |||
| Designation |
