Retesting of Raw and Packaging Material Standard Operating Procedure

SOPs

Purpose:

The purpose of this procedure is to describe the process for retesting of raw material and packaging materials (before retest date).

Scope:

This procedure is applicable for all raw materials (APIs and excipients) and some packaging materials received in XX Pharmaceuticals Limited.

Definitions/Abbreviation:

[][]SOP: Standard Operating Procedure.
[][]QC: Quality Control.
[][]API: Active Pharmaceuticals Ingredients

Responsibilities:

The roles and responsibility is as follows:

Officer/Executive/Sr. Executive, QC & Microbiology

[][]To ensure that the instructions of this procedure are correctly followed.
[][]To maintain the records properly as per SOP.

Executive, Warehouse

[][]To send retest request to QC in time.
[][]To ensure availability of containers to be sampled from quarantine area to the sampling booth and their replacement after sampling.
[][]To ensure cleanliness of Sampling booth and containers to be sampled.

Manager, Quality Control

[][]To ensure that this procedure is kept up to date.
[][]To confirm that the SOP reflects the required working practices.
[][]To arrange training on the SOP to all concerned personnel and to ensure implementation of the SOP after training.

Head of Quality Assurance

[][]Approval of the SOP.
[][]To ensure the overall implementation of the SOP.

Procedure:

[][]Mention the retest date on passed label at the time of first release.
[][]Frequency of re-testing will be one year from test date.
[][]If the next retest date exceeds the expiry date, assign the retest date same as expiry date.
[][]The expiry date provided by the manufacturer will not be extended in any circumstances for active raw material.
[][]In case of excipients and packaging material, the expiry date may be extended on the basis of retest result if the expiry date is mentioned as best before/use before/retest date in manufacturer’s COA.
[][]In such cases, recommended expiry will be assigned instead of expiry and the next retest frequency will be every six months.
[][]The expiry date may be extended as per manufacturer’s recommendation.
[][]If there is no manufacturer’s recommendation, the expiry date may be extended twice for every six month up to one year from expiry date on the basis of retest result.
[][]Executive, warehouse will raise ‘Retesting Advice Form’ (as per Annexure-I) by ERP for the identified raw/packaging materials subject to retest or expiry.
[][]In case of material to be retested, warehouse will send the retest advice form at least 7 days before the retest date and QC will test and release/reject retested material within the retest date.
[][]In case of material to be expired, warehouse will send the retest advice form on the expiry date and QC will reject the expired material after necessary entries in retest advice form.
[][]QC will receive retesting advice form from warehouse and enter necessary information in Raw Material Register and assign the new Lab. Control No. for retest as below:
e.g. Lab. Control No./R1
Where, Lab. Control No. is of the identified material subject to retest.
/ is separator
R1 is retest for first time (e.g. R1, R2…..)
[][]Take sample from last used container for active and excipients sufficient for necessary retest parameters to relevant test specification.

[][]Collect sample following SOP for Raw material sampling and release procedure SOP for Packaging material sampling and release procedure and affix ‘UNDER RETEST’ label on the previous ‘PASSED’ label in cascading manner.

Carryout the following tests for each raw material

[][]Description/Appearance
[][]LOD/Water Content/Moisture Content
[][]Chromatographic Purity/Related Substance
[][]Assay
[][]pH/Acidity/Alkalinity test
[][]Microbial limit test
[][]Bacterial Endotoxin test
[][]Other relevant test (If necessary)
[][]Carry out required tests as described in the respective test method.
[][]Record analytical raw data in analytical worksheet and analyst logbook. Entry all results in certificate of analysis in ERP.
[][]Verify the test report against specification in ERP.
[][]Follow SOP for handling of out of specification if the test result does not comply with the specification.
[][]After approval/rejection, take print out the COA and two copies of approved ‘Retesting Advice Form’.
[][]Attach the retest report and related documents with the previous test reports.
[][]Prepare the required number of status labels (PASSED/REJECTED) for retested material.
[][]QC will send a copy of approved ‘Retesting Advice Form’ to warehouse.

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Manufacturing Trend Analysis Standard Operating Procedure

Quality Control, SOPs

Manufacturing Trend Analysis, Purpose:

Manufacturing Trend Analysis, the purpose of this SOP is to define a procedure for trending of manufacturing data and to ensure that management reviews the trends and takes appropriate action.

Manufacturing Trend Analysis, Scope:

This procedure is applicable for all products manufactured at general block and are analyzed in Quality Control and Microbiology Laboratory of XX Pharmaceuticals Limited.

Definitions / Abbreviation:

[][]SOP: Standard Operating Procedure.
[][]QC: Quality Control.

Responsibilities:

[][]The roles and responsibility is as follows:
[][]Executive/Executive, QC & Microbiology
[][]To ensure that the instructions of this procedure are correctly followed.
[][]To maintain the records properly as per SOP.

Manager, Quality Control

[][]To ensure that this procedure is kept up to date.
[][]To confirm that the SOP is technically sound and reflects the required working practices.
[][]To arrange training on the SOP to all concerned personnel and to ensure implementation of the SOP after training.
[][]To ensure effective assessment of trend analysis of Product.
[][]Take correction action to prevent reoccurrence.

Head of Quality Assurance

[][]Approval of the SOP.
[][]Review all trend analysis to take appropriate action.
[][]To ensure the overall implementation of the SOP.

Procedure:

[][]Manager, Quality control will issue the ‘Finished Product Trend Card’ (Annexure-I) by making entry in the ‘Trend Card Issue Register’ (Annexure-II)
[][]QC Executive will make entry in ‘Finished Product Trend Card’ and MS Excel format at the time of report submission.

Trend the following key parameters by QC Executive taken from IPC data:

Tablet:

[][]Disintegration Test
[][]Average weight

Capsule:

[][]Disintegration Test
[][]Filled weight

Powder for suspension:

[][]Filled weight
[][]Trend the following key parameters by QC Executive taken from analytical data:

Tablet:

[][]Assay (Active content)
[][]Dissolution Test (if applicable)

Capsule:

[][]Assay(Active content)
[][]Moisture content
[][]Dissolution Test (if applicable)

Powder for suspension:

[][]Assay (Active content)
[][]Moisture content
[][]Dissolution Test (if applicable)
[][]Quality Control Manager will review the trend at the time of report approval.
[][]If there are any atypical findings that indicate potential quality or performance issues, then follow the below instruction:
[][]Carry out an immediate laboratory investigation as per procedure for out of specifications. But this action will not prevent from releasing the batch to commercial.
[][]If the laboratory investigation indicates that there is no laboratory error, then it must be reported to AGM, Quality Assurance to conduct an investigation and take action to bring the situation in control.
[][]Preserve all the data securely for Periodic Product Review.

List of Annexure:

Annexure-I: Finished Product Trend Card
Annexure-II: Trend Card Issue Register

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Raw Material Sampling and Release Standard Procedure

Quality Control, SOPs

Raw Material Sampling and Release, Purpose:

Raw Material Sampling and Release, the purpose of this procedure is to describe the process for sampling and release of the raw materials (actives and excipients).

Raw Material Sampling and Release, Scope:

This procedure is applicable for all raw materials (APIs and Excipients) received in XX Pharmaceuticals Limited.

Definitions/Abbreviation:

[][]QC: Quality Control
[][]API: Active Pharmaceuticals Ingredients
[][]GRN: Goods Received Note
[][]CoA: Certificate of Analysis
[][]AQL: Acceptance Quality Limit
[][]BOPP: Bi-axially Oriented Polypropylene
[][]Mfg. Date: Manufacturing Date
[][]Exp. Date: Expiry Date
[][]ERP: Enterprise Resource Planning
[][]SS: Stainless Steel

Responsibilities:

The roles and responsibility is as follows:

Officer/Executive, QC and Officer/Executive, Microbiology

[][]To ensure that the instructions of this procedure are correctly followed.
[][]To maintain the records properly as per SOP

Executive, Warehouse

[][]To ensure availability of containers to be sampled from quarantine area to the sampling booth and their
replacement after sampling.
[][]To ensure cleanliness of sampling booth and containers to be sampled.

Manager, Quality Control

[][]To ensure that this procedure is kept up to date.
[][]To confirm that the SOP reflects the required working practices.
[][]To arrange training on the SOP to all concerned personnel and to ensure implementation of the SOP after training.

Head of Quality Assurance

[][]Approval of the SOP.

Procedure:
General Precaution(s):

[][]Take sample for microbial testing first followed by other sampling.
[][]Use clean and dry sampling device for sampling.
[][]Use sampling device after moping with freshly prepared 70% IPA for collecting the sample for microbiological limit test.
[][]Material of only one consignment shall be sampled at a time.
[][]Use different sampling devices for sampling of different materials.
[][]For sampling of volatile and hazardous chemicals and solvents, follow instructions as given in their handling procedures.
[][]All solid as well as liquid raw materials except solvents are to be sampled in sampling booth.

Sampling: Raw Material Sampling and Release

[][]Receive the GRN for raw material from the warehouse then compare with Manufacture’s CoA and enter the details (GRN Received Date, GRN No., Lab. Control No., Name of material, Code No., Invoice/Challan No., Manufacturer Lot No., Manufactured by, Supplied by, Mfg. Date, Exp. Date, Qty. received, Received by & date) in the Raw Material Register (as per Annexure-I) maintained in QC department.
[][]If the Manufacture’s CoA is not received, inform to Supply Chain Department.
[][]Ensure that material is received from Approved Vendor.
[][]If the material is not from Approved Vendor, then the material is not to be sampled.
[][]Assign the work of sampling of the material to the QC Executive.
[][]Share the copy of GRN and Manufacturer CoA with Microbiology Laboratory, when required.
[][]Inform Warehouse to ensure cleanliness of sampling area and fill-up the Cleaning Checklist before Sampling of Raw Materials (Annexure-VIII) and then start-up of sampling booth.
[][]Assigned QC Executive will take required no. of “SAMPLED” label as per labeling SOP.
[][]Assigned QC Executive will prepare and checked ‘SAMPLING IN PROGRESS’ label (as per Annexure-II); prepare required containers/poly bags for sampling according to sampling plan for the material to be sampled.

Sampling plan

[][]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.
[][]In case of all excipient, 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 = 4.16 ≈ 5 containers.

Sampling container

[][]Select the sample container according to the nature of the material to be sampled.
[][]Use clean fresh poly bags for solid materials.
[][]Use clean dry glass bottle with screw cap for liquid, dry amber glass bottle with screw cap for light sensitive liquid and transparent stoppered flask for solvents.
[][]Use sterilized screw capped conical flask (autoclaved at 121°C for 15 minutes) for sampling of raw material for microbial test.
[][]Sample all light sensitive solid materials in black polyethylene bag.
[][]Sample all the moisture sensitive materials in air tight container.

Sampling note: Raw Material Sampling and Release

Solid

If the material is in paper bag, take the sample by cutting a small ‘V’ on the bag and in case of Drum open the lid & inner polyethylene then push the Sampling thieve and take sample into a labeled poly-bag. Then place a clean poly-bag over the tear area and properly seal the poly-bag with adhesive tape. In case of Drum, tie the inner-polyethylene with rubber band/cable tie, finally twist the lid properly.

Liquid

Deep the liquid sampling device vertically into the sample drum and collect the sample or pipette after gently stirring the liquid and transfer the liquid sample to a labeled, cleaned container. Solvent in distorted metal drum must be sampled in addition to the rule of Ön + 1. Sample all flammable solvents in solvent dispensing room.

Sampling device

Use stainless steel sampling devices specially designed for solid and liquid material.

[][]For solid materials received in drums/container use specially designed S.S. sampling device by which material can be sampled from different level (thief sampler).
[][]For liquid and solvents received in drum, use specially designed S.S. drum sampler.
[][]For liquid material received in small container use specially designed small SS liquid sampler.
[][]For solid material received in bags use specially designed SS solid sampler/SS spoon.
[][]For microbiology analysis, use screw capped conical flask/glass bottle and SS spoon (autoclaved at 121°C for 15 minutes).
[][]Clean and maintain the sampling device (tools) as per SOP for cleaning and storage of sampling tools after completion of sampling.

Damaged containers or torn bags

[][]Check the physical condition and cleanliness of raw material containers before opening for sampling.
[][]If any container found in damaged condition, intimate warehouse in-charge.
[][]Damaged containers whose integrity is doubtful should be sampled and tested separately.
[][]Inform warehouse in-charge to take initiatives for repacking of damaged container or torn bags if necessary.

Gowning  procedure

[][]Wear fresh gown before entering into sampling booth.
[][]Wear sterile gloves, mask before sampling for microbiology analysis.
[][]Cover the hands with gloves and wear a cap and mask to cover hair and nose respectively.
[][]Cover the footwear with shoe cover.
[][]Use separate apron, nose mask, hand gloves, cap & shoe covers for sampling of different material.
[][]Mop the hands with 70% IPA and air dry before proceeding for sampling and particularly when samples are to be drawn for Microbiological testing.

Sampling procedure

[][]Check the Cleaning Checklist before Sampling of Raw Material (as per Annexure-VIII).
[][]Inform Warehouse before going for sampling to arrange the raw material containers which are to be sampled in sampling booth area and ensure the cleanliness of these containers externally, before bringing the container to be sampled to the sampling area.
[][]Enter the Warehouse (Raw Material) with sampling basket, sampling utensils, sampled label, poly-bags, GRN and ‘Sampling in progress’ label.
[][]Check the details given on the GRN with the suppliers label and ensure that the “Quarantine” label affixed by the warehouse personnel on all raw material containers of a consignment.
[][]Select number of containers/ bags as per sampling plan and inform Warehouse personnel to send the raw material containers to the material entry airlock.
[][]Check that ‘CLEANED’ label is affixed to the sampling booth and then affix the ‘Sampling in-progress’ label outside of the sampling booth. Enter the sampling booth.

Operate the sampling booth

[][]Receive the desired container(s) within material entry airlock. Check that the containers are free from dirt & dust externally. Do not sample the container/bag whose packing integrity has been lost (material has been exposed to environment).
[][]Take the raw material inside the sampling booth. Sample in a manner so that laminar airflow can be in operation without any interruption.
[][]Enter the information about the material sampled into the ‘Sampling Register’ i.e. Date, GRN No., Lab. Control No., Name of material, Code No., Manufacturer Lot no., Manufactured by,  Sampling start time (as per Annexure-IV).
[][]Wear disposable hand gloves just before start of sampling.
[][]Open the container for sampling one by one.
[][]Check the physical condition of the raw material for any gross abnormalities like dis-colourisation, lumps, foreign matter and physical heterogeneity. Record information in Raw Materials Sampling Report (as per Annexure-V).
[][]Collect the sample aseptically into sterile screw capped conical flask by sterilized sampling device for microbiology analysis.
[][]Assign the sampled Container No. as 1/25, 2/25, 13/25, 25/25 etc. with Reference to drum number of container sampled.
[][]Draw the sample from different levels of the container. (i.e. From Top, Middle & Bottom). The weight of the total sampled quantity should be according to List of Raw Material Sampling Quantity (prepared as per Annexure-III).
[][]For excipient, prepare composite sample by taking equal quantity of material from the sampled drum. Mix thoroughly in big polythene bag for retained sample and testing sample. For identification test take individual small quantity of sample from each sampled container.
[][]For active raw material, prepare composite sample during sampling for assay for every 10 containers of the consignment by taking equal quantity of material from individual sampled container. Mix thoroughly in plastic bag to make sample for assay test. For complete analysis (except identification and assay) and retention sample make composite sample by taking equal quantity from all bags or container during sampling. For identification test take individual small quantity of sample from each container.
[][]Take the individual sample from each sampled container for microbiological analysis in sterile container, if specified.

Reseal the container properly after sampling as follows: Raw Material Sampling and Release

[][]Fibre/Plastic container pack: Shrink the inside poly bag by twisting it sufficiently. Bent it & tie it using cable tie. Place the lid of container & close it tightly & seal it.
[][]Woven and Paper Bag: Close the sampling point and seal it properly using BOPP tape.
[][]Liquid RM container: Place the lid of container & keep it tightly closed.
[][]Affix yellow colour duly filled & signed ‘SAMPLED’ label on each containers from which the samples are collected and ‘UNDER TEST’ label on all containers of a consignment.
[][]After completion of sampling switch off the sampling booth.
[][]Record sampling details in Raw Materials Sampling Report (as per Annexure-V).
[][]Enter the Sampling end time, Sampled quantity, Sampled by and Remarks (if any) into the ‘Raw Material Sampling Register’ (as per Annexure-IV).
[][]Place the used sampling device in container labeled as ‘TO BE CLEANED’ containing a poly bag.
[][]Shift sampled container outside the sampling booth.
[][]Inform warehouse personnel to transfer it to quarantine area.
[][]Leave sampling booth and affix ‘TO BE CLEANED’ label outside the sampling booth. Inform warehouse personnel for cleaning.
[][]Warehouse personnel will clean the sampling booth, enter the sampling booth cleaned by in ‘Raw Material Sampling Register’ (as per Annexure-IV) and then affix ‘CLEANED’ label outside the sampling booth.
[][]If any discrepancy found, immediately inform the warehouse in-charge.
[][]Keep the collected samples in the sample receiving room of QC Laboratory in dedicated rack for Raw Material or in refrigerator, if specified.
[][]Keep the retention sample in retention sample room or in refrigerator, if specified.
[][]Enter the sampled by (initial) and date in the ‘Raw Material Log Register’ (as per Annexure-I).

Release:

[][]Enter the sampled by (initial) and date in the ‘Raw Material Log Register’ (as per Annexure-I).
Issue the Raw Material Analytical Work Sheet (as per Annexure-VI) (for commercial raw material) with initial and date on every sheet to the analyst and enter the worksheet issued by (initial and date) in the ‘Raw Material Log Register’ (as per Annexure-I).
[][]Carry out the physical appearance and identification test separately for active raw material from each container.
[][]Microbiology will perform microbial limit test from all sampled container and bacterial endotoxins test from composite sample.
[][]Perform identification test of excipient from all sampled containers.
[][]For active raw materials, prepare sub-composite sample from each 10 container and then prepare composite sample from all the sub-composite samples. Perform the test of sub-composite sample if composite sample shows out of specification result to identify easily which container(s) is in problem. Retain all the sub-composite samples until release of the material.
[][]For active raw materials perform rest of the test as per the specification from the composite sample prepared from all containers. Carry out assay test from the composite sample and take result.
[][]For excipient perform the complete test as per specification from the composite sample prepared from the sampled containers.
[][]Check the appearance of capsule shell according to Sampling Plan for Normal Inspection of Capsule Shell (as per Annexure-IX).
[][]Test all parameters according to the Raw Material Specification and analyze the batch exactly as written in the method of analysis.
[][]Record all analytical raw data and calculations, and attach the printout of weight(s) in the analyst logbook.
[][]Fill up the Raw Material Analytical Work Sheet (as per Annexure-VI) and attach printout of required raw data.
[][]Weigh the sample ± 5.0% of specified quantity for assay test and ±10.0% of specified quantity for all other tests.
[][]Use bracket like [ ] to indicate that the result is taken from manufacturer’s/supplier’s certificate of analysis (CoA) (if available).
[][]Entry all data in previously created certificate of analysis for raw materials in ERP (as per Annexure-VII).
[][]Verify the test report with specification followed by Approval/Rejection in ERP.
[][]Follow SOP for handling of out of specification if the test result does not comply with the specification.
[][]After approval/rejection print out the COA and two copies of GRN under the heading of

  • Approved/Rejected quantity.
  • Date of Release/Rejected.
  • Approved/Rejected status.

[][]Submit all report to QC Manager for approval.
[][]Submit one copy of GRN with the initial with date of In-Charge, QC or his/her designee to store.
[][]Compile a bunch with CoA (as per Annexure-VII), filled Raw Material Analytical Work Sheet (as per Annexure-VI) and raw data, Raw Materials Sampling Report (as per Annexure-V), QC copy of GRN after approval.
[][]Fill up the Trend Card with necessary data.
[][]Prepare the required number of green “PASSED” label for passed.
[][]In case of Rejection, prepare the required no. of red “REJECTED” label.
[][]Fill up the Raw Material Rejection Form (as per Annexure-X) for rejection of raw material.
[][]Paste “PASSED”/“REJECTED” label in cascading manner (overlapping upto 3/4 th of the status bar of the previous label) over the “UNDER TEST” label without hiding any information of the previous label.

List of Annexes: Raw Material Sampling and Release

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Sampling Tools Cleaning and Storage SOP

Quality Control, SOPs

Sampling Tools Cleaning and Storage; Purpose:

Sampling Tools Cleaning and Storage; The purpose of this procedure is to describe the instruction of cleaning and storage of sampling tools.

Sampling Tools Scope:

This SOP is applicable to sampling tools used for Quality Control Laboratory and Microbiology Laboratory at XX Pharmaceuticals Ltd.

Definitions/Abbreviation:

[][]SOP: Standard Operating Procedure: A written authorized procedure, which gives instructions for performing operations.
[][]QC: Quality Control.

Responsibilities:

[][]The roles and responsibility is as follows:
[][]Laboratory Attendant, QC & Microbiology
[][]To prepare of cleaning solution.
[][]To clean and store all sampling tools by following SOP.
[][]Executive, QC & Microbiology
[][]To ensure that this procedure is followed.
[][]To maintain the records properly as per SOP.

Manager, Quality Control

[][]To ensure that this procedure is kept up to date.
[][]To confirm that the SOP is technically sound and reflects the required working practices.
[][]Arrange training on the SOP to all concerned personnel.
[][]To ensure implementation of the SOP after training.
[][]Schedule calibration of the instrument at the defined intervals.

Head of Quality Assurance

[][]Approval of the SOP.
[][]To ensure overall implementation of this SOP.

Procedure:

Precaution(s):
[][]Wear hand gloves, mask and protective clothing before cleaning of sampling tools.
[][]Be sure that the sampling tools are cleaned just after use.
[][]After cleaning of tools, be sure that the tools are free from any residual content of detergent or sample.
[][]During handling, sterilized gloves should be worn after sterilization of microbiology sampling tools.
Cleaning of Sampling Tools:

For scoop/spoon:

[][]Clean the sampling devices with potable water following by 0.5% soap or detergent solution.
[][]Finally rinse with purified water to remove the adhering material.
[][]Check the cleanliness physically and clean again if necessary.
[][]Dry in hot air oven for use in QC sampling.
[][]Sterilize at 2000C for 1 hour or autoclave at 1210C for 15 minutes for the sampling of Microbiology analysis.

For pipette (glass) and Glass Rods:

[][]Pass the running potable water through the pipette to remove the adhering material.
[][]Sink the pipette into 0.5% soap or detergent solution.
[][]Rinse with potable water to remove detergent.
[][]Finally rinse with purified water.
[][]Confirm that the tools are cleaned properly, clean again if it is necessary.
[][]Dry in hot air oven for use in QC sampling.
[][]Sterilize at 2000C for 1 hour or autoclave at 1210C for 15 minutes for the sampling of Microbiology.

Storage of Sampling Tools:

[][]After dry, remove the cleaned tools from the oven and wrap the dry tools individually with cleaned polybag.
[][]Ensure that there is no exposure of sampling tools after wrapping the cleaned dried tools with polybag.
[][]Finally keep it at closed condition.
[][]Affix the tag “CLEANED” label duly signed with date on the sampling tools.
[][]Use the tools within 7 days sampling of Chemical test and within 24 hours for sampling of microbiology test.

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Sampling Booth Start-up, Operation and Cleaning

Quality Control, SOPs

Sampling booth Purpose:

The purpose of this SOP is to describe the operation and cleaning procedure of Sampling Booth in order to comply with cGMP standard.

Sampling booth Scope :
The scope of the procedure is applicable to the Sampling Booth installed at the Warehouse of general block of XX Pharmaceuticals Limited.

Definitions/Abbreviation:

[][]SOP: Standard Operating Procedure
[][]QC: Quality Control

Responsibilities:

The Roles and Responsibilities are as follows:

Officer/Executive/Sr. Executive, Quality Control

[][]To ensure that this procedure is followed.
[][]To maintain the records properly as per SOP.

Executive, Warehouse

[][]To ensure that this procedure is followed.
[][]To check & ensure cleaning of sampling booth.

Manager, Quality Control

[][]To confirm that the SOP is technically sound and reflect the required working practice.
[][]To arrange the training on the SOP to all concerned personnel and to ensure the implementation of the SOP after training.

Head of Quality Assurance

[][]To approve the Document
[][]To ensure the overall implementation of the SOP.

Procedure

Precautions:
[][]The working person must follow safety procedures of works.
[][]For any trouble, disturbance switch OFF the Sampling Booth.
[][]Don’t sampling solvent and flammable liquid inside the sampling booth

Operation

[][]Check the Sampling Booth first physically.
[][]Check electric connection and mechanical set up.
[][]Machine switch on.
[][]Light on and blower on.
[][]Open the door.
[][]After completion desired work clean the Laminar Unit properly.
[][]Close the door and switch off main switch.
[][]Switch ON Sampling Booth.
[][]Switch ON Light.
[][]Switch ON the Laminar Air Flow.
[][]Increase or decrease air flow by pressing up/down button.
[][]Operate the Sampling Booth for 30 minutes before starting sampling.
[][]Record the machine operation start time & end time and other parameters on the  Equipment Log Book’

Cleaning

[][]Remove dust from the Sampling Booth with a vacuum cleaner and then clean with lint free cloth.
[][]Clean the booth with wet mop.
[][]Wipe the water with lint free cloth.
[][]After final cleaning affix the ‘CLEANED’ label.
[][]Record the cleaning status in the ‘Equipment Log Book’.

Download Here:

[][]Annexure I: Equipment Log Book

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Instrument calibration Standard operating procedure

Engineering, SOPs

Instrument calibration Purpose:

Instrument calibration, This SOP ensures that all type laboratory instruments of QC, PD, IPQC, Microbiology and balances of Production department are appropriately calibrated and calibration status maintained on due time.

Scope :

This procedure is applicable for calibration frequency of all types of laboratory instruments installed in QC, PD, IPQC, Microbiology and balances of Production department of General Block of XX Pharmaceuticals Ltd.

Definitions :

[][]QC: Quality Control.
[][]ENG: Engineering department.
[][]PD: Product development.
[][]IPQC: In-process Quality Control.

Responsibilities:

The roles and responsibility is as follows:

Officer/ Executive

[][]Ensure that the instructions of this procedure are correctly followed.
[][]Ensure that all equipment’s are included in the Instrument list.
[][]Maintain and track the calibration schedule.
[][]Ensure that all equipment’s bear appropriate calibration label and are used after calibration.
[][]To verify the third party calibration report and raw data.

Manager, Quality Control

[][]Ensure that this procedure is kept up to date.
[][]Ensure that the calibration requirement are assessed and are fully documented for all pieces of the instrument.
[][]Ensure appropriate personnel from the section are trained on this procedure.
[][]Confirm that SOP is technically sound and reflects the required working practices.

Manager, Quality Assurance

[][]Approval of SOP.
[][]Approval of calibration frequency and calibration schedule.

Precaution(s):

[][]There are no significant hazards or special instructions relating to the process/activities described in this SOP.

Procedure:

[][]Calibrate the equipment regularly as per frequency stated in the instrument calibration frequency (prepared as per format in Annexure-I) and as per calibration due date stated in the instrument calibration schedule (prepared as per format in Annexure-II) for individual equipment.
[][]Review the instrument calibration frequency when new instrument is included.
[][]Review the instrument calibration schedule yearly.
[][]Mention the responsibility (Third Party / Supplier name) for external calibration and (calibrator name and department) for internal calibration.
[][]Calibrate the instrument within 3 days of calibration due for monthly calibration period, within 7 days of calibration due for 3 and 6 monthly calibration period and 15 days of calibration due for yearly calibration period.
[][]In case of any breakdown or replacement of any damaged part where calibration needs to be carried out, the calibration schedule will be reviewed accordingly.
[][]Executive/ Sr. Executive of respective department will intimate the Engineering department/ Supplier service engineer/ outside agencies for the calibration of the instruments/ equipments.
[][]Maintain all standards, reagents, instruments and equipments etc. required for calibration.
[][]Calibrate the instrument across the operating range at a frequency appropriate to the reliability and frequency of use. Tolerance must be specified and should reflect the manufacturer’s specification or process tolerance or whichever the tightest.
[][]Re-evaluate calibration requirement immediately if there is any change in the instrument in use.
[][]Calibration must be performed by trained personnel or by approved Third Party Service Engineer.
[][]Calibration record must include:
=>Equipment name, model number and instrument ID No.
=>The name of the person who carried out the calibration.
=>Date of calibration.
=>The date when calibration is next due.
[][]For calibration, use reference standards or reference instruments whose calibration is traceable.
[][]Store the calibration device, certified standard weight in a secure place.
[][]For internal calibration, affix the calibration sticker label “ CALIBRATED” (format of calibration labels should be as per SOP: Calibration management program, Ref. No. SOP/ENG/00Y/XX, where XX refers to current version no.), with performer initial, date of completion and calibration due.
[][]For external calibration, affix the calibration sticker provided by external calibrator with performer’s initial, date of completion and calibration due.
[][]If the instrument is found out of tolerance/ limit during calibration, a label ‘Out of calibration” will be affixed on the instrument (as per SOP: Calibration management program No. SOP/ENG/00Y/XX, where XX refers to current version no.).

Notify the relevant person/ department/ organization to repair (or replace if necessary) the instrument in a timely manner.

 

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Annexure I Instrument Calibration Frequency
Annexure II Instrument Calibration Schedule

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Assigning of laboratory control number for different items

Quality Control, SOPs

Assigning of laboratory control number; Purpose

The tenacity of this SOP is to define the procedure of assigning Laboratory control number (Lab. Control No.) of all type raw material, packaging material, water, intermediate, bulk and finished product that are analyzed in Quality Control and Microbiology Laboratory.

Assigning of laboratory control number; Scope

This procedure is applicable for all type of raw materials, packaging materials, water, intermediate, bulk and finished products of XX Pharmaceuticals Limited.

Definitions / Abbreviation:

[] GRN: Goods Received Note

[] Lab. Control No.: A system of alpha-numerical number which represents request for analysis of materials/ water/ products received from respective department.

[] QC: Quality Control.

[] SAF: Sampling Advice Form

Responsibilities

The roles and responsibility is as follows:

[] Sr. Executive/Executive, Quality Control & Microbiology

[] To confirm that this procedure is followed.

[] To maintain the records properly as per SOP.

Assistant Manager, Quality Control

[] To confirm that this procedure is kept up to date.

[] To check that the SOP reflects the required working practices.

[] Organize training on the SOP to all concerned personnel.

[] To confirm implementation of the SOP after training.

Head of Quality Assurance

[] To ensure the overall implementation of the SOP.

[] Take initiative to Approval of the SOP.

Procedure:

[] All newly delivered samples & the accompanying documents (e.g. test request) must be assigned a separate registration number.

[] Assign Laboratory control number (Lab. Control No.) in following way:

Put first two or three letters according to the abbreviations mentioned below –

  • BBW     Boiler Blowdown Water
  • BFW     Boiler Feed Water
  • CTW     Cooling Tower Water
  • DW       Drinking Water
  • EM       Environment Monitoring
  • ET        Endotoxin Test
  • ETP      Effluent Treatment Water
  • FP        Bulk Product (Semi-Finished)
  • GMB     General Microbiology
  • PM       Packaging Material
  • PMS     Packaging Material of Source Approval
  • PSC     Purified Steam Condensate
  • PTW     Potable Water
  • PW       Purified Water
  • RM       Raw Material
  • RMS     Raw Material of Source Approval
  • SHC     Sodium Hypochlorite
  • ST        Sterility Test
  • STB      Stability Sample
  • WFI      Water for Injection
  • WW      Wash Water

Write down a hyphen (-) after the abbreviation, then serial number consist of three digits i.e. 001, then a  slash and put two digits of month i.e. 08 for month August.

Again write down a slash (/) then last two digits of the year i.e. XX for year 20XX. For example, first raw material received on August 20XX will get the Lab. Control No.: RM-001/08/XX.

GMB will be included before abbreviation of each test in case of microbiology lab control no./lab reference no. and put slash (/) after that.

Record Lab. Control No. in Register against each GRN / SAF.

Record the same in respective documents and status label also.

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Specification and analytical method preparation and review

Quality Control, SOPs

Specification and analytical method; Purpose

The tenacity of this SOP is to define the procedure for preparation, review & approval of specification & analytical methods in quality control & microbiology laboratory.

Scope

This procedure is applicable for all raw materials (APIs and excipients), water, packaging materials and finished products of  XX Pharmaceuticals Limited.

Definitions/Abbreviation:

[] COA: Certificate of Analysis

[] ERP: Enterprise resource planning

[] PMS: Packaging material specification

[] QA: Quality Assurance

[] QC: Quality Control

Responsibilities

The roles and responsibility is as follows

Officer/Executive/ Senior Executive, Quality Control

[] To confirm that this procedure is followed.

[] To retain the records properly as per SOP.

Assistant Manager, Quality Control

[] To confirm that this procedure is kept up to date.

[] To ensure that the SOP is technically sound & reflects required working practices.

[] Arrange training on the SOP to all concerned personnel.

[] To confirm implementation of the SOP after training.

Head of Quality Assurance

[] Take initiative to approval of SOP.

[] To ensure overall implementation of this SOP.

Procedure

Precaution(s)

There is no significant precaution or special instructions relating to the activities described in this SOP.

Preparation
  • Enter code no. in ERP, then assign the specification reference number using the format and the analytical method reference number using the specific format
  • Check whether, material is included in different Pharmacopeia [BP/EP/USP] or not.
  • Prepare specification & analytical method strictly align with Pharmacopeia if the material is included in BP/EP/USP.
  • Prepare specification & analytical method strictly align with Manufacturer’s guides/COA /analytical methods if the respective raw material or packaging material is not encompassed in BP/EP/USP. Include any additional test parameter as internal requirement.
  • QC will share rest of the QC test sample & raw data with PD. PD will suggest to include any in-house parameter in specification (as when required/not).
  • Compare specification & analytical method received from two or more suppliers; prepare specification & analytical method based on the suitable one based on feasibility study on site. Discuss with the concerned suppliers in case any difference identified.
  • For printed packaging material, Officer/Executive, QC will receive copy of artwork & approved shade card/design from QA and then prepare the specification and transfer to QA for approval. After approval of the specification, QC will receive control copy of specification along with artwork and approved copy of shade card/design from QA.
  • QC will prepare specification for unprinted packaging materials (Foil, Sachet, PVC/ PVDC Film etc.).
  • The issue date & review date should be in the day-month-year (dd-month-yyyy) format i.e. 25-August-20YY.
  • Assign two years review time for next revision from date of preparation for specifications and analytical methods.
  • For draft specification & analytical method; assign one year review time from date of preparation.
  • Follow respective standard format (as per concerned Annexure) for the preparation of specification & analytical method.
  • Enter final specification of raw material & packaging material in the ERP.
Review
  • Review specification & analytical method from draft to final one & change version no. to next one.
  • Review final specification & analytical method with a proper change control procedure when any change   is necessary.
  • Review method & specification if there is any change in respective Pharmacopeia. Put a new version number with a new review date.
  • If no modification is required at the time of review, then use subsequent review portion assign next expiry date 2 years from the review date and use the same.
Approval
  • Check analytical method & specification.
  • Manager, QA or Manager, QC will give approval after ensuring that each page of the document has been signed by person who prepared & person who checked specification after its finalization.
  • Keep master document in QA department.
  • Keep controlled copy in the QC & Microbiology department (as when required).
  • Retrieve previous specification & analytical method by revised one after review. Treat previous one as ‘OBSOLETE’.
  • Keep the ‘OBSOLETE’ copy in a file after stamping as ‘OBSOLETE’ in red ink
  • Discard the ‘OBSOLETE’ specification least after two years from the date of obsolete.

 

Download All Annexure here

Annexure I Format for Packaging Material Specification

Annexure II Format for Raw Material or Water Specification

Annexure III Format for Finished Product Specification

Annexure IV Format for Analytical Method of Raw Material or Water

Annexure V Format for Analytical Method of Packaging Material

Annexure VI Format for Analytical Method of Finished Product

 

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HPLC analysis and system suitability check procedure

Quality Control, SOPs

HPLC analysis and system suitability; Purpose:

The purpose of this SOP is to describe the procedure for HPLC analysis and checking of system suitability.

HPLC analysis and system suitability; Scope

This procedure is applicable to all HPLC analysis that will be carried out in quality control laboratory of XX Pharmaceuticals Limited.

Definitions/Abbreviation
  • Standard Operating Procedure (SOP)
  • Standard Operating Procedure. A written authorized procedure, which gives instructions for performing operations.
  • HPLC: High performance liquid chromatography
  • QC: Quality Control
  • RSD: Relative standard deviation
Responsibilities

The roles and responsibility is as follows:

Officer/Executive/ Senior Executive, Quality Control

  • To ensure that the instructions of this procedure are correctly followed.
  • To maintain the records properly as per SOP
Assistant Manager, Quality Control
  • To confirm that this procedure is kept up to date.
  • To check that the SOP reflects the required working practices.
  • To organize training on the SOP to all concerned personnel & to ensure implementation of the SOP after training.
Head of Quality Assurance
  • Take initiative to approval of the SOP.
  • To confirm the overall implementation of the SOP.

Procedure:

General Precaution(s):

  • Ensure that the mobile phase is filtered and degassed properly by sonication before use.
  • Suggested injection procedure should be run in one single sequence.
Analytical procedure:
  • Prepare desired mobile phase, filtered by 0.22 or 0.45 µm membrane filter & degassed for at least 5 minutes with the help of sonication.
  • Equilibrate the column for at least 30 minutes or more until baseline gets stabilized with desired mobile phase & check the baseline to ensure the system is ready for injection.
  • Prepare standard solution & assay sample and keep record of weights.
  • At first inject blank to confirm the absence of unknown peak at the retention time of Principal peak & then inject standard solution to check retention time of the principal peak of interest. Run chromatogram minimum 2 minutes extra after principal peak elution is over and peak is properly integrated.
  • Unless otherwise specified in the individual method, data from five replicate injections of standard are used to calculate RSD, if the requirement is 2.0% or less; data from six replicate injections are used if the RSD requirement is more than 2.0%. Tailing factor of principal peak of interest should be between 0.8 and 1.5 unless otherwise stated in individual method.
  • Inject standard & assay preparation solution into the HPLC system as per suggested injection procedure previously mentioned.
  • Following are the suggested injection procedure to be followed unless otherwise specified in respective method.
Injection procedure for test homogeneity of Blend/Granules sample
Sample ID with No. of Injection
  • Blank: 1 Time
  • Resolution or System Suitability solution (If applicable) : 1 Time
  • Standard: 5 Times
  • Sample-1: 1 Time
  • Sample-2: 1 Time
  • Sample-3: 1 Time
  • Sample-4: 1 Time
  • Sample-5: 1 Time
  • Sample-6: 1 Time
  • End Standard: 1 Time
Injection procedure for Assay
  • Blank: 1 Time
  • Resolution or System Suitability solution (If applicable) : 1 Time
  • Standard: 5 Times
  • Sample: 1 Time
  • End Standard: 1 Time
Injection procedure for dissolution
  • Blank: 1 Time
  • Resolution or System Suitability solution (If applicable) : 1 Time
  • Standard: 5 Times
  • Sample-1: 1 Time
  • Sample-2: 1 Time
  • Sample-3: 1 Time
  • Sample-4: 1 Time
  • Sample-5: 1 Time
  • Sample-6: 1 Time
  • End Standard: 1 Time
Injection procedure for Content Uniformity
  • Blank: 1 Time
  • Resolution or System Suitability solution (If applicable) : 1 Time
  • Standard: 5 Times
  • Sample-1: 1 Time
  • Sample-2: 1 Time
  • Sample-3: 1 Time
  • Sample-4: 1 Time
  • Sample-5: 1 Time
  • Sample-6: 1 Time
  • Sample-7: 1 Time
  • Sample-8: 1 Time
  • Sample-9: 1 Time
  • Sample-10: 1 Time
  • End Standard: 1 Time
  • For injection of more than 12 samples, run end standard after every 12th sample.
  • Calculate the result comparing the area of sample solution with the average area of 5th standard (6th standard if six replicate injections required) and respective end standard.
Chromatogram review and documentation:

The custom report covers the following information and can be modified as per the specific need.

  • Acquired by
  • Sample Name
  • Sample ID
  • Tray No.
  • Vial No.
  • Injection Volume
  • Data File
  • Method File
  • Batch File
  • Date Acquired
The peak table in custom report for standard covers the following data, however select other data as per requirement.
  • Title
  • Sample Name
  • Sample ID
  • Ret. Time
  • Area
  • Theoretical Plate
  • Tailing Factor
  • Resolution

The peak table in custom report for sample covers the following data, however select other data as per requirement.

  • Title
  • Sample Name
  • Sample ID
  • Ret. Time
  • Area
  • Result
  • Unit
General guideline:
  • In the test for Assay, run all Standard & Sample chromatograms minimum 2 minutes extra after the principal peak elution is over & peak is properly integrated or as per the method.
  • In Chromatographic Purity/Degradation/Related Substances, run the chromatogram 2.5 times the retention time of principal peak or as specified in individual method. In case of specific impurity analysis, run the chromatogram minimum 2 minutes extra after the principal peak elution is over and peak is properly integrated.
Allowable modification in chromatographic system:

Following are general criteria, which provide extent of allowable variation to get system suitability. The adjustments are allowed only to improve quality of chromatography unless otherwise directed in the respective method/pharmacopoeial monograph.

pH of mobile phase:

pH of aqueous buffer used in mobile phase preparation can be adjusted to within ± 0.2 units of the value or range specified. (Example: If specified pH is 7.0 then allowable limit for adjustment is 6.80 – 7.20)

Concentration of salts in buffer:

Concentration of salts used in the preparation of aqueous buffer employed in mobile phase can be adjusted within ± 10% if the permitted pH variation is met. (Example: If specified concentration is 1.0% then allowable limit for adjustment is 0.90%–1.10%)

Ratio of components in the mobile phase

Following adjustment limits apply to minor components of the mobile phase (specified at 50% or less). The amount(s) of these component(s) can be adjusted + 30% relative. However the change in any component cannot exceed + 10% of absolute (i.e. in relation to the total mobile phase). Adjustment can be made to one minor component in ternary mixture. Examples of adjustments for binary and ternary mixture are given below.

Binary mixtures

Specified ratio of 50:50: 30% of 50 is 15% absolute, but this exceeds the maximum permitted change of + 10% absolute in either component. Therefore, the mobile phase ratio may be adjusted only within the range of 40:60 to 60:40.

Specified ratio of 2:98: 30%of 2 is 0.6% absolute. Therefore the maximum allowed adjustment is within the range of 1.4:98.6 to 2.6:97.4.

Ternary Mixtures

Specified ratio of 60:35:5: For the second component, 30% of 35 is 10.5% absolute, which exceeds the maximum permitted change of + 10% absolute in any component. Therefore the second component may be adjusted only within the range of 25% to 45% absolute. For the third component, 30% of 5 is 1.5% absolute. In all cases, a sufficient quantity of the first component is used to give a total of 100%. Therefore, mixture range of 50:45:5 to 70:25:5 or 58.5:35:6.5 to 61.5:35:3.5 would meet the requirement.

Detector wavelength
  • Deviations from the wavelengths specified in the method are not permitted.
  • Stationary phase:
  • Column length: ±70%.
  • Column internal diameter: ±25%.
  • Particle size: Maximum reduction of 50%, No Increase    permitted.
  • Flow rate: When the particle size is changed, the flow rate may require adjustment, because smaller particle columns will require higher linear velocities for the same performance (as measured by reduced plate height). Flow rate changes for both a change in column diameter and particle size can be made by:

F2=F1x [(dc22xdp1)/( dc12xdp2)]

Where F1 and F2 are the flow rates for the original and modified conditions, respectively; dc1 and dc2 are the respective column diameters; and dp1 and dp2 are the particle sizes.

When column dimensions are changed, the flow rate may be adjusted using the following equation:

F2=F1x [(l2d22/( l1d12)]

Where F1 and F2 are the flow rates for the original and modified conditions, respectively; l1 and l2 are the respective column lengths; and d1 and d2 are the diameters.

  • Injection volume: Injection volume can be reduced as far as consistent with acceptance precision and detection limits; no increase is permitted.

Column temperature: ±10°C.      F2=F1x [(l2d22/( l1d12)]

This is all about

HPLC analysis and system suitability.

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HPLC Column Washing Procedure in best effective way

Quality Control, SOPs

HPLC Column Washing Procedure; Purpose

The tenacity of this SOP is to define the procedure for washing of HPLC column to avoid any intrusion on repeated usage & to escalation column lifespan.

HPLC Column Washing Procedure; Scope

This procedure is applicable for all HPLC columns used within quality control laboratory of XX Pharmaceuticals Limited.

Definition: 
  • COA: Certificate of analysis
  • HPLC: High performance liquid chromatography
  • QC: Quality Control
  • SOP: Standard Operating Procedure
Responsibilities

The roles and responsibility is as follows

Senior Executive/Executive, Quality Control
  • To confirm that the instructions of this procedure are correctly followed.
  • To accomplish the HPLC column washing properly in accordance with this SOP.
  • To keep record of HPLC column washing time properly.
Manager, Quality Control
  • To confirm that this procedure is kept up to date.
  • To ensure that the SOP reflects the required working practices.
  • To assemble training on the SOP to all concerned personnel and to confirm implementation of the SOP after training.
Head of Quality Assurance
  • Take initiative to approval of the SOP.
  • To confirm the overall implementation of the SOP.
Procedure
  • Use HPLC grade solvents for column washing.
  • Freshly prepared, filtered and degassed solvent or solution should be used.
  • Purge solvent line to make them free from air bubbles.
  • Do not change flow rate at increment greater than 0.2 ml/min.
  • Keep column with proper end fitting during storage.
  • Do not over make tighter the column end fittings.
Pre-Wash (mobile phase run/ Prior to analysis) procedure
  • Set column on column compartment of HPLC.
  • Select shipping solvent, from COA of respective manufacturer, If not mentioned in COA, store the column based on column properties like Nitrile /ODS/Amine group etc.
  • Run shipping solvent (e.g. Azide solution, 65% Acetonitrile,) mentioned in COA of respective manufacturer for 15-20 minutes.
  • Gradually change the organic phase composition depending on the organic phase composition in mobile phase to reach the same in mobile phase. For example, gradually decrease the organic phase from 65% Acetonitrile (in shipping solvent) & finally reach 30% Acetonitrile (in mobile phase). For the Gradient HPLC this can be conducted through time program and for Isocratic HPLC, this can be done using intermediate solvents, as appropriate. Accomplish this run within 15 to 20 minutes.
  • Change line with mobile phase & execute HPLC analysis.
Post-Wash (mobile phase run /after completion of analysis) procedure
  • For mobile phase containing Buffer and counter ion
  • Replace mobile phase with purified water. Purge line. Run same for 15-20 minutes.
  • Depending on shipping solvent, gradually reach the same. For example, if 65% Acetonitrile is shipping solvent, then start with 100 % purified water and gradually increase the organic phase and finally reach at 65% Acetonitrile. For the Gradient HPLC this can be conducted through time program and for Isocratic HPLC, this can be done using intermediate solvents like 15%, 30%, 45% Acetonitrile, as appropriate. Accomplish this run within 55-60 minutes conducting each solvent composition period 15-20 minutes.
For mobile phase without buffer and counter ion

Depending on the shipping solvent, gradually reach the condition from the organic phase composition of mobile phase. For example, if 65% Acetonitrile is shipping solvent and organic phase composition in mobile phase is 30% Acetonitrile, then start with the initial organic phase of 30% Acetonitrile (70% Purified water) and gradually increase the organic phase and finally reach at 65% Acetonitrile. For the Gradient HPLC this can be conducted through time program and for Isocratic HPLC, this can be done using intermediate solvents as appropriate. Accomplish this run within 55 to 60 minutes conducting each solvent composition period 15 to 20 minutes.

 For mobile phase containing tri-ethyl amine
  • Replace the mobile phase with a mixture of methanol and 0.05% phosphoric acid (50:50 v/v) & run for 30 minutes.
  • Depending on the shipping solvent, gradually reach same. For example, if 65% Acetonitrile is storing solvent, then start with 20 to 30% Acetonitrile & gradually increase the organic phase and finally reach at 65% Acetonitrile. For the Gradient HPLC this can be conducted through time program and for Isocratic HPLC, this can be done using intermediate solvents as appropriate. Accomplish this run within 55 to 60 minutes conducting each solvent composition period 15 to 20 minutes.
  • Stop run. Remove column from HPLC unit, do end capping properly both ends &  place in respective column box.
  • Store column box in an allocated place.
  • Record HPLC column washing time after analysis in logbook for operation of HPLC.

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