ORAL DOSAGE FORM SOPs

1.0 PURPOSE

To provide an Instruction for handling of samples sent to public testing laboratory

2.0 SCOPE: 

This SOP is applicable to all quality control and microbiological laboratories.

5.0 PROCEDURE:

5.1 Analyst shall check the Specification / Standard Testing Procedure of the respective sample received in QC for tests that can be done In-house.

5.2 Analyst shall identify tests which need to be tested at Public testing laboratory. Plan all stability samples analysis In-house only. In case of exceptions (e.g. non-availability of instrument due to breakdown, non availability of resources etc.) outsource samples to external public testing laboratories and handle the same through approval of temporary change control.

Note: QA shall ensure the status of approval from regulatory agency and customer e.g. relevant

5.3  Analyst shall pack the samples in air tight clean, dry glass vial or in polybag or in any suitable container.

5.4 Pack the samples as mentioned with data logger. Place the data loggers inside the shipper/pack of particular sample and record the details in ‘Data Logger Register.

• For Stability sample data logger to be placed in one shipper for one NRGP number, NRGP be number to be mentioned in the ‘Data Logger Register’All the samples sent for testing outside the location shall accompanied with data logger.

5.5 If storage specified is less than ambient supervisor shall pack the samples with ice or gel bags or dry with data loggers.

5.6 Analyst/Designee QC shall organize for downloaded data logger data from public testing laboratory.

5.7 Send the labeled sample (s) along with analysis request form, STP and other documents (if required) to approved public testing laboratory.

5.8 Manual routing

5.8.1 Analyst shall label the samples.

5.8.2 Analyst/Designee QC shall send samples along with analysis request form, STP (uncontrolled document) and other documents (if required) to approved public testing laboratory.

5.8.3 QC Head/Designee QC shall enter the details in outside samples entry register and provide the reference number to the outsourced sample.

5.8.4 QC Head//Designee QC shall check and ensure the availability of following details, but not limited to (wherever applicable); 

• Specification / STP details,
• Batch No / A.R No,
• Raw data,
• Date of analysis,
• Standard and sample chromatograms,
• Standard and sample Spectra,
• Particle size histogram,
• Particulate matter printout,
• PXRD Diffractograms,
• DSC thermographs, etc.

For Complete SOP with Annexures - Click on Read more, Subscribe and Download         

1.0 PURPOSE

To lay down the procedure for Operation of Emergency Shower and eyewash unit

2.0 SCOPE: 

This SOP is to be applied at the time of Operation of Emergency Shower and Eyewash unit at the Quality control Laboratory.

5.0 PROCEDURE:

5.1 Fpor Eye Wash

 5.1.1 If some chemical/reagent goes into the eyes during analysis, immediately keep the face in the area for washing provided the equipment.

5.1.2 Press the lever at the sides of the shower for water flow

5.1.3 Rinse the eyes thoroughly with the help of running water

5.2 For body wash

5.2.1 If some chemical/reagent spread on the body or any part (other than face) during analysis,  immediately keep that body/body part below the shower for washing provided on the top in the  equipment

5.2.2     Pull the lever for water flow

5.2.3     Rinse the body / Body part thoroughly with the help of running water

5.2.4     After washing pull the lever to stop the flow.

5.3       Cleaning

5.3.1     Clean the surface of equipment thoroughly

5.3.2     Ensure that used water should be clean and does not contain any particle.

For Complete SOP with Annexures - Click on Read more, Subscribe and Download         

1.0 PURPOSE

To provide an Instruction for testing approval and disposition of In-process, Semi-finished and finished goods.

2.0 SCOPE: 

This SOP is applicable to all Quality control laboratories.

5.0 PROCEDURE:

5.1       Manual Routing :

5.1.1     Analyst/Designee QC shall receive the in-process sample for analysis along with intimation form / test request form, from production/ quality assurance.

5.1.2      Ensure received samples are packed in black polythene bag if the product sample vial or bottle received  is light sensitive.

5.1.3     Receive the semi-finished/ finished goods sample for analysis along with intimation form / test request, from quality assurance

•             : In case sensitive products received for analysis, check and ensure the samples are received in triple laminated polybag with specific instructions on test request form (TRF). Perform the physical parameters like Hardness and Moisture content within 24 hours from receipt of samples for analysis.

5.1.4     Ensure received samples are packed in black polythene bag if the product sample vial / ampoule / minibag etc. received is light sensitive.

5.1.5     Check the label against details furnished in intimation form / test request form / Batch packaging record. In case of any discrepancies get it corrected from concerned personnel.

5.1.6     In case received product samples are light sensitive and sample vial / bottle / ampoules / minibags etc. is not packed in carton/ black polythene bag, ensure the sample container are transferred to black polythene bag before storing in sample storage cabinet.

5.1.7     In case received product samples are light sensitive and sample vial / bottle / ampoules / minibags etc. is not packed in carton/ black polythene bag, ensure the sample container are transferred to black polythene bag before storing in sample storage cabinet.

5.1.8     Store the received samples in the (secured) designated staging area under the storage condition as per the respective specification.

5.1.9      Issue authorized Analytical worksheet for each sample as per working instruction (WI)

For Complete SOP with Annexures - Click on Read more, Subscribe and Download         

1.0 PURPOSE:

To provide a procedure for preparation, review, approval, distribution, revision and retrieval of stability protocol.

2.0 SCOPE: 

This SOP is applicable to the stability protocols for all products

5.0 PROCEDURE:

5.1  Designing of protocol

5.1.1    Stability protocol preparation, checking, approval and authorization for development, exhibit, site transfer and commercial batches shall be as per Annexure 3.

5.1.2    Stability study to be initiated after completion of tests within three working days from date of finished product sampling.

5.1.3    The stability storage condition shall be based on the product storage condition.

5.1.4    Test Parameters, time point shall be decided by QA.

5.1.5    Stability protocol for exhibit, commercial and site transfer batches shall be based on the shelf life specification (SLS) of the product. Any other additional tests as required shall be included.

5.1.6    Quality Assurance department shall ensure the regulatory compliance of the protocol for exhibit batches, validation batches, commercial batches, and any marketing requirement.

5.1.7    Minimum number of samples for stability studies is as described in each individual stability protocol after calculating the quantity required for stability analysis in consultation with QA Contingency samples shall be kept at least sufficient for one complete analysis for all stability storage conditions or as per requirement.                                                                                                                                    Note: The samples for commercial batches shall be in the same packing as the marketed pack.     

5.1.8    For all the samples, accountability shall be maintained through sample receipt and issuance register.  

            Note: For the post approval (NDA/ANDA) manufacturing batches stability protocol shall be same as regulatory submitted protocol during the regulatory submissions.

5.2       Designing of protocol for Contract Stability

5.2.1    Preparation, checking and approval of protocol for contract stability shall be handled as per the technical agreement with the contract giver.

5.2.2    If approved protocol is provided by the customer then the same shall be used for conducting the stability study.

5.2.3    Same protocol shall be received with stability samples and reviewed by QA for compliance with respect to the samples size, samples labels and samples integrity.

5.2.4    All the details shall be documented in the samples receipt register with protocol No. date of incubation of samples, Batch No., storage conditions, samples quantity received.

For Complete SOP with Annexures - Click on Read more, Subscribe and Download         

1.0 PURPOSE:

To provide a procedure for analytical method validation

2.0 SCOPE: 

This standard operating procedure is applicable to quality control.

5.0 PROCEDURE:

5.1  Enter the samples in the register and assign the activity concerned personal.

5.2  Allot number for method validation

5.3  Prepare method validation protocol and submit for review.

5.4  Refer guideline for carrying out method validation activity.

5.5 Review pre-qualification method validation requirements.

5.6 Review the validation protocol.

5.7 Submit the protocol for approval and authorization and organize method validation note book  from QA.

5.8 Initiate method validation activity as per authorized method validation protocol

5.9  Record the activity in validation notebook.

5.10 Attach weight printouts, write batch No/lot No /no of sample and standards and write chemicals details etc... In method validation note book. Include Batch no/ Lot no of sample in sequence and report.

5.11 File raw data (Method validation note book, chromatogram, graphs, etc) and label the file appropriately.

5.12 Prepare draft method validation report and submit.

5.13 Review the validation report and raw data and in case of any discrepancies organize for correction as per method validation report check list.

5.14 Organize repeat analysis in case of any parameter not meeting acceptance criteria upon justification.

5.15 Review the validation report and if found satisfactory organize for method validation report and approve the same.

5.16 Review the validation report and approve the same.

5.17 Handover the validation report and raw data for QA authorization and archival

5.18 Initiate method development upon investigation if validation fails to meet acceptance criteria.

5.19 In case of any editorial change in the protocol or repeat organize for erratum.

5.20 If there is repeat analysis during method validation, repeat the analysis during method validation from shall be issued and issuance shall be entered in the register.

For Complete SOP with Annexures - Click on Read more, Subscribe and Download     

1.0 PURPOSE

To provide a procedure for Document management–Worksheet /Template/Analytical records.

2.0 SCOPE: 

This procedure is applicable to the Quality Control laboratory.

5.0 PROCEDURE:

5.1 Supervisor shall receive all the incoming samples and enter into the respective analytical report numbering registers as per the respective site specific procedure.

5.2 Supervisor shall allot analytical reference number (AR No.) wherever applicable.

5.3 Issuance of worksheet Reference Process flow

5.3.1 QA shall issue worksheet pad to supervisor and record the serial number and the date issued in    Work pad issuance register.

5.3.2 Analyst/Designee QC shall issue work sheet to analyst by writing details (Code followed by  number as per Table-1) in work sheet.

5.3.3     Maintain counter foil of each worksheet pad under lock and key.

5.3.4 Organise for worksheet printing beginning of every calendar year or whenever worksheet gets exhausted.

5.3.5  Refer table-1 for codes and numbering of worksheets

5.4  Analytical Worksheet Template Management Reference Process flow

5.4.1     Analyst shall prepare the analytical worksheet templates by referring respective specifications / standard testing procedures.

5.4.2     Number each analytical worksheet template with a unique number as given below:

            AWS/XX/NNNN/Rn.

            Where, AWS: Analytical worksheet

            XX: Nature of sample i.e., refer table-1 for the codes              

            NNNN: Serial number of the analytical worksheet template starts from 0001.

              Rn: Revision status

            E.g.: First analytical worksheet template prepared for Finished product shall be numbered as:    AWS/FP/0001/R0

5.4.3     Approval details shall be recorded in the first page of analytical Worksheet template (along with material name, specification no., STP No., AWS Ref No.

5.4.4 Analyst shall record specification no., STP No., AWS No., Page No. & material name on  subsequent pages from second page onwards at the beginning of each page.

5.4.5  Analytical worksheet template shall contain the provision for recording all the data that is required to establish that the analysis has been performed as per the relevant STP/GTP as applicable.

5.4.6  In general, Analytical worksheet template shall contain the provision to record the following but  not limited to:

• Provision to write the instrument details like the instrument identification numbers, system condition/parameters as specified in the respective STP.
• Record of chemicals / standards / media / microbial culture/ reagents being used and their manufacturing lot numbers, grade used, use before details and any drying details of standards as required.
• For volumetric and test solution the internal tracking / lot number, strength as applicable, any dilution done and use before date.
• Record of any weighing(s) / dilution(s) performed.
• Record of time / duration / dates.
• Any system suitability requirement as mentioned in the respective test procedure.
• Record of any observation.
• Space for calculation.
• Bracketing standard calculation
• Pass / Fail status.
• Signature of analyst with date and reviewer signature with date.

5.4.7     Analyst/Designee QC shall verify the worksheet template for the contents against respective standard testing procedures.

5.4.8     Analytical Worksheet template shall be checked by QC Head or designee and approved by QA head or designee.

5.4.9     In case of any revision in testing procedure simultaneously analytical worksheet template shall also be revised through change management procedure.

5.4.10   *When a STP undergoes a change, even if that change doesn’t affect the worksheet template, the     worksheet template shall also be revised to reflect the current version of the STP number. In an   event of a modification/correction of error needed to be executed in the Analytical worksheet        template independent of any change in the STP, the worksheet template shall be revised to reflect      the newer version (Revision No.), while keeping the STP number and revision same.

5.4.11   Master copies of analytical work sheet template shall be printed on A4 size green color sheets and shall be under the control of QA. QA shall take photo copy from the master copy on A4 size yellow color sheets and issue the controlled document to QC.

5.4.12   Analytical work sheet templates are issued serially having the Issue No. which starts with the last  two digits of the year followed by 4 continuous serial numbers.  e.g.: for the year 2024 Issue No.  starts as 240001 where 24 indicates the last two of the year 2024 and the next digits 0001indicates the serial number.

5.4.13   Old version of template shall be stamped as OBSELETE, the obsolete copy shall be removed  from use. Master copies and obsolete copies shall be maintained by QA.

For Complete SOP with Annexures - Click on Read more, Subscribe and Download         

1.0 PURPOSE

To provide an Instruction for management of Reserve samples/Control samples

2.0 SCOPE: 

This SOP is applicable to Quality Control laboratory

5.0 PROCEDURE:

5.1 Finished products

5.1.1     For collection of Reserve samples and Periodic observation samples of Finished product, refer Site-specific SOP on sampling and AQL checks in packaging. Refer Annexure-4 for Entry / Issue of sample register.

5.2 Raw materials

5.2.1     Analyst shall collect Reserve samples for all the batches received (both active ingredients and inactive ingredients except liquids like water, acids, alkali flammable solvents and gases).

5.2.2     Analyst shall store the samples in air tight glass container (amber /plain) with roll on caps/ sealed vials / heat sealed poly bags /self-sealed poly bags and affix with a label, for traceability printed from HHD (refer procedure titled “Sampling of Non Sterile Raw Material and Excipient”. In case HHD is under maintenance, label the reserve samples as per Annexure -2.

5.2.3     Analyst shall refer respective specification for the storage condition.

5.2.4     For manual routing, analyst shall enter the details in the Reserve sample entry register as per procedure titled “Allotment of AR No.”.

5.3       Packaging materials

5.3.1     Analyst shall attach a sample of printed packaging materials such as cartons, labels, literatures etc., to the respective analytical reports.

5.3.2     Analyst shall store representative samples of printed primary packaging materials (Ceramic printed) such as PFS affix with a label, for traceability refer Annexure -2.

5.3.3     For manual routing, enter the details in the Reserve sample entry register.

5.3.4     Unprinted packaging materials and miscellaneous materials such gloves etc., are not kept as reserve samples.

5.4       Inspection of Periodic observation samples

5.4.1     Analyst shall inspect approximately 30 Tablets / Capsules and approximately 6 sachets and 1 bottle of oral solution and 5 tubes of ointment/creams once in a year up to expiry for appearance, obvious physical defects, packing integrity and record the details of this inspection in the Periodic observation sheet as per Annexure-5 (refer table -1).

Note: Periodic observation procedure mentioned below is applicable to other locations if oral dosage units are manufactured. Any suitable annexure mentioned can be used to record the observation (refer annexure-6 and annexure-8).

5.4.2  In case of clear PVC / PVDC foil blister packs, perform periodic observations by using the reserve samples only, without removing the dosage unit from the blister. Note: In case the entire control sample is used for a batch, then enter in the register and discontinue further periodic observation (refer Annexure-6).

5.4.3 In case of sachets, analyst shall open the units and spread the powder on a clean butter paper or a petri dish and examine the powder for any variation in the physical characteristics of the product. In case of liquids, ointment / creams transfer the content to petri dish or test tube and examine for any variation in the physical characteristics of the product.

5.4.4 In case of any abnormality observed during Periodic Observation analyst shall inform to Manager/designee for further action. If required send the product to QC for complete analysis.

5.4.5 Destroy the unit opened for annual inspection and reconcile the quantity destroyed in register

5.4.6 In case manufacturing date is not available on the sample pack, consider the date of receipt for the annual inspection.

5.4.7 For manual routing, allotment of A.R. Number to the Periodic observation to be done as: Allot the A. R. No. to all the product as “PO/XXXXXXX/YY”, where “PO” stands for periodic observation, “XXXXXXX” stands for B. No. of the product, and “YY’ stands for Year of observation.

For Complete SOP with Annexures - Click on Read more, Subscribe and Download         

1.0 PURPOSE

To provide an Instruction for handling of Laboratory Instrument / Equipment’s Electronic data  and review system.

2.0 SCOPE: 

This SOP is applicable is applicable for electronic data files generated by software connected to server based and standalone systems in Quality Control Laboratory.

5.0 PROCEDURE:

5.1       General Instructions:

5.1.1    Separate individual or Respective instrument login user ID as applicable and password to be allotted for all operating systems by the ENG through request form.

5.1.2    No software other than the intended to be used on these computers.

5.1.3    The date and time of the server is synchronized with the control timer clock in consultation with ENG

5.2       Laboratory instrument software access control management:

5.2.1    Classify the access levels under, Analyst, Reviewer, Manager & Administrator or in-line with features of the instrument / equipment software.

5.2.2    Create user ID in the instruments / equipment’s software as per procedure or in-line with features of the instrument / equipment software.

5.2.3    Wherever the instrument/equipment application does not support creation of individual window user ID’s, group ID’s shall be used. Ensure the following procedure where windows group ID’s and password exists:

The analyst / operator to operate the instrument / equipment with group user ID and password.

5.3       Password policy Management:

5.3.1    Password policy to be set or as per respective instrument software policy.

            Standalone software password policy: Follow the procedure wherever applicable else follow as per software features.

            Minimum Password Length:  7 Characters

            Maximum password Expiry: 30 days

            User lockout duration: 1 minute

            User lockout after 3 failed login attempts.

5.4       Naming of data file and file path for Server based systems:

5.4.1    Follow the Program, method and sequence naming as per SOP titled “Operation and calibration of HPLC (LabSolutions Software)”.

For Complete SOP with Annexures - Click on Read more, Subscribe and Download         

1.0 PURPOSE

To provide an instruction for operation and calibration of Conductivity Meter

2.0 SCOPE: 

This procedure is applicable to the operation and calibration of the Conductivity Meter in the Quality Control Department.

5.0 PROCEDURE:

5.1       Procedure for operation       

5.1.1    Switch on the Main supply and press ON/OFF button of the conductivity meter to switch on the meter.

5.1.2    Rinse the conductivity cell with purified water.

5.1.3    Dip the conductivity cell in the solution under test and stir gently

5.1.4    Note the reading display.

5.2       Calibration procedure

5.2.1    Rinse the conductivity cell with purified water.

5.2.2    Dip the conductivity cell in the standard solution of 1413µs/cm, Press the CAL key, then ENTER and wait for reading. Press the mode key to get the corresponding TDS value.

5.2.3    Record the Conductivity and TDS values of standard solution.

5.2.4    Report for any discrepancy observed in the Calibration report to Department head and Stop using the Conductivity Meter. Affix BREAK-DOWN tag to the conductivity meter and inform the utility department for rectification.

5.2.5    Daily Verification: Accuracy and after each Maintenance Job.

For Complete SOP with Annexures - Click on Read more, Subscribe and Download         

1.0 PURPOSE

To provide a written procedure for calibration and maintenance of Laboratory Instruments and Equipment.

2.0 SCOPE: 

This procedure covers the steps to be followed for Installation, Qualification, Calibration, and Maintenance of Laboratory Instruments and equipment.

5.0 PROCEDURE:

5.1   General instructions:

5.1.1 Analyst/Designee QC shall maintain dust-free environment with suitable temperature control wherever applicable at laboratory.

5.1.2 Analyst shall keep the Instruments / Equipment bench and surrounding areas clean and tidy at all times.

5.1.3 Analyst/Designee QC shall provide identification number to all Instruments and Equipment used in laboratory.

5.1.4 Analyst/Designee QC shall maintain Master Calibration Plan, for all the Instruments /Equipment available.

5.1.5  If prepared manually get the same approved by manager and display in the laboratory.

5.1.6 Analyst/Designee QC shall maintain usage Log Book for Instruments / Equipment (if site specific SOP not available,

5.1.7    For Instruments /Equipment which are not having audit trails and where date and time can be edited, supervisor shall supervise the analysis and approve the analysis in respective instrument log book once analysis is completed

5.1.8    Analyst/Designee QC shall prepare the list of Instruments /Equipment which are not having audit trails and date and time can be edited, display the list ensure the log book as is issued for the same.

5.1.9    When under use, analyst shall display the status by placing status board on Instruments / Equipment. Update the mobile phase / carrier gas / medium details as below:

            Mobile phase: Content of mobile phase and ratio used.

            Carrier gas: Name of carrier gas.

            Medium: Content of medium and ratio as applicable

5.1.10  Analyst/Designee QC shall maintain a list of Instruments / equipment under AMC

5.1.11  Analyst/Designee QC shall maintain a list of Spares at each location.

5.1.12  Analyst/Designee QC shall organise calibration after each AMC, and update Master Calibration Plan

5.1.13  Analyst/Designee QC shall update Instruments / Equipment History Card after breakdown maintenance, spares replacement, calibration, AMC

5.1.14  If any Instruments / equipment received from another location, Analyst/Designee QC shall get the copies of relevant documents such as Installation, Qualification and latest calibration data.

5.1.15  Analyst/Designee QC shall organize a copy of the operating procedure for reference from the location and prepare a new operating procedure.

5.1.16  Analyst/Designee QC shall allot the identification number as per location specific numbering procedure.

5.1.17  Head QC shall organize qualification/ calibration and update Master Calibration Plan; for calibration.

5.1.18  If any Instruments / Equipment received from another location or moved to another location within the laboratory, Analyst/Designee QC shall evaluate the qualification requirements as specified in Validation master plan.

5.2 Installation and qualification of laboratory Instruments and Equipment:

5.2.1    Analyst/Designee QC shall follow cGMP, safety, maintenance, industry guidance and statutory / regulatory requirements while Installation and Qualification.

5.2.2    Analyst/Designee QC shall affix under Installation Label for Instruments / Equipment under  installation

5.2.3    Analyst/Designee QC shall qualify the Instruments / Equipment as per installation and qualification protocols, which is either provided by manufacturer / service provider or prepared in-house.

5.2.4    Analyst/Designee QC and Head QC shall review completed Installation and Operational / Performance Qualification report for compliance.

5.2.5    Once qualified, supervisor shall include the Instruments / Equipment in Master calibration plan, Master plan for preventive maintenance and in AMC (as applicable). Affix the calibration status label

5.2.6    If any discrepancy is observed, Analyst/Designee QC shall inform Head QC for further necessary action.

5.2.7    Analyst shall enter individual usage log for each Instruments / Equipment

For Complete SOP with Annexures - Click on Read more, Subscribe and Download