SOP for Numbering system for analytical document to be used for regulatory submission

Objective:- To lay down a procedure for numbering system for analytical document to be used for regulatory submission.

Scope: This SOP is applicable for numbering system for analytical document to be used for regulatory submission in quality control laboratory.

Responsibility: Chemist or above of QC Laboratory.

Accountability: Head – Quality Control.

Procedure: Quality Control personnel shall prepare the analytical document for long term, intermediate and accelerated stability study data, summarized protocols for stability studies of exhibit batches and commercial batches, Exhibit Batches Constitution Study Protocol and Reports for Stability Study, and Exhibit Batch Constitution and Compatibility Study Protocol and Report.

Summary Sheet for Stability Study Data:

Stability Summary Sheet for Long term Stability Study data shall be prepared.

Stability Summary Sheet for Intermediate Stability Study data shall be prepared.

Stability Summary Sheet for Accelerated Study data shall be prepared.

Summarized Protocol for Stability Study of Exhibit Batches:

Summarized Protocol shall be prepared as per Annexure and document number shall consist of 17 alphanumeric characters e.g. PRT/ESS/XXXXXX-ZZ

First three characters ‘PRT’ denote protocol.

Second characters ‘/’ slash is separator.

Third three characters ‘ESS’ shall denote exhibit batches stability studies.

Fourth character ‘/’ slash is separator.

Fifth six characters ‘XXXXXX’ denote product code.

Six characters shall denote dash (-).

Seventh two characters ‘ZZ’ denote version number e.g. ‘00’ for new version.

Summarized Protocol for Stability Study of Commercial Batches:

Summarized protocol shall be prepared as per Annexure and document number shall consist of 17 alphanumeric characters e.g. PRT/CSS/XXXXXX-ZZ.

First three characters and second character defined above.

Third three characters ‘CSS’ shall denote commercial batches stability studies.

Fourth character, fifth six characters, sixth character and seventh two characters defined above..

Exhibit Batch Constitution and Compatibility Study Protocol:

Exhibit Batch Constitution and Compatibility Study Protocol shall prepare as per Annexure and document number for protocol shall consist 20 alphanumeric characters e.g. PRT/CCS/XXXXXX/YY–ZZ

First three characters ‘PRT’ denote protocol

Second character ‘/’ slash is separator

Third three characters ‘CCS’ denote constitution and compatibility study

Fourth character ‘/’ slash is separator.

Fifth six characters ‘XXXXXX’ denote product code

Sixth character ‘/’ slash is separator.

Seventh two characters ‘YY’ denote protocol number

Eighth character ‘–‘dash is separator.

Ninth two characters ‘ZZ’ denote version number.

Exhibit Batch Constitution Study Protocol of Stability Study:

Document number for Exhibit Batch Constitution Study Protocol of Stability Study shall consist of 20 alphanumeric characters e.g. PRT/CSS/XXXXXX/YY-ZZ

First & second, character defined above.

Third character ‘CSS’ denoted constitution study of stability

Fourth, fifth, six, seventh, eighth & ninth character defined above.

Report for Exhibit batch Constitution and Compatibility Study:

Exhibit batch Constitution and Compatibility Study report shall be prepared as per annexure.

First character ‘RPT’ denotes Report.

Second character is slash ‘/’ for separation.

Third character ‘CCS’ denotes constitution and compatibility study.

Fifth, six, seventh, eighth and ninth character defined above.

Analytical data shall be recorded in the supplementary.

Report for Exhibit batch Constitution Study for Stability Study:

Report for Exhibit batch Constitution Study for Stability Study shall be prepared as per annexure and document number shall consist of 20 alphanumeric characters e.g. RPT/CSS/XXXXXX/YY -ZZ

First three characters ‘RPT’ denote report.

Second two characters ‘CSS’ denote constitution study for stability sample

Third, Fourth, fifth six, seventh, eighth and ninth character same as above.

List of Annexure

• Summary Sheet for Long Term Stability Study  Data
• Summary Sheet for Intermediate Stability Study Data
• Summary Sheet for Accelerated Stability Study Data
• Summarized Protocol for Stability Studies of Exhibit Batches
• Summarized Protocol for Stability Studies of commercial Batches
• Exhibit Batch Constitution and Compatibility Study Protocol
• Exhibit Batch Constitution Study Protocol of Stability Study
• Report for Exhibit Batch Constitution and Compatibility Study
• Report for Exhibit Batch Constitution Study of Stability Study

SOP for Maintaining Quality Control equipment / instrument log book

Objective : To lay down the  procedure for maintaining equipment / instrument log book in Quality Control Department.

Scope: This procedure is applicable for maintaining equipment / instrument log book in Quality Control Department.

Responsibility: Chemist or above of QC department

Accountability: Head Quality Control

Procedure:

The equipment / instrument log book shall be maintained for equipments / instruments used in Quality Control department.

The equipment / instrument log book shall be controlled by Quality Assurance department and QA department shall issue the instrument log book to QC  department.

In instrument log book, analyst shall enter the start time just after analyst starts work  on respective instrument.

The end time shall be entered immediately at the end of analytical activity.

After completion of analytical activity analyst shall be responsible for maintaining cleaning of instrument as per SOP on cleaning of respective instrument and cleaning status shall be recorded in instrument usage log book.

Start time shall be the time, when analyst starts the usage of the instrument and end time shall be the time, when analyst leaves the instrument. (Leave means either completion of analytical activity or hand over the operation to the second analyst).

If samples are being loaded in long sequence (HPLC / GC) then analyst may enter the end time entry on next working day with initial and date after verification of run of the sequence.

If sequence has been interrupted due to malfunctioning of instrument or due to any other reason this instrument shall be handled as per SOP.

Recording of time shall be in 24 hour format and if end time shall be on next day then entry shall be made as ‘AA : BB (dd-mm-yyyy)’

Where ’AA’ is for hour, ‘BB’ is for minute and ‘dd-mm-yyyy’ is for date e.g. 24-11-2025 for 24^th November 2025.

If instrument is not working properly then record observation in Instrument Breakdown History Record and affix “OUT OF ORDER” label and follow SOP for further action.

HPLC / GC instrument log book  shall be as per Annexure and log book of remaining instruments except HPLC and GC shall be as per Annexure.

Note : All entries shall be done online & Not more than one entry is allowed in one row.

After each entry one line shall be left blank for better readability.

List of Annexure :

• Instrument Log Book (HPLC / GC)
• Instrument log book (General)
• Instrument Breakdown History Record

SOP on Entry and Exit into Sampling Booth Area

Objective: To lay down a procedure for entry and exit into sampling booth area.

Scope: This procedure is applicable for entry and exit into sampling booth area.

Responsibility: QC Chemist or above

Accountability: Head – Quality Control

Procedure:

Entry Procedure into Sampling Booth Area:

Enter into the personnel air lock area.

Take clean secondary gown.

Wear headgear and then wear secondary gown over the Primary gown.

Wear booties.

Sanitize the hands, using disinfectant provided in the change room.

Enter into the Sampling booth area.

Hand gloves shall be used during sampling operation.

Exit Procedure from Sampling Booth Area:

Before exit, enter into the change room from sampling booth area and discard the hand gloves in the waste bin.

Ensure sampling booth area has been cleaned as per SOP on Cleaning of Sampling Booth Area.

Remove and keep Headgear, booties and secondary gown in the used gown

Exit through the personnel air lock.

Status of the activity shall be mentioned on status board fixed on outside personnel air lock area.

List of Annexure – Activity Status Label

SOP on Intermediate and finished product Analysis, Approval and Rejection

Objective: To lay down the procedure for analysis, approval and rejection of Intermediate and finished product.

Scope: This procedure is applicable for analysis, approval and rejection of Intermediate sample, validation sample and finished product sample in QC Department.

Responsibility: Chemist or above /Executive / nominee

Accountability: Head – Quality Control

Procedure: Quality Assurance personnel shall collect Intermediate samples, validation samples and finished product samples and handover the sample along with sample intimation slip filled with all details to QC section in-charge or nominee. Finished product sample shall be given along with finished product intimation slip and intermediate product and validation sample with sample intimation slip.

QC section in-charge or nominee shall receive the sample and verified the all given details with that particular sample and after that record information of finish product in finish product control register , Intermediate product in intermediate product control register and validation sample in validation product control register.

A.R.No. of product shall be generated as per current version of SOP.

In case of allocated batch, QA shall provide batch packing allocation form , along with finished product intimation slip. From this allocation form, QC Executive / nominee shall ensure that first packed batch have to be analyzed and analytical results for subsequently packed batches shall be referred from that of first packed batch.

Incase of finished product sample (Tablets / Capsules) manufactured for Domestic, ROW markets, if difference between packing of first batch and subsequently packed batches is not more than 30 days then only results of first packed batch shall be taken for reference to subsequently packed batch, otherwise complete analysis of this subsequent batch shall be performed as per respective specification.

Incase of finished product sample (Dry powder Injection) manufactured for Domestic, ROW markets, results of filled vials (intermediate stages) shall be taken for reference for release of finished product.

Quality Control Executive / Nominee shall allocate the sample to chemist for analysis.

Quality Control Chemist shall perform the analysis as per specification and standard test procedure of respective product, and record the observation and calculation in respective work sheets.

After completion of analysis, QC chemist shall submit worksheet along with intimation slip to QC executive / Nominee for review.

QC executive / nominee shall review analytical data w.r.t. Specification & STP for adequacy and prepare Certificate of Analysis for Finished product.

If all the results of analysis found within specification product shall be passed than QC Executive or nominee shall prepared Certificate of Analysis for Finished product.

If results of any test found out of specification then SOP SOP on handling, investigation and reporting of out of specification results) shall be followed for necessary action.

Based on the conclusion of OOS investigation, product shall be rejected or passed.

After review, QC executive / nominee shall send the worksheet to QC Head or nominee.

Incase of intermediate & validation samples QC head or nominee shall give final approval.

Incase of finished product sample manufactured for Domestic, ROW and regulated markets QC Head or nominee shall approve worksheet and review the COA.

Finished product sample manufactured for Domestic, ROW and regulated markets Approval of COA shall be done by QA Head or nominee.

List of Annexure

• Finished Product Control Register
• Intermediate Product Control Register
• Validation Product Control Register

SOP on handling of alarm system of Stability Chambers

Objective: To lay down a procedure for handling of alarm system of stability chambers.

Scope: This SOP is applicable to handling of alarm system of stability chambers.

Responsibility:

Chemist or above of QC Laboratory.

Electrician or above of Engineering department.

Security supervisor or above.

Accountability:

Head – Quality Control

Head – Engineering

Head – P&A department

Head – Quality Assurance

Procedure:

Alarm System comprises of :

Buzzer on each Stab.ility Chamber.

Alarm panel fixed in Stability room.

Alarm buzzer fixed in Security Office.

Whenever there is overshoot / undershoot of temperature or overshoot of RH with respect to set point then;

Audio alarm will be generated on particular stability chamber having temperature or RH issue.

Indicator will glow and Audio alarm will be generated in Alarm panel with respect to respective stability chamber.

Audio alarm will be generated in security office.

As Audio alarm beeps, security person shall intimate to engineering person regarding audio alarm of stability chambers.

Unit-VI Engineering person will identify the respective stability chamber with the help of alarm panel and rectify the problem.

If Engineering person is not able to rectify the problem then he shall inform to QC head to call vendor’s service engineer and further activity shall be performed as per current version of SOP No. QC-SG-018 (SOP on handling of stability chambers).

SOP on handling of rinse and swab sample

Objective: To lay down the procedure for handling of rinse and swab sample.

Scope: This procedure is applicable for handling of rinse and swab sample in QC Department.

Responsibility: Chemist or above of QC department & Executive / nominee of QC department.

Accountability: Head – Quality Control department.

Procedure: In-process Quality Assurance personnel shall collect the sample of rinse or swab sample and handover the sample to QC department along with sample intimation slip filled with all details.

Quality Control chemist or above shall record information of rinse and swab sample in rinse and swab sample inward register.

A.R. No. of rinse and swab sample shall be generated as per SOP.

Quality Control Executive / Nominee shall allocate the sample to chemist for analysis.

Quality Control Chemist shall perform the analysis as per standard test procedure of respective product, and record the raw data in continuation sheet.

After completion of analysis, Executive / Nominee shall review the results and shall send to Head QC for final approval.

After approval from QC Head one signed copy of rinse and swab intimation slip shall be sent to IPQA section.

If results are found out of specification, then SOP on handling investigation and reporting of out of specification results shall be followed for necessary action.

List of Annexure – Rinse and swab Sample Inward Register

SOP on Retesting of Primary Packing material

Objective: To lay down the procedure for retesting of primary packing material for material lying in warehouse for longer period.

Scope: This SOP is applicable for retesting of primary packing material for material lying in warehouse for longer period.

Responsibility: Chemist or above of QC Department & Officer or above of Warehouse Department.

Accountability: Head – Quality Control.

Procedure: On receipt of material, warehouse shall send the GRN to QC as per SOP and QC shall perform sampling of packing material as per SOP and release the material as per SOP.

At the time of release of primary packaging material, QC person shall assign in-house retest date of material as per below mentioned table-1

Table-1.

Sr. No.	Name of Primary Packing Material	Retest Period
1	All type of Foils	2 years
2	Rubber Stopper	6 Months
3	HDPE Containers (Bottle)	2 years
4	White Closure with induction wad	2 years
5	LDPE Bag	2 years
6	Activated carbon 1 gram pouch	6 months
7	1 gram 2-in-1 desiccant  pillow pouch	6 Months
8	Triple Laminated bag	2 years
9	Glass Vials	2 years
10	1 gram Silica Gel Pouch (Roll Form)	6 Months

Retesting can also be carried out as per any directive from Quality assurance department on need basis or risk analysis.

In case, if expiry date assigned by vendor is coming before the in-house retest date, then re-test date shall not be applicable and material shall be considered expired as per label from vendor.

If retest or re-evaluation date assigned by vendor is coming before the in-house retest date, then retest date shall be in line with that of vendor. Thereafter the material shall be reassessed immediate before use to establish its suitability. The validity of this reassessment shall be as per given tablet -1 from the date of release. This shall be followed till the material continues to meet with the specification.

After receiving re-test request from ware-house, QC personnel shall enter the material details in re-test packing material control register.

QC personnel shall allot the A. R. No. by adding suffix ‘/ Rn’ where ‘/’ is for separation, R is for retesting and n is the number of times of re-testing after the initial analysis for the release of the material. For example, if request for re-testing of packing material is received first time and the initial A. R. No. is PM/25/0001 then A. R. No. of re-test material shall be PM/25/0001/R1 and packing Material sampling shall be done as per SOP.

‘TEST FOR RETESTING’ mentioned in the respective packing material specification, shall be performed during retesting of packing material.

Analysis and approval of re-test packing material shall be done as per SOP.

During COA preparation for retested packing material, the analytical data for the test performed during retesting shall be included and other test shall be taken from initial analysis and COA shall be prepared as per SOP.

Expired or rejected packing material shall be destroyed by ware-house as per SOP.

List of Annexure

• Retest packing material Control Register
• Test to be performed During Re-testing of primary packaging material

 

SOP on Backup / restore and archive of analytical data in electronic form

Objective: To describe the procedure for backup / restore and archive of analytical data in electronic form.

Scope: This SOP is applicable for backup / restore and archive of analytical data in electronic form in quality control laboratory.

Responsibility: QC Executive or Nominee & QA Officer and Above

Accountability: Head-QC & Head-QA

Procedure: QC Executive / Nominee shall prepare list of instruments along with software for which backup of analytical data shall be taken as per Annexure.

Backup of Fortnightly Data:

QC Executive / Nominee shall take backup of Fortnightly data from primary drive to pre – defined secondary drive and to external hard disc. Primary Drive and Secondary Drive (to which fortnightly data shall be stored) shall be mentioned in Annexure.

Assign Id. No. to external hard disc as QCHRD-XX, where XX is the sequential number i.e. 01, 02.

Back up path for external hard disc shall be; External hard disc → Year →Month → Individual instrument Id. No. → Analytical data.

QC Executive / Nominee shall create ‘year’ folder, named as ‘YYYY’, where YYYY is for year.

‘Month’ sub folder shall be created on monthly basis and named as ‘XXX’, where XXX denotes first three letters of the month.

‘Instrument Id. No.’ sub folder shall be named as actual instrument Id. No. of the instrument.

Primary drive to external hard disc data backup process shall be maintained.

External hard disc shall be kept under the custody of QC Head.

Primary drive to secondary drive data backup process shall be maintained.

Monthly Archival of Data:

Data from secondary drive shall be archived on DVD on monthly basis and activity shall be recorded.

Note: Month shall be considered from first day to last day of the calendar month.

DVD shall be labeled as per following pattern; e.g. SM/XXXXX-ZZ/MM/YY

Where; SM denotes Storage media , XXXXX – Instrument Id., ZZ -Number……01, 02…… ,MM – Month ,YY- Year….07, 08, 09…

Monthly archival shall be completed within 15 days of next month.

The Data Storage media carrying the archived data shall be handed over to QA department.

QC Executive / Nominee shall ensure that primary drive and secondary drive of each system shall not contain data older than two months prior to current month at the time of monthly archival.

The Data Storage media shall be labeled for identification with following details:

Instrument Name & Id. No., Computer Id. No., Archived Data Period.

Verification of Archived data:

QC Executive / nominee shall verify the integrity of the archived data from primary drive to secondary drive or in DVD and in hard disk w.r.t the data lying in primary drive and record shall be kept.

QC Executive / nominee shall restore archived analytical data from DVD & hard disk and select randomly any set of analysis, open and compare it with the original hard copy of the same to check the data integrity and record shall be kept as per the respective format for verification of data integrity.

Incase where the analytical data is directly accessible from DVD / hard disk, through application software, there is no need to restore data in primary drive. Verification shall be done on DVD or hard disk directly.

QC Executive / nominee shall check the data integrity of the archived data of the January and June month of every year, after every 6 months for 5 years and record shall be kept as per the respective format for verification of data integrity.

A Person shall maintain logbook for received data media.

Data Retrieval and Restoration Procedure:

If it becomes necessary to restore the previous data, prior approval of Head – QA shall be taken.

Only QC Executive / Nominee shall be allowed to restore the data.

Log for restoration of data shall be maintained.

Data storage media shall be returned to the QA department.

Backup/ Restore Failure:

If any error or failure is reported in backup or restoration procedure, QC Executive / Nominee shall contact local InfoTech for problem solving.

Vendor support may be sought in cases where problem of backup / restoration failure could not be solved. Further usage of system shall be temporarily stopped till problem is resolved.

All backup and restore failures shall be recorded in remarks column of respective records.

Preservation of Records: All monthly archived data along with records shall be preserved for a period of 5Years.

Precautions for Record Keeping:

All storage media shall be kept in a proper cover to avoid scratches.

Storage media shall be kept within a flame proof cabinet.

Storage media shall be kept within controlled environmental conditions.

Storage media shall be kept in vertical position.

List of Annexures : 

• List of Instruments for which Back up to be taken
• Record Log for Data Backup Process (Fortnightly) (For Primary drive to secondary drive)
• Label of Data Storage Media
• Verification record for archived data from one drive to another drives
• Record for Received Data Storage Media
• Data Retrieval and Restoration request
• Records of Retrievals of Backup Data
• Record Log for Data Backup Process (Fortnightly) (For primary drive to external hard disc)
• Verification of data Integrity for HPLC / GC
• Verification of data Integrity for UV-visible Spectrophotometer
• Verification of data Integrity for Polarimeter
• Verification of data Integrity for FTIR
• Verification of data Integrity for TOC analyzer

SOP on retesting of raw material

Objective: To lay down the procedure for retesting of raw material for material lying in warehouse for longer period.

Scope: This SOP is applicable for retesting of raw material for material lying in warehouse for longer period.

Responsibility: Chemist or above of QC Department.

Accountability: Head – Quality Control.

Procedure: Material shall be transferred to Quarantine area by warehouse personnel as soon as retesting period is due.

Approved label shall be defaced and new Quarantine label shall be affixed alongside defaced approved label on each container of the material by warehouse personnel.

Intimation for re-sampling shall be sent to Quality control department by warehouse for the material to be retested.

QC personnel shall enter the material details in Retest raw material control register and sampling shall be done as per SOP.

A.R. No. shall be allotted by adding suffix ‘/ Rn’ where ‘/’ is for separation, R is for retesting and n is the no. of times of retesting. For example, if intimation for retesting of raw material is received first time and its previous A. R. No. is RM/25/0051 then A. R. No. of material to be retested shall be RM/25/0051/R1.

Retesting period of active and inactive raw materials having microbiological analysis shall be six months. Inactive raw material, not having microbiological analysis shall have retest period of one year.

Retesting can also be carried as per any directive from Quality Assurance Department.

If Expiry date of material is coming before the in-house retest date then retest date shall not be applicable and material shall be considered expired as per expiry date given by vendor.

Raw material shall be retested five times, after that material shall be sent to FR & D for further investigation and decision shall be taken, based on the investigation done by FR & D.

Analysis and approval of retest raw material shall be done as per SOP.

Expired or rejected raw material shall be destroyed by Ware house as per SOP.

Retesting parameters of raw material has been mentioned in respective raw material specification.

Annexure – Retest raw material Control

SOP On Entry, exit and gowning procedure in Quality Control Department

Objective: To lay down a procedure for entry, exit and gowning procedure in quality control department.

Scope: This SOP is applicable to entry, exit and gowning procedure in quality control department.

Responsibility: Every person entering in QC department.

Accountability: Head – Quality Control & Head – Quality Assurance

Procedure:

Entry procedure for company employees and visitors:

Company employees shall take company apron and cap from almirah, wear apron, cap and enter into the department.

Visitors shall take disposable apron and cap from almirah dedicated for visitors, wear the disposable apron and cap and enter into the department.

Entry procedure for laboratory helpers and housekeeping persons:

Laboratory helpers shall take their white colour dedicated uniform from almirah, wear it and enter into the department.

Housekeeping persons shall take their orange colour uniform from almirah, wear it and enter into the department.

Exit procedure for company employees and visitors:

Company employees shall remove apron and cap in change room, hang the on hangers, and leave the change room.

Visitors shall remove the disposable apron and cap in change room and put in bin dedicated for used apron and cap and leave the change room.

Exit procedure for laboratory helpers and housekeeping persons:

Laboratory helpers and housekeeping persons shall remove their uniform in change room and keep in almirah then leave change room.

List of Annexure / Formats: Not applicable.

References (if any): Sop on SOP .