Standard Operating Procedure for Receipt, Qualification and Handling of Analytical Standards.
To lay down a procedure for Receipt, Qualification and Handling of Analytical Standards.
The scope of this SOP is to Procure, Qualify, Store, Handle and Disposal of Reference Standards, Secondary Reference Standard OR Working Standard, Gas Chromatography Standards used in the Quality Control Laboratory for analysis at [Company Name].
QC-Personnel: Receipt, qualify, handle and destruction after use of analytical standards
Laboratory Supervisor: Review of Qualification report
Section Head-QC: Review the qualification report.
Head-QC/ Designee: Ensure the Compliance of the SOP.
Pharmacopoieal Reference standard: These are authentic Substance of high purity with Critical characteristics and Suitable for their intended purpose supplied by the official Pharmacopoieal sources.
In-House Reference standard: These are authentic substance, Characterized and verified In-House and suitable for their intended purpose.
Working standard/ Secondary reference standard: Secondary Reference Standards OR Working Standard are the standards that are Qualified against the current lot of the Reference Standard. Secondary Reference Standards are also called as Working Standard.
• Accessed to Analytical standards shall be done authorized personnel as per the List of authorized personnel displayed at the Analytical standards storage room/ cabinet.
• The list shall be updated on need based which shall be authorized by Head Quality Control Laboratory (Head QC).
• During handling of analytical standards, wear Personal Protective Equipment (PPE) such as hand gloves, safety goggles, and nose mask as applicable.
• After completing the weighing activity, remaining quantity of working standard shall not be transfer into the original container.
• For the liquid standards, transfer the material into the clean and dry glassware. After weighing do not transfer the remaining quantity into the original container.
• For every new analysis use the fresh working standard vial. Once the vial is opened, it shall be discarded after the analysis is completed and report is reviewed if there is no out of specification or laboratory event observed.
• At the time of usage, analyst shall ensure the correctness of the standard vial against the specification like name of the standard, lot number and validity period.
• In case any abnormality observes such as, wrong standard issued, Lot no., working standard is not within the validity period, do not use the vial and inform to laboratory support team person.
• Before using and weighing of the reference standard or working standard, place the standard vial in the Desiccator OR Tray provided to attain the room temperature or as per the requirement.
• When working standard is quantity is consumed before its validity period, new working standard can be prepared using the current lot of reference standard.
• If the potency of Analytical Standard is grater than 100%, it shall be considered as 100% for the calculation.
• Temperature record for the working standard storage cabinet shall be verified on daily basis. For weekly off/ holiday, temperature record shall be verified on subsequent working day.
• During use, after opening the analytical standards, it needs to be closed tightly with the Parafilm or Aluminum Crimp Cap shall be kept in the upright position in respective cabinet by authorized person.
• If analytical standard is required to be dried before use, take a cleaned and dried weighing bottle for drying. Do not use original container as drying vessel for drying.
• Reference standard which is required for Retention Time (RT) / Relative Retention Time (RRT) or resolution and which are not used for any quantitative estimation, the usage quantity of such reference standard can be reduced where, the final concentration shall be kept as per the test procedure with prior approval from department head.
• In case, where statement mentioned on the reference standard “Reconstitute and quantitatively transfer the entire contents of the vial without weighing” and for protein and peptide or wherever applicable, lower weight of reference standard may be used for working standard qualification. Final concentration of the solution will remain similar.
• Lab support team person shall verify all the analytical standards on monthly basis as per respective format.
• Procurement, Receipt and Storage of Analytical Standards:
– Procure the reference standards from source such as USP, BP, EP, IP, or from official distributor.
– Reference standards or impurity standards (Other than Pharmacopoeial) shall be procured from API manufacturers.
– Procurement of reference standard shall be initiated at least two months prior to its requirement.
– Lab support person shall initiate the procurement requisition with the details of Reference Standard such as name of the material, quantity required etc.
– During receipt of Reference Standard, Lab support person shall verify following details:
i. Name of the material
ii. Current Lot Number
iii. Use before, valid up to, expiry date or re-test date as applicable.
iv. Documents received along with the Reference Standard such as Invoice, MSDS, COA, etc.
v. Storage condition of the reference standard
vi. Data logger received along with the received standard
– If any abnormality observed at the time of receipt, it shall be informed to supplier.
– The validity of reference standard shall be checked for current lot by referring current catalog, confirmation from authorized source using respective web site.
– If all the above details are found satisfactory, then the Reference Standard or Impurity shall be received and updated in the standard inward log.
– The received standard shall be stored in chamber according to its storage condition.
– In case Reference Standard, Impurity Standard or Working Standard is procured from other than API manufacturer, complete analysis report with the characterization data as applicable.
– If analytical standards are received with similar name from different suppliers, nomenclature (IUPAC name/ other synonyms) and Pharmacopoeial names shall be verified for difference if any.
– Lab support team person shall verify all the Reference Standard stored in Quality Control laboratory trend on monthly basis against current official catalog of USP, EP, BP or IP as applicable.
– If any lot found expired, same shall be removed from respective storage chamber and properly segregated. Destruction record shall be maintained.
– Current lot of reference standard shall be used up to its validity period.
– In case, the Reference Standard found expired or Material is not available for analysis, quality control laboratory can request to other manufacturing or testing location of organization.
– On receipt of Analytical Standards, if the required documents such as COA or any relevant data is not provided, standard needs to be segregated and shall not be used until the required documents received.
– At the time of receipt of standard, lab support team person shall verify the temperature for any possible excursion. If Data is found satisfactory, material shall be inword.
– If the temperature is not within the limit, Stability data and relevant supporting information shall be requested and verified for evaluation. Based on evaluation of data working standard shall be accepted/ rejected.
– After receiving of standard, QC shall request respective site to send complete transit data of Data Logger.
– QC shall verify the transit data. If found satisfactory, then only be issued for routine use and details of transit data shall be kept for record.
– Working Standard 5 shall be internally qualified against the current lot of Reference Standard.
– In case any Working Standard is received from company’s other location or material manufacturer, shall be kept as per storage condition as per the instruction available on container or on the certificate of analysis.
– During receipt of Working Standard, lab support team person shall verify following details such as Name of the material, Lot Number, Use before or valid up to or Expiry date or Re-test, CoA of Reference Standard to ensure that the Working Standard is valid for use.
– Documents received along with the standard such as Invoice, Delivery Note, MSDS, COA, Storage condition shall be maintained.
– Validity of Working Standard must be less than or equal to the material using which the working standard is prepared.
– QC personnel verify the material received along with the label and supporting documents received.
– The received standard shall be stored in storage cabinet according to its storage condition.
– Gas Chromatography standards shall be procured from approved source same procurement procedure shall be followed as described in the above section.
– On receipt the standard, the QC person shall verify the certificate of analysis and the same shall be recorded. Record verification shall be done similar to the reference standard.
– The purity is assigned on the basis of the certificate of analysis received from the supplier or manufacturer. Such received material are not further qualified and neither subsequent standard are prepared against these materials.
– List of GC standard list be verified and updated on monthly basis or as and when required.
– The use before date for GC standard chemicals shall be based manufacturer’s recommendation maximum 6 months from the date of opening.
• Qualification of Secondary Reference Standard or Working Standard:
– Material selected for qualification of working standard should be of recent or current lot of approved raw material with highest purity/ potency.
– Available lot having maximum purity lot material shall be used for qualification of working standard.
– To get the approved raw material from warehouse department, QC personnel shall initiate the material requisition note and it should be approved by QA.
– On approval of sample request, QC person shall sample the required quantity of material to prepare the working standard.
– Use current lot of reference standard shall be used for qualification of working standard.
– Secondary Reference Standards or Working Standards are the standards that are Qualified against the current lot of the Reference Standard.
– If the Working Standard is to be qualified using under test material, required sample quantity can be taken from already sampled material.
– If Working Standard is qualified using under test material, it shall be made effective only after approval of under test material.
– The working standard qualification shall be done as per respective raw material specifications. For the qualification, following test shall be done:
iv. Water Content
– If Working Standard received from other locations of the organization, the Working Standard shall be received along with COA. Based on the COA, Working Standard shall be used for routine analysis.
– To qualify the secondary reference standard or working standard, the Assay, LOD, and Water content shall be carried out in triplicate and all other remaining tests shall be carried in a single set by single analyst.
– For calculation of Assay test on dried basis/ anhydrous basis, mean of the three set of LOD / Water content shall be taken respectively.
– The Relative Standard Deviation (% RSD) for Assay in triplicate set must not be more than 1.0 % and the average of Assay is considered as the assay of Working Standard.
– If the % RSD between the assay results found more than 1.0 % then, qualification of WS shall be repeated by another analyst in triplicate.
– If the % RSD between the Assay results of second analyst is within 1.0 % then, second analyst result shall be considered as valid and investigate for initial failure.
– After completion of WS qualification, report shall be verified by reviewer and approved by QA / QA.
– After approval from of working standard, QC Person shall take the make Certificate of Analysis (COA).
– For qualification of In-House Working standard and for those where reference standards are not available from Pharmacopoeia Commission, it shall be sent to Research and Development laboratory for the characterization study.
– After completion of qualification, Working Standard shall be stored in respective chamber as per the applicable storage conditions.
• Procedure for Filling Working Standard Vial:
– All Working standard material shall filled in the amber color glass vials with rubber caps and sealed with aluminum cap as per the requirement.
– Working standard vials filling activity shall be done in Laminar Air flow.
– Qualified working standard shall be filled in each and individual vials as per the requirement up to its vial capacity (1 vial should be sufficient enough for single analysis).
– The Working standard vials are labeled with the information such as Working Standard Name, Number, Potency, Vial No., Water content or LOD results.
– Place the filled vials of working standards in the storage cabinets as per defined storage conditions.
• Assigning of Shelf life to Analytical Standards:
– The validity of Working Standard shall be given one year or shelf life of the material whichever is less.
– Working Standard received from other location or Impurity Standards shall be used till its expiry date.
– Validity of Gas Chromatography standard shall be as per the expiry specified on the supplier’s COA or container. In case of validity is not provided, considered it as1 year from the date of opening and based on chemical nature or maximum 6 months from the date of opening.
– To assess the stability of working standard, assay and LOD or water content to be performed in single set analysis to ensure that there was no significant change during the storage. The retest results shall meet the acceptance criteria of the relevant specification and that should not differ by more than 1% in assay from its initial value obtained during WS qualification.
– If the significant change is observed more than 1%, then further investigation shall be carried out.
– The assessment of Stability of Working Standard shall be checked after six months and expiry on the basis of Protocol. If no significant change is observed in defined period, there shall be no further assessment to be carried out as the Standard is in stable condition.
– When the Validity for Analytical Standards provided by the supplier i.e. Retest, Expiry, Valid up to, as month and year. In that case, the validity shall be considered as last date of month.
• If any abnormality is observed before the expiry of the standard, i.e. in the appearance (color change of the liquid standard), then it is discarded.
• Issuance of Analytical Standards:
– Lab support team person shall issue the standard vial in sequential order.
– Record of issuance shall be maintained.
– Working standards received from other sources shall also be recorded in inward register and issuance record shall be maintained.
• Handling of Analytical Standard:
– Take required quantity from the vial.
– Do not return dispensed quantity of material into the vial.
– The reference standards shall be collected in container kept for designated purpose in chemical lab from its original pack.
• Assigning of numbering for Analytical standards. [Numbering to be decided by organization]
• Disposal of Analytical standards:
• Destroy the expired reference standards as per the respective procedure of Hazardous waste.
Reference standards verification on Monthly
Assessment of Stability of Working Standard on Half Yearly
7. Format for recording:
• List of authorized person to access standards
• Reference Standard /Working Standard/ Impurity Standard Inward Register
• Material Requisition Format
• Certificate of Analysis for Working Standard
• Standard Label
• Standard Consumption Record Logbook
• List of Standards
Guideline references: https://www.who.int/docs/default-source/medicines/norms-and-standards/guidelines/quality-control/trs943-annex3-establishmentmaintenance-distribution-chemica-reference-substances.pdf?sfvrsn=71064286_0