SOP for Preparation of Working Standard

1. OBJECTIVE:

To lay down a procedure for procurement of working standard.

• SCOPE:

This procedure is applicable for procedure for procurement of working standard.

• RESPONSIBILITY:

QC Officer/ QC Executive

• ACCOUNTABILITY:

QC Manager.

• PROCEDURE:
  • Requirements:
    • Reference Standards are classified as:
    • Pharmacopoeial Reference Standard: These are for the products mentioned in the Pharmacopoeia i.e. USP, BP, EP and Indian Pharmacopoeia.
    • Non Pharmacopoeial Reference Standard: These are for the products, which are not mentioned in the Pharmacopoeia.
  • Procurement and storage of Reference standard:
    • Pharmacopoeial Reference Standards shall be procured from the authentic sources.
    • Non Pharmacopoeial Reference standards are procured from the manufacturer of specific substance or shall be provided by authentic sources with COA.
    • Reference standard shall be procured whenever:-
    • New lot number of pharmacopoeial reference standard is released by regulatory agencies.
    • Whenever non pharmacopoeial reference standard expired.
    • When new product is introduced in the facility.
    • Existing stock of reference standard is spoiled or consumed.
    • The current catalog for current Batch no / Lot no shall be verified for procurement of reference standard.
    • Purchase requisition shall be raised by Q.C. officer for the desired “Reference Standard” to be procured and shall be authorized by Head of Q.C.
    • Reference standard (Non Pharmacopoeial) shall be received from manufacturer along with copy of certificate of analysis and supporting data like MSDS and certificate.
    • On receipt of reference standard a copy of GRN and delivery challan or voucher copy shall be filed for ready reference.
    • On receipt check the integrity of seal and label details.
    • In case of failure to comply with Integrity of vial or Appearance of material, inform to purchase department for necessary action.
    • Record the detail in the reference standard logbook.
  • Usages and Destruction of Reference Standards:
    • Record the date of opening for the testing or for the Qualification of working standard in reference standard logbook.
    • During usage of reference standard, precautions should be taken such that contents of the vial are not contaminated with other products.
    • Seal the reference standard vial after usage & keep in the designated place.
    • Usage duration validity of impurity standard shall be determined against approved Impurity standard.
    • If the reference standard is expired (for non-pharmacopoeial) and /or replaced (for pharmacopoeial) by a new lot of reference standard dispose off the previous lot by dissolving in a suitable solvent and discarding the solution.
  • Preparation & Qualification of Working Standards:
    • Non-Pharmacopoeial reference standard received in sufficient quantity shall be directly used for routine analysis.
    • Raw material for working standard preparation shall be selected on following basis:
    • Recently manufactured and approved batch, tested as per respective pharmacopoeia/In House specification available in stores.
    • Batch of high purity shall be selected for working standard.
    • For preparation of WS basically two methods are used according to pharmacopoeial or in house method.
    • Absolute: – Method in which directs analysis is performed. For this no reference Standard is require like E1%. etc. potentiometricaly /Titration method.
    • Relative: – In this method reference standard is required to prepare working standard like HPLC, UV- Vis- spectrophotometer.
    • In case Reference standards are not available with the location, it shall be procured from authentic sources.
    • In case, the reference standard is not available with the above mentioned, than the working standard shall be prepared by analyzing the sample from FDA approved external agency.
    • Perform the following test:
      • Description
      • Identification (IR and/or HPLC or as specified in the respective specification if IR or HPLC not mentioned in the respective specification as Id. test).
      • Water Content / Loss on drying
      • Related Substances (if Required)
      • Assay
    • Any other test specific to the substances
    • Above tests should be carried out as per the standard testing procedure mentioned in respective material specification.
    • Assay shall be performed in triplicate.
    • In the test of Assay prepare one reference standard solution and Three working standard solution as per the respective standard testing procedure.
    • System suitability shall be performed, as per respective pharmacopoeia / specification and each WS preparation shall be injected in duplicate.
    • The area variation between two injections of individual sample preparation should not be more than 0.5 % of its mean value.
    • Calculate the average of 3 assay values obtained on as is basis. The RSD of these 3 assay values should not be more than 1.0 %.
    • Record the total analytical data in the worksheet.
    • Prepare analytical report for the test performed for the Qualification of WS.
    • Validity period of the working standard shall be one year from the date of preparation of working standard .In case the shelf life of batch selected for working standard preparation is less than 1 year then the validity period of working standard shall be expiry date of the batch.
    • Preserve the working standard in clean & dry amber colored vial under controlled Room temperature.
    • Prepare thirteen vials of each material and use single vial for each month. After completion of 1 month interval discard any material remaining in the vial and continue with next vial. On opening of vial, analyst shall mention the date of opening on the vial.
    • Each vial should be properly sealed and labeled.
    • Keep all the vials of working standard in desiccators and as per storage conditions mentioned on the labels.
  • Storage of working standard:
    • Working standards shall be stored in amber colored vials with rubber stopper and Sealed with aluminum cap.
    • These vials shall be properly segregated, labeledand stored.
    • Vials shall be stored as per the storage condition of the material.
    • Vial in use shall be stored in desiccators.
    • Silica used in desiccators shall be dried weekly and/or whenever the colour of silica changes.
  • Usage & Destruction of working standards:
    • The Executive QC shall issue one bottle, to the analyst for its use for not more than 31 days.
    • Issuance of Working Standard bottle shall be recorded in working standard logbook.
    • One bottle shall be used for one month only; the consumption shall be recorded.
    • Only two vial prepared for Costly materials, one vial use for half yearly.
    • In case, if consumption is more, or any incident like braking of takes place, another bottle shall be issued on approval from manager QC.
    • Working standard consumption record shall be maintained.
    • On completion of one month, the remaining quantity of Working Standard shall be destroyed by dissolving in a suitable solvent & discarding the solution.
    • Record the destruction in the working standard logbook.
    • Prepared the list of working Standard.
• TRAINING:

Trainer   : Manager – Quality Control

Trainees : Staff of the QC departments

• DISTRIBUTION:

Master Copy                  :           QA Department

Controlled Copy            :           QC Department

Display Copy                 :           QC Department

• REFERENCES:

In-House

• ABBREVIATIONS:

Abbreviations	Extended Form
SOP	Standard Operating Procedure
NA	Not Applicable
QC	Quality Control
Sr. No.	Serial Number
QA	Quality Assurance
DEPT.	Department

1. REVISION HISTORY OF CHANGE:

Sr. No.	Date	Revision Details	Revision No.
01	18/01/2020	NEW SOP	00