SOP for Preparation and Handling of Working Standards in Pharmaceutical industry | Working Standard in Pharma |
- Working standard SOP covers below points:
- What is Primary reference standards
- What is Secondary reference standards
- What is Working standards
- Preparation of working standard
- Analysis of working standard
- Filling of working standard vials
- Usage and validity of working standard
- Handling of working standard
- Storage of working standard
- Disposal of working standard
1.0 OBJECTIVE :
- To provide a procedure for Preparation, Labeling and Handling of Working Standards.
2.0 SCOPE :
- This SOP is applicable for preparation, labeling and handling of working standards in Quality Control Department.
3.0 RESPONSIBILITY :
- Quality Control Officer and above
4.0 ACCOUNTABILITY:
- Quality Control Head
5.0 PROCEDURE :
5.1 PRIMARY REFERENCE STANDARD:
- These are material of highest purity available.
- These may be used to validate the purity of working standards.
- These standards are shown to have suitable properties for intended use, the demonstration of suitability being made without comparison to an existing standard.
- Sources :
- BPCRS (British Pharmacopoeia Chemical Reference Substances)
- EPCRS (European Pharmacopoeia Chemical Reference Substances)
- USPRS (United States Pharmacopeia Reference Substances)
- NCL (National Chemical Laboratory)
- IPCRS (Indian Pharmacopoeia Chemical Reference Substances)
- IFPRESS (Indian Foundation For Pharmaceutical Reference Standard Substances)
5.2 SECONDARY REFERENCE STANDARD :
- These are used only when traceable reference material are not available (e.g. impurities, melting points standards, UV calibration standards).
- These are materials which are verified through independent test method with certificate from manufacturer (Suppelco, Fluka, Sigma Aldrich, Merck).
5.3 WORKING STANDARD :
- This is standard which is prepared in the quality control department for daily use.
- Working standard is a material of typical quality and is prepared by calibrating a passed material against a primary reference standard.
- Procure WS from manufacturer particularly in case of new active Pharmaceutical ingredients.
5.4 PREPARTION OF WORKING STANDARD :
- Select the latest approved batch of raw material for working standard having Assay value more than 99.0% (Calculated on anhydrous basis or on dried basis).
- Select the batch which is not having any deviation report or out of specification (OOS) during sampling and testing.
- Give requisition to ware house department for raw material required.
- Collect quantity of material for the preparation of working standard as per consumption of material.
- Give the reference number to working standard as follows,
- Working Standard Number : WS/01
- Where, 01 corresponds to serial number starting from 01 continuously to have details of total Working standards.
- The new Working Standards shall be prepared before the expiry of the existing working standard.
5.5 ANALYSIS OF WORKING STANDARD :
- Carry out tests for preparation of working standard such as,
- Description
- Identification (Preferably IR/Melting Point/Light absorption/TLC)
- Loss on drying or Moisture content
- Assay, according to Pharmacopeial requirement.
- Carry out assay determination against Reference standard.
- Compare the analysis result with Reference standard.
- Carry out assay of the selected raw material considering supplier’s working Standard or previous Working Standard or raw material passes from approved PTL as a standard, if Reference standard is not available.
- Compare the analysis with Supplier’s Working standard or previous Working Standard before validity or assay of raw material passed from approved PTL.
- Perform the assay in duplicate by two different chemists and RSD for four values of assay should not be more than 1.0 %.
- Compare the IR spectra of the prepared working standard against Pharmacopoeial IR reference spectra.
- Check the LOD or moisture content of working standard.
- Enter the details in analytical worksheet of working standard (Annexure No.: 04).
- Attached the print copy of analysis data and photocopy of Raw material COA which is used for preparation of working standard and vendor’s COA with analytical worksheet.
- Review the report by approved analyst after completion of reporting.
- Prepare certificate of analysis (Annexure No.: 02).
5.6 FILLING OF WORKING STANDARD VIALS :
- Use hand gloves, masks while filling the material in to the vials.
- Weigh and fill the material in to the vials.
- Distribute the working standard in 15 light resistant (Amber coloured) glass vials of 15 ml capacity and preserve 3 vials as stock Working standard (Approx. 2 gm for each vial), if material are required in minor quantity for analysis then distribute it in less quantity and vice versa.
- Stick the label on each working standard vial with all the details (Annexure No.: 01).
5.7 USAGE AND VALIDITY OF WORKING STANDARD :
- Use vial till the end of every month after opening, if some quantity remain in this vial then destroy it on end of same month.
- Replace the Previous Working standard vial with fresh vial on first day of every month.
- Cover the rubber bung with parafilm tape after removal of aluminum seal.
- Keep one vial of each Working standard in the allocated area for daily use in a Desiccator, containing silica gel.
- After use of vial, seal the vial with parafilm tape and keep it into the desiccator of working standard.
- Assigned One year shelf life for working standard from date of analysis.
- Maintain details of preparation and consumption of working standard in Working Standard Consumption Record Register (Annexure No.: 03).
5.8 HANDLING OF WORKING STANDARD :
- Always allow equilibrating to room temperature before weighing for a test.
- Avoid exposure of material with atmosphere.
- Do not insert spatula or butter paper in the vial to avoid the contamination.
- Discard the excessive material taken out from vial.
5.9 STORAGE OF WORKING STANDARD :
- Store all additional vial of Working standard as per the storage requirement of the individual standards, properly closed with rubber bungs and sealed with aluminum seal.
- Store the Working standards as per their respective storage condition, specified on the label of Working standard vials.
- Avoid contamination by carefully handling to ensure its integrity.
5.10 DISPOSAL :
- Wet the content by emptying in a waste beaker containing water and dispose off.
- Deface the label of the working standard vials.
- Discard the vial in dustbin for broken glasswares.
- Record the destruction of working standard as a remark in working standard consumption record register.
6.0 ABBREVIATIONS:
| Abbreviation | Expanded form |
| WS | Working Standard |
| WS No. | Working Standard Number |
| gm | Gram |
| Mfg. Date | Manufacturing Date |
| Exp. Date | Expiry Date |
| LOD | Loss On Drying |
| 0C | Degree Celsius |
| PTL | Public Testing Laboratories |
| IR | Infra Red |
| TLC | Thin Layer Chromatography |
| Approx. | Approximately |
| COA | Certificate of analysis |
| RSD | Relative standard deviation |
7.0 ANNEXURES:
| Annex. No. | Title |
| 01 | Label of Working Standard vial |
| 02 | Certificate of Analysis- Working Standard |
| 03 | Working Standard Consumption Record Register |
| 04 | Analytical Worksheet for Working Standard |
8.0 SOP REFERENCES
- British Pharmacopoeia
END OF THE SOP
ANNEXURES :
Annex. No. 01 Label of Working Standard vial
Annex. No. 02 Certificate of Analysis – Working Standard
Annex. No. 03 Working Standard Consumption Record Register
Annex. No. 04 Analytical Worksheet for Working Standard
