| Preparation and Handling of Working Standard |
| 1.0 OBJECTIVE To lay down procedure for Preparation and Handling of Working Standard in quality control department. 2.0 SCOPE This SOP is applicable for Preparation and Handling of Working Standard in quality control department. 3.0 RESPONSIBILITY QC – Officer/ Sr. Officer / Executive and above. 4.0 ACCOUNTABILITY Head-QC 5.0 PROCEDURE 5.1.1 Working Standard 5.1.2 Working standards is to be prepared from current approved raw material against the current lot of reference standards procure of registered pharmacopeia agencies. 5.1.3 The raw material batch is selected with highest expiry and with highest potency. 5.1.4 All lot details of working standards should be mentioned on current working standard COA for traceability. 5.1.5 Following are the test to be carried out for qualification of a working standard. 5.1.5.1 Description 5.1.5.2 Identification 5.1.5.3 Assay 5.1.5.4 Loss on drying / Water 5.2 Standardization procedure: 5.2.1 Analyze the raw material against the reference standard as per respective STP. 5.2.2 Carry out the test for description by visual evaluation and record. 5.2.3 Calculate the assay of the sample to be standardized against reference standard. Carry out the sample analysis in triplicate preparation. 5.2.4 Determine LOD / Water (by KF) in single. 5.2.5 Prepare 15 vials of standardized working standard. Use one vial for one month. Fill approximately 2.0 g quantity of working standard in each vial. After completion of one-month interval discard any material remaining in the vial and continue with next vial. Note: For costly materials, prepare two vials for use. 5.2.6 Vial no. 13 to 15 should be used in case of any breakage and consume within one month’s then issue of vial no. 13 to 15. 5.2.7 Perform the test mentioned in the Work sheet and fill the details as per the respective material. 5.2.8 The average of three assay values should be used to determine the working standard potency. The RSD of 3 values should not be more than 2.0 %. Prepare COA of all the working standards (as mentioned in format No.: XXX). 5.3 All running vials should be kept in desiccators containing silica and another stock vials should be packed by wrapping with poly film, kept in a tray, and stored as per the individual monograph / MSDS. 5.4 After the preparation of the WS, allot a unique number as below: E.g. QC/WS/001/XX QC : Quality Control WS : Working Standard 001 : Continuous serial number starting from 001 XX : Last two digit of Standard qualification year. For example: QC/WS/001/23. Prepare the WS label and stick properly to a respective vial (as mentioned in Format No.: XXX. 5.5 The WS should never be used after the validity. If any change in description is observed during storage the same should be discarded. 5.6 A thorough investigation should be made to find out the reason for such change and documented. 5.7 Refrigerated vials are to be brought to room temperature before use. 5.8 All working standard should be listed in Format No. XXX. 5.9 After every use of working standard, make entry in working standard usage log as per format number QC01-042/F04. 5.10 On every first date of month, new vials shall be opened and all the last month vials shall be discarded. Make the entry of vial issuance/ destruction in the format number XXX. 5.11 In-House Standard: 5.11.1 When an official Pharmacopoeia reference standard is unavailable for a particular material, an in-house standard must be qualified. 5.11.2 Material of approved batch having high potency and high expiry shall be selected from all available batches of the same material for qualification. 5.11.3 A protocol shall be prepared for Evaluation & Characterization of the In-house standard refer format no. XXX. 5.11.4 Following are the test to be carried out for qualification of In-house reference standard. • Description • Identification • Related Substance (area normalization) • Loss on drying / Water 5.11.5 Calculate the related substance of the sample to be standardized against (area normalization). Carry out the sample analysis in triplicate preparation. 5.11.6 RSD of the test result shall be within the limit as specified in the given below: Test RSD% Related Substances Total Impurities: NMT 15% (Below LOQ values shall not be considered for calculation of RSD) 5.11.7 Determine LOD / Water (by KF) in single. 5.11.8 Calculate the Potency using the formula below: Potency= 100- (Total Impurities + % LOD/ Water) 5.11.9 Prepare 15 vials of standardized In-house standard. Use one vial for one month. Fill approximately 2.0 g quantity of In-house standard in each vial. After completion of one-month interval discard any material remaining in the vial and continue with next vial. 5.11.10 Vial no. 13 to 15 should be used in case of any breakage and consume within one month then issue of vial no. 13 to 15. 5.11.11 After the preparation of the WS, allot a unique number as below: E.g. QC/IHS/001/XX QC : Quality Control IHS : In-House Standard 001 : Continuous serial number starting from 001 XX : Last two digit of Standard qualification year. For example: QC/IHS/001/23. 5.11.12 Prepare the In-House standard label and stick properly to a respective vial (as mentioned in Format No.: XXX). 5.12 The In-house standard should never be used after the validity. If any change in description is observed during storage the same should be discarded. 5.13 All In-House standards should be listed in Format No. QC01-042/F08. 5.14 After every use of working standard, make entry in working standard usage log as per format number XXX. 9.0 ABBREVIATIONS SOP Standard Operating Procedure No. Number QA Quality Assurance QC Quality control MSDS Material safety data sheet WS Working standard RSD Related standard deviation COA Certificate of analysis LOD Loss on drying KF Karl Fischer |
