Selection, Standardization and Storage of reference and working standards

1.0       Purpose    :    To provide instructions for selection, standardization and storage of reference and         working standards.

2.0        Objective   :  To provide documented procedures for selection, standardization and storage of reference and working standards.

3.0       Scope        :     This procedure is applicable for selection, standardization and storage of reference         and working standards in QC Department.

4.0       Responsibility   :

§          Primary     : QC Chemist

§          Secondary : Overall QC Officer

5.0        Procedure     :

·        Selection and Storage of Reference Standards.

Ø       Reference standard/substance RS are issued by the respective Pharmacopoeia        Commission.

Ø       They are the official standards.

Ø       Select current lots of the reference standards.

Ø      Store them in suitable container (e.g. desiccators) moisture free atmosphere under temperature-controlled condition.

Ø      Maintain records for reference standard in respective logbook.

·        Selection, Standardization and Storage of Working Standards.

Ø      Working Standard shall be used for routine analysis.

Ø      Working standards should be standardized at regular intervals against the reference standards.

·        Procedure for Raw Materials working standards.

Ø      Working standards are selected from amongst the raw materials received and approved by the QC.

Ø      The selected raw material’s working standards having high purity or negligible impurities and low moisture content.

Ø      For solvent working standard shall be used from any reputed external manufacturer, pure grade materials with certificate of analysis.

Ø      Selected raw material working standard shall be re-tested and note down the observations in respective worksheet.

·        Procedure for Intermediates and Finished Products working standards.

Ø      Selected intermediate and finished product working standards can be prepared by

                                          repeated crystallization in suitable solvents.

Ø      These working standard having high purity or negligible impurities and low moisture / loss on drying content.

Ø      R&D and QA should authorize procedures for the preparation of intermediate and finished products working standard.

Ø      Approved methods should be used for the preparation of working standard.

Ø      Working standards should be standardized at regular intervals against the reference standards or previous working standards.

Ø      Frequency of standardization: Once in a Year.

Ø      Standardization should be done in triplicate analysis.

Ø      Loss On Drying / Moisture content and Assay tests parameters taken for standardization.

Ø      The average value should be reported.

Ø      Note down the observations in respective worksheet. And maintained relevant graphs in respective working standard file.

Ø      Re-standardization shall be done within + 15 days from the said date.

Ø      Bottle of working standards should be stored in a desiccators having activated silica gel, and kept at controlled temperature.

Ø      Information on status label includes name of material, working standard batch number, purity, LOD / moisture content, date of preparation, valid up to etc.

·        Storage of working standards.

Ø            After standardization the working standard is divided into equal quantities

Ø       (Approx – 2 to 10 gm each) and filled appropriate vials / bottles (minimum 2 to 4). Vials should be cleaned and dried.

Ø      Each vial/bottle is to be used for three months from the date of opening and then discarded. Open on date shall be mentioned on the label.

Ø      The other information of the label includes name of material, open on date, purity, LOD/Water value, and use before date and valid up to.

Ø      The bottles are then sealed and kept in desiccators at the prescribed storage condition for the future use.

Ø      The temp of the area of storage is maintained and monitored daily.

Ø      The last bottle is kept for use as a reference std. during next standardization. Reference standard to be re-validated every year.