OBJECTIVE:
To provide a procedure for controlling and storage of reference standards.
SCOPE:
This procedure shall apply to all the reference standards that are used for analysis.
RESPONSIBILITY:
- It is the responsibility of the QC Executives for ensuring that the standards are used appropriately, stored in the right conditions.
- It is the responsibility of the QC Manager to ensure that all standard prepared & qualified against reference standard & documented.
PROCEDURE:
Classification of Reference Standard:
- Primary Standards: These have been prepared and classified as such by competent accredited bodies such as USP, BP, FDA, WHO. Unless otherwise stated primary standards are taken as being 100% pure.
- Secondary Standards: This is prepared from a selected batch of an active ingredient after it has been tested against a Primary Standard and has passed all monograph requirements.
Classification of Secondary Reference Standards:
- Selection of Sample, Sample quantity & sampling of Raw material
- Select the latest approved batch of Raw material preferably having maximum assay.
- Sampling quantity shall be calculated on the basis of the sample required for analysis and preparation of secondary reference standard.
- Perform the sampling as per current SOP of sampling of secondary reference standard
2. Analysis of material:
- Carry out the following test for preparation of secondary reference standard
Assay*
Loss on drying/Water content
I.R. (Where applicable)
* Assay shall be done in Triplicate
- Enter the results in the data sheet for secondary reference standard of the respective material. Secondary reference standard data sheet shall be prepared as per Attachment-I
- Calculate the average of three assay values obtained on as is basis.
- The RSD of three assay values obtained on as is basis should not be more than 1.0% for chemical assay and 5.0% for microbial assay.
- When approved the following should be entered on the Certificate of Analysis for Secondary Standards:
a. Name of Secondary standard.
b. Date of certification.
c. Expiry date.
d. Assay (as such).
e. Loss on drying/ Water content
f. Analyst’s signature and date.
g. Approval signature and date.
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3. Preparation & labelling of vials
- Prepare the List of secondary reference standard as per Attachment-II (List of Secondary reference standard). Assign the reference number to Secondary Reference Standard as follows. Number the Secondary Reference Standard as
SRS/XXX-YY/BB
Where,
SRS : Secondary Reference Standard,
XXX : Corresponds to the serial no starting from 001.
YY: Corresponds to the last two digit of year in which secondary
reference standard prepared.
BB: Corresponds to the no. of vial prepared for particular
secondary reference standard starting from 01.e.g.
SRS/001/20-01, where SRS – Secondary Reference Standard,
001 is the reference no for – Ibuprofen, 20 describes the secondary reference standard prepared in year 2020, 01 – First secondary reference standard in series in the year 2020. The second secondary reference standard of Ibuprofen prepared in the year 2020 shall be numbered as SRS/001/20-02
- Store the material in light resistant glass vials closed with cap.
- Label the vials with the following details.
a. Name of Secondary Reference standard
b. Ref. No.
c. Assay (On as such basis)
d. LOD/Water content
e. Date of preparation
f. Use before
- Assign one-year shelf life for secondary reference standard when expiry of sample used for secondary reference standard preparation is more than one year
- If the secondary reference standard is not qualified in-house and is supplied by an external party, the results from the certificate of analysis shall be adopted and recorded on the secondary reference standard analytical report. A reference standard number is assigned to such reference standard and recorded.
4. Storage and handling of reference standards:
- Store all secondary reference standard in A.C control area (below 27°C)/ refrigerator (Between 2 to 8°C). Keep the vials air tight protected from heat, moisture and light. Primary Standards should be stored in their original stoppered containers.
- Moisture sensitive Reference Standards must be stored in desiccators.
- Unless otherwise directed, Reference Standard must be dried before use as directed in their labeling or in the monograph.
- Reference Standards will be used in the assay of certain raw material or finished dosage forms, or to determine a specific impurity in either.
5. Precaution:
- Analyst shall check the expiry of secondary reference standard before use.
- The analyst shall keep the standard out of the recommended storage for as short as possible to protect from light and moisture.
- Equilibrate secondary reference standard to room temperature before use, which are stored in refrigerator.
- Use required quantity and do not put back the secondary reference standard in vial.
- Ensure proper closing of the vial after use.
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