QCS-012 - Quality Operations Procedures for Pharmaceutical, API, and Biotechnology - page 57

SOP No. QCS-012.00 Effective date: mm/dd/yyyy
Approved by:

2. Secondary or internal working standard
• The equipment used is the one speciied in the compendial monograph applicable to
the method used to certify a potential secondary or internal working standard against
a primary reference standard.
• All the reagents to be used are those speciied in the oficial monograph applicable to
the method used to certify a potential secondary or working standard using fresh certi-
fied raw material as a sample. Perform the standard preparation and sample prepara-
tion, and determine the purity of the raw material (secondary reference vs. the primary
reference standard) according to the procedure in the monograph that is being used.
• Perform the analysis as mentioned below, using separate standard and sample weigh-
ing for each determination.
• Calculate the assay result of the house standard versus the primary reference standard
for each of the individual determinations.
• Calculate the average and percent relative standard deviation (% RSD) for all the assays.
• If the % RSD is 2.0 or less, then the potential secondary or house standard can be used
as a reference standard for further analytical work using its average assay value as its
purity.
• Record all assay data in the notebook.
• All the secondary or in-house standards have to be restandardized after 1 year.

12.5 Procedure for internal Working standards (secondary

reference standards) PreParation

12.5.1 S amPling
After the material has been identified as a potential internal working standard, sampling of incom-
ing raw material should be performed for characterization and certification testing. Sampling con-
siderations should include, but are not limited to, the following:

1. The material is fresh (not older than 6 months).

2. The immediate container and packing components are intact and in good condition at the
time of receipt.

3. No unfavorable, uncontrolled conditions occurred during transit, for example, exposure to
excessive humidity or heat.

4. Appropriate documentation is included with the shipment, that is, dated purchase order
and invoice, certificate of analysis including manufacturing date, and data for all tests
required as per specifications.

5. Samples are taken under laminar flow conditions into clean, dry, sterilized containers of
adequate size and provided with hermetic seal: samples are properly labeled and assigned
an internal lot number.

6. The amount of sample is sufficient for all qualification tests and the quantity of material is
sufficient for 1 year's usage after the qualification.

12.5.2 t eSting
The samples of materials for qualification as internal working standards will be tested against cur-
rent primary standards according to current standard control procedures of ABC Pharmaceutical
Company and/or compendial specifications and methods.