Scientist Solutions - USP Reference Standards

Bettye said:

Does any one have an information what is required for making one's own reference standards, instead of purchasing USP's reference standards?

What is the validation like? Is it worth the the trouble (cost vs. time)?

I'm new in QC, so any advice would be helpful.

Title: PRIMARY AND SECONDARY REFERENCE STANDARD GENTAMICIN:

1.
PURPOSE
This procedure provides guidelines for the use, qualification and documentation of primary and
secondary standards.

2.
GENERAL
The procurement, storage and use of all reference standards in the proper manner are vital to
accurate testing. Thus, an official reference standard, either primary standard or a qualified
secondary standard must be used for all testing which requires a reference standard.

3.
MATERIALS
Certificate of Analysis (COA)
Loss on Drying (LOD)
Test Item Specification (TIS)
United States Pharmacopoeia (USP)
Reference Standards (Primary or Secondary standards)
4.
SAFETY
Standard plant safety regulation applies.
5.
RESPONSIBILITY/AUTHORITY
Shownintext.
6.
PROCEDURE
6.1.
Primary Standards: Standards supplied by official agencies such as the NIST, USP, EP, or
BP and their values are certified.
6.1.1.
All primary standards will be stored as recommended in the compendial monograph
or as directed by the manufacturer/supplier. They all should be stored in their
original containers away from heat and protected from light. Keep container tightly
closed and store in a dry, cold place.
6.1.2.
It is the responsibility of each analyst to ascertain that his/her particular supply for
primary standard is current and within the established expiration dating.
6.1.3.
Accept the potency as stated on C of A or label amount.
6.1.4.
Where a primary standard is required to be dried before using, transfer an appropriate
amount to a clean dry vessel. Do not use the original container as the drying vessel,
and do not dry a reference standard repeatedly at temperatures above 25°C.

6.1.5. Prepare primary reference standard per Gentamicin Microbial Assay: BCLT 01-2100-
02-036 and follow Section 5.1.
6.2. Secondary Standards: Standards that have been assayed and are used to determine the assay
value of samples. A secondary standard may be used in place of a primary standard, once the
material has been qualified. Qualification of a secondary standard is determined based on
the following method.
6.2.1. Direct determination per BCLT 01-21-00-02-036 and comparison to a primary
standard.
6.2.2. All compendial secondary standards should be stored as per the compendial
monograph. All noncompendial secondary standards can be stored as recommended
by the manufacturer. Special precaution and appropriate technique should apply
when handling and transferring a secondary standard to a container for storage.
6.2.3. Establishing Standards and Expiration Dates
6.2.3.1. The standard will be prepared per according to the appropriate monograph,
TIS, or BCLT.
6.2.3.2. When the secondary standard is qualified, it must be tested by two separate
technicians in duplicate on the same day, or by the same technician in
duplicate on two different days.
6.2.3.3. All four results should meet the target concentration specified for primary
standard per appropriate monograph or TIS.
6.2.3.4. When results are out of specification, initiate the investigation to identify
for the cause for the failure per RA/QAOP 01-10-01-10, Out of
Specification Investigation.
6.2.3.5. All compendial secondary standards should be stored as per primary
standard.
6.2.3.6. Once the secondary standard is qualified and accepted, prepare secondary
standard monthly per BCLT 01-21-00-02-036.
6.2.3.7. The secondary standard shall have the same shelf life as primary standard.
6.2.3.8. All secondary standards should be properly qualified and approved by
appropriate supervisor prior to use.
6.3. Documentation Requirements
6.3.1. A formalized report demonstrating the legitimacy of the secondary standard has to be
approved by the appropriate supervisor.

6.3.2.
The raw material may be stored at the specified temperature in a sealed container for
up to 12 months prior to use.
6.3.3.
The use of all reference standards will be properly documented in the laboratory
notebooks.
7.
REFERENCES
7.1.
CCOP 01-12-01-02, Use of Primary and Secondary Reference Standards
7.2.
TIS SN-16-30-D8-103, Gentamicin Sulfate, 1.0 mg/mL Gentamicin in 0.9% NaCl Injection
7.3.
BCLT 01-21-00-02-036, Gentamicin Microbial Assay
7.4.
Certificate of Analysis for Gentamicin Standard
7.5.
USP