Chemistry Reference
In-Depth Information
A.5.9 S
olutIon
S
tAbIlIty
Stability of the stock standard solution will be evaluated by comparing the average
assay value (duplicate injections) of a peak in a freshly prepared dilution of the stored
stock standard solution (at both refrigerated and room temperature conditions) versus
the freshly prepared working standard solutions at each time interval.
The sample stability will be evaluated by calculating the percent assay at each
time interval and comparing the results against the assay value at time 0, and must
not differ by more than 30%.
A.6
exAmple AcceptAnce crIterIA
parameter
Acceptance criteria
System Suitability
Linearity
r
2
≥ 0.995
Resolution
≥2.5
Retention Time
6.5 ± 1 min
Overall Standard Precision (6 injections)
Area RSD ≤ 10%
Check Std. Recovery
90% to 110%
Specificity
All peaks of interest are resolved from one another.
Lack of detectable peaks co-eluting with the peaks of interest in the
chromatograms of a diluent blank
Accuracy
Assay level
97% to 103% NMT 2% RSD
Impurity level
75% to 125% NMT 25% RSD
Precision (repeatability)
RSD ≤ 2% for both retention time and area
Precision (intermediate)
Assessed for equivalence using the Student's t-test for establishing the
equivalence of means. The test will be applied at the 95% confidence level.
LOD
Detectable peak
LOQ
Recovery 75% to 125% with NMT 25% RSD for the analysis of six samples
Robustness
Meet system suitability criteria for all experiments and samples ≤30%
difference from original method conditions
Solution Stability
(Stock standard and
samples)
The Reference Standard and Sample Preparations stored at both ambient and
2°C-8°C should remain within 100% ± 2% of the initial assay value at each
storage time interval
A.7 stAtement oF expected results
It is expected that the results obtained during this validation will demonstrate the
suitability of the test method to accomplish its intended purpose.
A.8 dAtA recordIng
All sample data will be recorded in accordance with standard operating procedures
and quality systems. It is sometimes customary to refer to notebooks, data forms, or
other recording means (e.g., electronic laboratory notebooks). If data forms are used,
examples should be attached to the protocol as an appendix, or included as part of
the method.
