Overview of Validation Stability Exercises and Criteria
Validation Exercise Minimum
Experiments
Performance Criteria
Stock Solution n ≥6; long term at typical storage conditions; bench top at conditions representing typical processing conditions for ≥6 hours Precision of area response or relative response must be £15.0% RSD; RD within 7.0% for analytes, 20.0% for internal standards
Bench top ≥ 4 hours
n ≥6 at QC Low and High levels
Mean accuracy within ±15.0% RE of nominal; precision £15.0% RSD
Freeze/Thaw 3 freeze/thaw cycles
n ≥6 at QC Low and High levels
Mean accuracy within ±15.0% RE of nominal; precision £15.0% RSD
Long term n ≥ 6 at QC Low and High levels at -10 to -30°C or -50 to -90°C for at least 1 and 4 months. Mean accuracy within ±15.0% RE of nominal; precision £15.0% RSD
Reinjection Reproducibility Calibrations standards (CS) and QCs (n=6 at each level) re-injected from an acceptable validation batch run, maintained at autosampler temperature for ≥72 hours. Mean accuracy within ±15.0% RE of nominal; precision £15.0% RSD; calculated using calibration standards from re-injected run
Extract Stability Stored extracts at QC Low, Mid, and High levels (n=6) maintained at autosampler temperature for ≥72 hours. Mean accuracy within ±15.0% RE of nominal; precision £15.0% RSD; calculated using freshly extracted curves or back calculated using the original curves from the batch the aged extracts were originally extracted and injected
Table 3: Overview of Validation Stability Exercises and Criteria
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