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 |