johne0212
第1楼2010/05/13
LoD and LoQ could be assessed by different approaches. From the following procedures, choose the one which is the most appropriate to the method to be validated:
1) LoD and LoQ estimation by signal/noise ratio procedure (chromatographic and spectroscopic methods):
Parameter Minimum requirement
Samples: Spike one blank sample at 3 low concentration levels close to the expected LoD and LoQ (at least 3 concentration levels)
Number of replicates: Analyze each spiked sample 3 times
2) LoD and LoQ by standard deviation of the blank (gravimetric, photometric, enzymatic, titrimetric methods):
Parameter Minimum requirement
Samples: 1 blank sample (or 1 sample with a low amount of analyte)
Number of replicates: At least 6 replicates
3) LoQ by target performance characteristics (precision and/or recovery):
Parameter Minimum requirement
Samples: Spike one blank sample at low concentration levels close to the expected LoQ (at least 3 concentration levels)
Number of replicates: Analyze each spiked sample at least 3 times.
4) LoQ corresponding to the lowest calibration point (lowest validated level)