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Validation criteria for chemical analysis, Heng Aie Yin Sia Wan Ern …
Validation criteria for chemical analysis
Glossary
Accuracy
nearness of a result or the mean of a set of
measurements to the true value.
Analytical batch
analyzed the samples together with the same method sequence and the same lots of reagents
and the manipulations common to each sample within the same time period or in continuous sequential time periods.
Detection limit
the lowest amount of analyte in a sample which can be detected but not necessarily quantitated as an exact value.
(
LOD
)
Limit of detection is the lowest concentration level that can be determined statistically different from a blank at a specified level of confidence. It is determined from the analysis of sample blanks.
(
MDL
)
Method detection limit is the minimum concentration of a substance than can be measured and reported with 99% confidence that the analyte concentration is greater than zero. It is determined from analysis of a sample in a given matrix containing the analyte.
Limit of quantitation (LOQ)
level above which quantitative e results may be determined with acceptable accuracy and
precision
LOQ
must be a value greater than MDL
Linearity
ability of the method to elicit results that are directly proportional to analyte concentration within a given range.
Method Detection Limit (MDL)
The minimum amount or
concentration of analyte in the test sample that can be reliably distinguished from zero
dependent on sensitivity, instrumental
noise, blank variability, sample matrix variability, and dilution factor
Non-standard method
method that is not taken from authoritative and validated sources. This includes methods from scientific journals and unpublished laboratory-developed methods.
Precision
agreement between a set of replicate
measurements without assumption of knowledge of the true value.
standard deviation or confidence limit of
test results
Ruggedness or robustness
measure of an
analytical procedure’s capacity
indication
of its reliability during normal usage
unaffected by small, but
deliberate variations
Range
interval between the upper and lower
concentration of analyte in sample
Specificity
ability of a
method to measure analyte in the presence of components
Sensitivity
change in instrument response
slope of the calibration curve near theLOQ.
Standard method
published by
international, regional or national standards-writing bodies
FDA "official" methods
methods found in compendia specified in the FD&C Act and prescribed in the CFR and methods in applications and petitions that have official status are included.
preferred for use and are verified for use in the laboratory
supplemented with additional details in the form of a laboratory procedure to ensure consistent application
methods specified by the manufacturer of the equipment are considered as standard methods
Validation method
establish the performance characteristics and limitations of a method
Selectivity
extent to which a method can determine particular analyte(s) in a mixture(s) or matrix(ces) without interferences from other components of similar behavior
Verification
confirmation by examination and
provision of objective evidence
Quantitative
System suitability
Accuracy
repeatability
Precision
reproducibility
Linearity
Single analyte / single matrix methods - R2≥0.995
Multi residue, multi class mass spectrometer - R2 ≥ 0.990
Limit of Detection
MLD should be within ± 30% of the
known value
LOD determined by analyzing sample blanks, calculating the standard
deviation, and expressed as the mean plus 3 standard deviations.
Limit of Quantitation
Minimum amount/concentration that can be quantified with
acceptable precision
Analyze reference materials
selecting spike ranges
Run a matrix blank
R2 (coefficient of determination) for a calibration curve
Single analyte：R2 should be ≥0.995
Multi residue-R2
value of ≥ 0.990
working range or target level.
lowest calibrator- one-half
this concentration
highest calibrator -twice this concentration
Certified
Reference Material (CRM)
80% - 120% of stated or known
value
percent recovery
within +20% of the
known value
standard curve
analyze calibration standards with known analyte
Heng Aie Yin
Sia Wan Ern
Yong Hui Syen