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Method validation criteria - EffiValidation

The method validation criteria that can be evaluated are:

Repeatability
Accuracy
Linearity
Reproducibility
Selectivity/Specificity
Limit of Detection/Quantification
Robustness/Ruggedness
Sensitivity
Range
Intermediate precision

Repeatability

Repeatability is the precision obtained under the best possible circumstances (i.e. within the same laboratory, by the same analyst, by the same instrument, within one day when possible) and measures the size of random error included in the method results. Statistically, the precision is the dispersion of results around the mean, irrespective of whether the mean is correct representation of the true value. In the software EffiValidation, there are two ways of estimating repeatability:

Level by Level from Multiple Measurements
From Parallel Measurements

Level by Level from Multiple Measurements: results from repeated measurements obtained for the given concentration level are entered in rows; each row represents one concentration level, see example below:

Repeatability values are calculated as standard deviation and relative standard deviation for each level (row). The repeatability of the method is calculated as a polled variance/standard deviation

The software EffiValidation also automatically checks data for outliers (by means of the Cochran, Grubbs and Dixon test) and for data normality. Results are presented within other tabs of the same Results window OUTLIERS and NORMALITY:

Accuracy

Accuracy is the closeness of agreement between the test results and the true/accepted/assigned/reference value. If statistical testing shows that the difference between the test results and the reference value is not statistically significant, the validated method is considered accurate. In case the difference is found statistically significant, the method does not give accurate, but biased results (results include a systematic error). In the software EffiValidation, there are several ways of estimating accuracy depending on the situation:

Limited Concentration Range - Sample Reconstitution Possible
Limited Concentration Range - Reference Material Available
Large Concentration Range - Blank Material Available: t-test
Large Concentration Range - Blank Material Available: Regression
Large Concentration Range - Blank Material not Available: t-test
Large Concentration Range - Blank Material not Available: Regression
Comparison of Two Methods/Laboratories: t-test Level by Level
Comparison of Two Methods/Laboratories: t-test on Difference of Results

Linearity

Linearity of a test method is its ability (within a given range) to obtain results directly proportional to the concentration (amount) of analyte in the sample. Statistically, linearity describes the degree of the linear relationship between the test results and concentration. To evaluate Linearity, one of the following methods can be used in software EffiValidation:

Correlation and QC Coefficient
ANOVA for Lack of Fit
Significance of the Quadratic term - F-test
Sign Test

Reproducibility

Reproducibility is the precision obtained under the worst possible circumstances (i.e. in different laboratories, by different analysts, using different instruments, within one long time interval) and measures the size of random error included in the method results. Statistically, the precision is the dispersion of results around the mean, irrespective of whether the mean is correct representation of the true value. In the software EffiValidation, there are two ways of estimating repeatability:

Data Available
Results Available

Selectivity/Specificity

Selectivity is the ability of the method to provide a signal which is selective with respect to the property of interest (e.g. concentration of the analyte of interest). If the method is selective, the influence of potential interferences (matrix) on results is negligible. When the influence of interferences is significant, then the method cannot be considered selective. To evaluate Selectivity/Specificity, the following approaches can be used:

Comparison of Calibration Lines
Comparison of Results with a Standard
Comparison of Results with Measurements without the Interference

Limit of Detection/Quantification

Limit of Detection is the level above which the signal of a sample can be reliable distinguished from a blank; this means that starting from this level a qualitative determination can be carried out. Limit of Quantification is the level above which a quantitative determination can be carried out with sufficient reliability. Both limits are determined as a multiple of standard deviation of blank, from the calibration line or from noise in chromatography. To evaluate the Limits, the following methods can be used:

3s - IUPAC
3s - Every Sample Corrected for Blank
3s - Continuously Measured Blank
From Calibration Line
From Signal of Blank in Chromatography

Robustness/Ruggedness

Robustness is the resistance of the method to small changes in the settings of experimental conditions (e.g. to changes in pH of the mobile phase in case of HPLC method, to changes in the detector temperature of a GC method, etc.). Robustness is evaluated by means of experimental design. Two methods can be applied using EffiValidation:

Dongs algorithm
AOAC with evaluation

Sensitivity

Sensitivity is defined by IUPAC as the change in signal caused by a unit change of concentration/amount (i.e. slope of calibration line). Alternatively, Sensitivity is evaluated as the minimum difference in concentration between two samples that can be reliably distinguished with the given method. To evaluate Sensitivity, two algorithms can be used in EffiValidation:

From Calibration Line
Minimal Difference in the Validated Property

Range

Range characterizes the range of concentration within which validation parameters such as Repeatability, Accuracy, Linearity, etc. have been evaluated and verified.

Intermediate precision

Intermediate precision characterizes the spread of test results around the mean value caused by random errors. Data to evaluate Intermediate precision shall be recorded under the measurement conditions which are between Repeatability and Reproducibility conditions; this means e.g. different analysts, the same instrument, within an intermediate time period.

Chromatographic system suitability

Chromatographic system suitability parameters are used to verify that chromatographic characteristics are sufficient, a good separation, peak shaping and repeatability of injection can be obtained. In the software EffiValidation, there are two types of guidelines used to evaluate chromatographic system suitability:

Ph.Eur.:

Theoretical Plate Number - PhEur
Resolution - PhEur
Symmetry Factor - PhEur

FDA:

Capacity Factor
Resolution
Tailing
Theoretical Plate Number

Now available: Version 3.0!

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The main features and improvements

Software validation requirements met
Emphasis on statistical methods to validate testing/calibration methods, estimate uncertainties, develop control charts and calibration models, and to enable inter-laboratory comparison
Database of samples, equipment calibrations, standards, chemicals, documents and complaints included
Automatic evaluation of data and hypothesis testing
Automated generation of test reports in numerical and graphical form
Easy-to-use, intuitive handling based on Microsoft standards, feasible for all laboratory personnel
And much more...

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