Method validation across the disciplines—Critical investigation of major validation criteria and associated experimental protocols

Application of the β-expectation tolerance interval to method validation of the M30 and M65 ELISA cell death biomarker assays

“…There are 3 classic approaches in validation to decide whether the technical characteristics of an analytical method are performing within specifications to an acceptable level [34][35][36]. The first referred to as the descriptive or 'fixed' criterion [37] decision rule, is when an acceptance limit is set a priori to the experimental phase, normally based on the desired level of performance expected from the particular class of assay under investigation, usually agreed through international standardisation [38][39][40].…”

“…The second is based on equivalence or a confidence interval, which can incorporate both precision and bias parameters and aligns the acceptance limit for each of these parameters based on the generation of pre-study validation data at either the 95% (more commonly) of 99% (less commonly) confidence interval. Its success is based on an accurate assessment of the error associated with each parameter by the accumulation of large sets of population data [35,41]. The third approach which is referred to as the difference approach, and is less frequently utilised in biomarker research, if at all, is performed using statistical hypothesis testing [36].…”

Evaluation of analytical calibration based on least-squares linear regression for instrumental techniques: A tutorial review

“…Although there is a general 22 agreement among these validation guidelines, diversity prevails in terms of 23 nomenclature, methodology employed and acceptance criteria [14]. In addition, 24 analytical chemists mostly are familiar with the validation guidelines relating to their 25 research area but experimental designs and acceptance criteria are different among 26 diverse disciplines [15]. Specifically for the pharmaceutical field, representatives from 27 the industry and regulatory agencies from Europe, USA and Japan tried to harmonize 28 the terms and basic requirements for new pharmaceuticals trough the validation 29 guideline so-called International Conference of Harmonization (ICH) [16].…”

Development of an analytical method for the targeted screening and multi-residue quantification of environmental contaminants in urine by liquid chromatography coupled to high resolution mass spectrometry for evaluation of human exposures

“…The determination of these limits was therefore assessed on the standard deviation of a blank. For these substances, the detection and quantification limits were obtained as follows: Mean Blank Noise + 3 standard deviation of blank and Mean Blank Noise + 10 standard deviation of blank, respectively [44]. In the first step, it was necessary to inject a series of samples of the blank matrix (without spiking) to determine the standard deviation of the blank.…”