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Validation is the confrmation by examination and the provision of efective evidence that the particular requirements for a specifc intended use are fulflled. ICH Q2(R1) defnitions Specifcit Specifcity is the ability to assess unequivocally the analyte in the presence of components which might be expected to be present.
Validation is the confrmation by examination and the provision of efective evidence that the particular requirements for a specifc intended use are fulflled. ICH Q2(R1) defnitions Specifcit Specifcity is the ability to assess unequivocally the analyte in the presence of components which might be expected to be present.
Validation is the confrmation by examination and the provision of efective evidence that the particular requirements for a specifc intended use are fulflled. ICH Q2(R1) defnitions Specifcit Specifcity is the ability to assess unequivocally the analyte in the presence of components which might be expected to be present.
Validation is the confrmation by examination and the provision of efective evidence that the particular requirements for a specifc intended use are fulflled. ICH Q2(R1) defnitions Specifcit Specifcity is the ability to assess unequivocally the analyte in the presence of components which may be expected to be present. Typically these might include impurities, degradants, matrix, etc. ac! of specifcity of an individual analytical procedure may be compensated by other supporting analytical procedure"s#. $%Validation &.'( $xample of a Selectivity determination by )omparison of )alibration ines !cc"#ac The accuracy of an analytical procedure expresses the closeness of agreement between the value which is accepted either as a conventional true value or an accepted reference value and the value found. This is sometimes termed trueness. $%Validation &.'( $xample of the *ccuracy determination by a t+test 1 $#ecision The precision of an analytical procedure expresses the closeness of agreement "degree of scatter# between a series of measurements obtained from multiple sampling of the same homogeneous sample under the prescribed conditions. ,recision may be considered at three levels( repeatability, intermediate precision and reproducibility. ,recision should be investigated using homogeneous, authentic samples. -owever, if it is not possible to obtain a homogeneous sample it may be investigated using artifcially prepared samples or a sample solution. The precision of an analytical procedure is usually expressed as the variance, standard deviation or coe%cient of variation of a series of measurements. "i# .epeatability .epeatability expresses the precision under the same operating conditions over a short interval of time. .epeatability is also termed intra+assay precision. $%Validation &.'( $xample of the .epeatability determination evel by evel from /ultiple /easurements 2 "ii# 0ntermediate precision 0ntermediate precision expresses within+laboratories variations( diferent days, diferent analysts, diferent equipment, etc. "iii# .eproducibility .eproducibility expresses the precision between laboratories "collaborative studies, usually applied to standardi1ation of methodology#. %etection &i'it The detection limit of an individual analytical procedure is the lowest amount of analyte in a sample which can be detected but not necessarily quantitated as an exact value. Q"antitation &i'it The quantitation limit of an individual analytical procedure is the lowest amount of analyte in a sample which can be quantitatively determined with suitable precision and accuracy. The quantitation limit is a parameter of quantitative assays for low levels of compounds in sample matrices, and is used particularly for the determination of impurities and2or degradation products. $%Validation &.'( $xample of the 3etection and 4uantitation imit determination from a calibration curve 3 &inea#it The linearity of an analytical procedure is its ability "within a given range# to obtain test results which are directly proportional to the concentration "amount# of analyte in the sample. $%Validation &.'( $xample of the inearity determination 4 Ran(e The range of an analytical procedure is the interval between the upper and lower concentration "amounts# of analyte in the sample "including these concentrations# for which it has been demonstrated that the analytical procedure has a suitable level of precision, accuracy and linearity. Ro)"stness The robustness of an analytical procedure is a measure of its capacity to remain unafected by small, but deliberate variations in method parameters and provides an indication of its reliability during normal usage. $%Validation &.'( $xample of the .obustness determination 5 *nce#taint 5ncertainty is a parameter associated with the result of a measurement, that characterises the dispersion of the values that could reasonably be attributed to the measurand. The parameter may be, for example, a standard deviation, or the width of a confdence interval. 5ncertainty of measurement comprises, in general, many components. Some of these components may be evaluated from the statistical distribution of the results of series of measurements and can be characterised by standard deviations. The other components, which also can be characterised by standard deviations, are evaluated from assumed probability distributions based on experience or other information. The 0S6 7uide refers to these diferent cases as Type * and Type 8 estimations respectively. $%Validation &.'( $xample of the 5ncertainty determination from ,artial 5ncertainties 6 Cont#ol Cha#t * chart on which observations are plotted as ordinates in the order in which they are obtained and on which control lines are constructed to indicate whether the population from which the observations are being drawn is remaining the same. )ontrol charts are used especially in industrial quality control. ISO 17025:2005+ chapte# 5,-,1 states: The laboratory shall have quality control procedures for monitoring the validity of tests and calibrations underta!en. The resulting data shall be recorded in such a way that trends are detectable and, where practicable, statistical techniques shall be applied to the reviewing of the results. This monitoring shall be planned and reviewed and may include, but not be limited to, the following( a. regular use of certifed reference materials and2or internal quality control using secondary reference materials9 b. participation in interlaboratory comparison or profciency+testing programmes9 c. replicate tests or calibrations using the same or diferent methods9 d. retesting or recalibration of retained items9 e. correlation of results for diferent characteristics of an item. $%Validation &.'( $xample of a )ontrol )hart : example from the 0S6 ;<=; standard 7 Cali)#ation )alibration is a basic tool needed in quantitative analysis to construct the relationship between the measured analytical signal and sample concentration. )alibration process typically consists of "i# 3efning the purpose and range of calibration, "ii# ,reparation and execution of calibration experiments, "iii# )onstruction of the model, "iv# 5se of the model in routine practice $%Validation &.'( $xample of )alibration 8 Inte#la)o#ato# Co'pa#ison 0nterlaboratory studies2comparisons are performed with the aim of evaluating the extend of similarity in the results obtained by diferent laboratories using the same method. The study typically consists of "i# ,lanning, "ii# Selection2recruitment of laboratories, "iii# $xecution according the plan and "iv# statistical evaluation of results $%Validation &.'( $xample of 0nterlaboratory Study according the 0S6 ;<=; standard 9 .eat"#es Software compliance /odules o /ethod Validation o 5ncertainties o )ontrol )harts o )alibration o 0nterlaboratory )omparison o $lectronic aboratory oogboo!s o Software Validation ,roduct Tour /lect#onic &a)o#ato# &oo()oo0s Traceability of test results, samples, documents, equipment calibrations, reference standards, etc., is a basic requirement in both the 0S6 >?'<= accrediated and 7x, laboratories. Software $%Validation enables to maintain and control the following specifc laboratory loogboo!s( a. Samples9 b. Specifcations9 c. $quipment, d. 3ocuments, e. 3eviations, f. .eference standards9 g. )hemicals9 h. Volumetric solutions9 i. )ontacts. 10 $%Validation &.'( $xample of an electronic laboratory loogboo! .eat"#es Software compliance /odules o /ethod Validation o 5ncertainties o )ontrol )harts o )alibration o 0nterlaboratory )omparison o $lectronic aboratory oogboo!s o Software Validation ,roduct Tour 11