Method precision reproducibility

The quantitation of phospholipids by means of NMR spectroscopy is a valid method. Method precision (reproducibility) and instrument precision show for the main component a standard deviation <1% components near the limit of quantitation have a standard deviation below 5%. In terms of the liposome lyophilisate preparation used the extraction recovery of the phospholipids was 100%. 

Analytical techniques (including method, accuracy, precision, reproducibility, robustness, limits of detection). 

The ability of a tPLC system to produce the same values of retention time and peak areas for analytes of interest is determined by evaluating the precision obtained under standardized conditions and analytical methods. The precision (reproducibility) values obtained are functions of the autosampler, cartridge, and detectors employed. Due to the parallel design of the tPLC system described in this chapter, reproducibility evaluations of retention time and peak area involved comparisons of results obtained for these parameters for consecutive runs performed in the same column and across different columns. 

In the context of an analytical method to establish the accuracy, precision, reproducibility, response function and the specificity of the analytical method with reference to the biological matrix to be examined and the analyte to be quantified. 

The CE method was validated in terms of accuracy, precision, linearity, range, limit of detection, limit of quantitation, specificity, system suitability, and robustness. Improved reproducibility of the CZE method was obtained using area normalization to determine the purity and levels of potential impurities and degradation products of IB-367 drug substance. The internal standard compensated mainly for injection variability. Through the use of the internal standard, selected for its close mobility to IB-367, the method achieved reproducibility in relative migration time of 0.13% relative standard deviation (RSD), and relative peak area of 2.75% RSD. 

The precision of a test method is the variability between test results obtained on the same material using a specific test method (ASTM, 2004 Patnaik, 2004). The precision of a test is usually unrelated to its accuracy. The results may be precise, but not necessarily accurate. In fact, the precision of an analytical method is the amount of scatter in the results obtained from multiple analyses of a homogeneous sample. To be meaningful, the precision study must be performed using the exact sample and standard preparation procedures that will be used in the final method. Precision is expressed as repeatability and reproducibility. 

Method precision refers to the variability in measurement of the same sample. There are three main components of method precision repeatability (also known as system or intraassay precision), intermediate precision (also known as inter-assay or intra-laboratory precision), and reproducibility precision (also known as ruggedness, overall or inter-laboratory... 

Precision and Accuracy. Statistical requirements for precision and accuracy have been established to ensure that the method is reproducible and free from bias. 

Control sample a representative batch of drug substance (or drug product). Typically, control samples are tested in all analyses to ensure consistency in method performance across different runs. Sometimes, they are used as part of the system suitability test to establish the run-to-run precision (e.g., intermediate precision, reproducibility). 

Some laboratory errors are more obvious than others, but there is error associated with every measurement. There is no way to measure the true value of anything. The best we can do in a chemical analysis is to carefully apply a technique that experience tells us is reliable. Repetition of one method of measurement several times tells us the precision (reproducibility) of the measurement. If the results of measuring the same quantity by different methods agree with one another, then we become confident that the results are accurate, which means they are near the true value. 

There are a number of general requirements for a test method it must have adequate precision, reproducibility etc. There are, however, particular attributes related to the purpose of testing -... 

What factors can be used to predetermine the quality and utility of a method An analyst must consider the following questions Do I need a proximate analytical method that will determine all the protein, or carbohydrate, or lipid, or nucleic acid in a biological material Or do I need to determine one specific chemical compound among the thousands of compounds found in a food Do I need to determine one or more physical properties of a food How do I obtain a representative sample What size sample should I collect How do I store my samples until analysis What is the precision (reproducibility) and accuracy of the method or what other compounds and conditions could interfere with the analysis How do I determine whether the results are correct, as well as the precision and accuracy of a method How do I know that my standard curves are correct What blanks, controls and internal standards must be used How do I convert instrumental values (such as absorbance) to molar concentrations How many times should I repeat the analysis And how do I report my results with appropriate standard deviation and to the correct number of significant digits Is a rate of change method (i.e., velocity as in enzymatic assays) or a static method (independent of time) needed ... 

Accuracy Range Precision Repeatability Intermediate Precision Reproducibility Precision System Precision Method Specificity Selectivity Linearity... 

Earlier guidelines defined precision in terms of system precision and method precision. System precision was the measure of reproducibility based on multiple measurements of a single sample preparation. Method precision was the measure of reproducibility based on analysis of multiple sample preparations. Ruggedness was a measure of day-to-day, analyst-to-analyst, and instrument-to-instrument variation. 

Matrix effects (ME), caused by co-eluting endogenous and exogenous matrix components, significantly affect the efficiency and reproducibility of the ionization process of target analytes. This phenomenon represents a major concern for LC-MS bioana-lytical method precision, accuracy, sensitivity, and robustness. Amongst the atmospheric pressure ionization interfaces used in LC-MS systems, ESI source is more prone to signal alteration (ion suppression or enhancement) due to matrix. Therefore, careful evaluation and correction for ME must be considered particularly with ESI-MS. 

Data from a number of different particle size analysis instrumental methods including light scattering, field flow fractionation, hydrodynamic chromatography and microscopy were obtained for a series of polymethylmethacrylate latexes and were compared to DCP results (2). These and other comparative results have demonstrated the accuracy of the instrument and method. The reproducibility and precision of the instrument also were studied and are reported elsewhere ( 1 ). 

Reproducibility is defined as the long-term variability of the measurement process, which may be determined for a method run, within a single laboratory, but on different days. Reproducibility also applies to a method, either run by different operators, different instruments, or a combination of the above. The reproducibility standard deviation is typically twofold to threefold larger than that for repeatability. Precision is often expressed relative to 1 day as intraday (within-day) precision or relative to a period of days, as interday (between days) precision. Reproducibility, in the sense of intralaboratory precision, is related to the procedure being performed at two or more laboratories as in, e.g., a collaborative study. 

The quantitative measure of a method s ruggedness is the precision behavior it exhibits over the course of the various operational scenarios, examined during the validation exercise. Generally, a rugged method s reproducibility is 2 to 3 times greater than the method s repeatability (inherent method precision under normal controlled operating conditions). 

Precision studies can be performed under different conditions, and are strongly influenced by variables such as temperature, source and quality of reagents, reproducibility of reagent delivery, and instrumental noise. Therefore, if all precision studies are done in the same laboratory (intralaboratory study) higher precision is expected in comparison with interlaboratory studies, where several laboratories produce the data used to prepare the method precision profile. 

For many years, the pectin industry has measured gel strength using the IFT-SAG method (Cox and Higby, 1944 IFT, 1959). In this method, pectin gels are prepared under standard conditions, and the amount of sag under the force of gravity is measured with a micrometer called a Ridgelimeter. The method is precise, reproducible and simple to operate, but it is incapable of a comprehensive evaluation of gel structure. 

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