Method performance terms

Biopolymers are employed in many immunological techniques, including the analysis of food, clinical samples, pesticides, and in other areas of analytical chemistry. Immunoassays (qv) are specific, sensitive, relatively easy to perform, and usually inexpensive. For repetitive analyses, immunoassays compare very favorably with many conventional methods in terms of both sensitivity and limits of detection. 

PLC is used for separations of 2 to 5 mg of sample on thin-layer chromatography (TLC) plates (0.25-nun layer thickness) or high-performance TLC (HPTLC) plates (0.1-mm thickness). In these instances, the method is termed micropreparative TLC. The isolation of one to five compounds in amounts ranging from 5 to 1000 mg is carried out on thicker layers. PLC is performed for isolation of compounds to be used in other tasks, i.e., further identification by various analytical methods, such as ultraviolet (UV) solution spectrometry [1] or gas chromatography/mass spectrometry (GC/MS) [2], obtaining analytical standards, or investigations of chemical or biological properties [3]. 

In addition to the requirements regarding traceability of measurement results, the measurement methods employed should represent "state-of-the-art in the particular field. Failing to do so would lead to a reference material with an uncertainty that has become too large to serve as a quality control. The better the methods perform in terms of uncertainty and traceability, the better the reference material will serve the interests of the (potential) users. 

Insufficient testing is one of the major causes of method failure. The amount of data needed to publish a new procedure in a peer-reviewed journal and the procedural detail supplied therein are often insufficient to allow a different user to validate a method rapidly. The developer should evaluate if the method will work using chemicals, reagents, solid-phase extraction columns, analytical columns, and equipment from various vendors. Separate lots of specific supplies within a vendor should be evaluated to determine if lot-to-lot variation significantly impacts method performance. Sufficient numbers of samples should be assayed to estimate the lifetime of the analytical column and to determine the effects of long-term use on the equipment. 

Repeatability is a measure of the short-term variation in measurement results and is the precision that can be most easily determined. It is often used to establish compliance with method performance criteria. While repeatability is a... 

The complexity of the method in terms of number of steps and solvents needed depends on the sorbent chemistry. The development in a simplified scenario involves running an analyte in several concentrations in multiple replicates and assaying for recovery and performance. This procedure is described in detail for several silica and polymeric sorbents by Wells.42 However, if a number of sorbents are to be evaluated, the process becomes time-consuming if multiple 96-well plates (each with one sorbent packed in all the wells) must be screened separately. This process may take a week or more and consume an analyst s precious time as well. The most plausible solution is to pack different sorbents in the same well plate and use a universal procedure that applies to all of them. An example of such a multisorbent method development plate is the four-sorbent plate recently introduced by Phenomenex demonstrated124 to require only 1 to 2 hr to determine optimal sorbent and SPE conditions. 

In order that the soHds robotic system could be vaHdated fully, each separate step or component of the procedure was isolated and the results verified gravimetrically. The vahdated results showed that the TS, TSS, and TDS-ROE robotic methods performed excellently in terms of precision, accuracy, and method detection Hmit (MDL). These results were found to be equivalent to, or better than, results obtained by manual... 

To improve the method performance, notably precision, in these circumstances. The advances made have been commonly termed automation . 

The literature gives a wide range of practical guidelines for the evaluation of method performance characteristics [58]. Besides the diversity of approaches, also the terminology and way of reporting results vary widely. Differences may occur depending on the purpose and the application field of the method, and validation studies may become more difficult as the complexity of the analysis increases [86]. In what follows, terms and formulas are taken from the accepted IUPAC nomenclature for the presentation of results of chemical analysis [66]. For each validation parameter, definitions, ways of expression, determination guidehnes, and acceptance criteria are reported in Table 5. 

Measure of capacity of analytical procedure to remain unaffected by small but deliberate variations in method performance parameters, which provides an indication of its reliability during normal usage (term used by USP/ICH only)... 

Use of Standardized Methods The first level of AQA is the use of validated or standardized methods. The terms validated and standardized here refer to the fact that the method performance characteristics have been evaluated and have proven to meet certain requirements. At least, precision data are documented, giving an idea of the uncertainty and thus of the error of the analytical result. In both validated and standardized methods, the performance of the method is known. 

Solgel processing specifies a type of solid material synthesis method performed in a liquid and at low temperatures [152], The produced inorganic solids, mostly oxides or hydroxides, are formed by chemical transformation of chemical solutes termed precursors. The solid is formed as the result of a polymerization process that involves the establishment of M-OH-M or M-O-M bridges between the metallic atoms M of the precursor molecules [152], The drying process, after the gel formation, is carried out at a relatively low temperature to produce a xerogel, or by a supercritical drying process. 

The column and planar configurations just discussed are the most common modes of LC but not the only ones. At least four different methods have been proposed for performing LC without a solid support, and two have survived as viable methods. The term countercurrent chromatography is applied to these techniques, and a review of their development has been written by Ito and Conway.6 Countercurrent chromatography will not be discussed further here, but it should be noted that it has one main advantage it is free from undesirable adsorption and catalytic effects that sometimes result from the use of solid supports. 

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