Validation single-laboratory

EPA. 1987d. Project summary Single laboratory validation of EPA method 8140. Las Vegas, NV U.S. Environmental Protection Agency. EPA 600/S4-87-009. 

Table 8 Summary of CSL parameters and criteria for single-laboratory validation of procedures involved in a quantitative method ... 

Because of the small number of laboratories involved, validation of UK methods by inter-laboratory study has become impractical in most cases. Even where it is practical, it is usually impossible to validate all pesticide-matrix combinations. Moreover, single-laboratory validation data will have to be generated. Therefore, the CSL guidelines are one of the first that strictly focus on requirements of single-laboratory validation. Some examples of minimum requirements are given in Table 8. Additionally, these guidelines emphasize some other important aspects of validation and contain some new ideas. 

AOAC/FAO/IAEA/IUPAC Expert Consultation, Guidelines for Single Laboratory Validation of Analytical Methods for Trace-level Concentrations of Organic Chemicals, Workshop, 8-11 November 1999, Miskolc, Hungary (1999). Also available on the Word Wide Web http //www.iaea.oi trc/(see pesticides —> method validation). 

Yu R, Brown PN (2008) Single laboratory validation study for the determination of ginsenoside content in Panax ginseng C.A. Meyer and P. quinquefoUus L. Raw Materials and finished Products by High Pressure Liquid Chromatography. 5th Annual NHP Research Conference Toronto Ontario, March 27-29, 2008... 

Use of Validated Methods In-Home Versus Interlaboratory Validation Wherever possible or practically achievable, a laboratory should use methods which have been fully validated through a collaborative trial, also called interlaboratory study or method performance study. Validation in collaborative studies is required for any new analytical method before it can be published as a standard method (see below). However, single-laboratory validation is a valuable source of data usable to demonstrate the fitness for purpose of an analytical method. In-house validation is of particular interest in cases where it is inconvenient or impossible for a laboratory to enter into or to organize itself a collaborative study [4,5]. 

On the one hand, even if an in-house vahdated method shows good performance and reliable accuracy, such a method cannot be adopted as a standard method. In-house validated methods need to be compared between at least eight laboratories in a collaborative trial. On the other hand, a collaborative study should not be conducted with an unoptimized method [58]. Interlaboratory studies are restricted to precision and trueness while other important performance characteristics such as specificity and LOD are not addressed [105]. For these reasons, single-laboratory validation and interlaboratory validation studies do not exclude each other but must be seen as two necessary and complementary stages in a process, presented in Figure... 

The added value of single-laboratory validation is that it simplifies the next step—interlaboratory validation—and thereby minimizes the gap between internally (validated or not) developed methods and the status of interlaboratory validation. By optimizing the method first within the laboratory, as a kind of preliminary work, an enormous amount of collaborators time and money is saved [58]. 

Thompson, M, Ellison, S, and Wood, R (2002), Harmonized guidelines for single laboratory validation of methods of analysis. Pure and Applied Chemistry, 74, 835-55. 

Thomson M, Ellison SLR, Wood R (2002) International union of pure and applied chemistry, harmonized guidelines for single laboratory validation of method of analysis. Pure Appl Chem74 835-855. http //www.iupac.org/objID/Article/pac7405x0835... 

The ISO 17025 requires that every method is validated to demonstrate fitness for purpose [1]. Analytical methods can be validated during a collaborative trial or in a single laboratory validation experiment. Single laboratory method validation has become common practice for every analytical chemist. Several guidance documents have been published concerning the validation of analytical methods [2, 3]. Methods used for the official control of foodstuffs are validated according to the European decision EC 2002/657 [4]. 

By preference, an RM is analyzed under reproducibility conditions. Since the reproducibility standard deviation is not known in a single laboratory validation... 

Ji, D. et al. Determination of chondroitin sulfate content in raw materials and dietary supplements by high-performance liquid chromatography with ultraviolet detection after enzymatic hydrolysis single-laboratory validation. J. AOAC Int. 2007, 90, 659-669. 

Other methods used in the context of official controls such as those used for in-house control purposes may be single laboratory validated according to internationally accepted protocols (e.g. lUPAC harmonised guidelines). General criteria for the characterisation of methods of analysis exist. 

Codex (2002) Codex committee on methods of analysis and sampling. In-house method validation (document CX/MAS 01/9). See also Codex committee on methods of analysis and sampling. Consideration of IUPAC guidelines for the in-house (single laboratory) validation of methods of analysis (document CX/MAS 02/10). 

This relationship is widely used to predict a reasonable relative standard deviation for a given analyte concentration within a laboratory. AOAC (2003a) guidelines for single-laboratory validation of chemical methods also provide guidelines for acceptable recovery values, as shown in Table 4. Thus, armed with these guidelines it is possible to discern whether the experimental recovery rate, as well as the prcci.sioii of the method, is within acceptable boundaries. 

Association of Analytical Communities (2003b). Guidelines for Single Laboratory Validation of Chemical Methods for Dietary Supplements and Brdanicals. AOAC International, Gaithersburg, MD. 

McNabb, R, Selwood, A.L, and Holland, P.T., A mnltiresidne LC-MS method for algal toxins in shellfish Single-laboratory validation and interlaboratory stndy. J. AOAC Int., 88, 761, 2005. 

Anon, Guidelines for single laboratory validation of chemical methods for dietary supplements and botanicals, AOAC International, Gaithersburg MD, 2002, p. 38. 

McNabb, P. et al.. Multiresidue method for determination of algal toxins in shellfish single-laboratory validation and interlaboratory study, J AOAC Int 88, 761, 2005. 

STX is now distributed worldwide by IAEA and is being used in collaborative trials of the PSTs receptor binding assay (RBA). Single laboratory validation of the RBA using new radiolabeled saxitoxins were presented at the Marine and Freshwater Toxins Analysis First Joint Symposium and AO AC Task Force Meeting in Baiona, Spain, in April 2005. The limit of quantitation of the microplate format assay " was found to be 1.2 pg STX equivalent/100 g shellfish (regulatory limit 80 pg/100 g), with an overall repeatability of 17.7% for shellfish extracts run by one analyst on 5 independent days, and a correlation r =. 98 with the mouse bioassay. 

One other issue, also linked to the lack of standards, is the need of internationally validated methods. Several approaches can be used to validate a method, but the single-laboratory validation... 

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