Validation AOAC International

Established in 1894, AOAC International is an independent association of scientists and organizations in the public and private sectors devoted to promoting methods validation and quality measurements in the analytical sciences. AOAC has a mission to ensure the development, testing, validation, and publication of reliable chemical and biological methods of analysis for foods, drugs, feed-stuffs, fertilizers, pesticides, water, forensic materials and other substances affecting public health and safety and the environment. 

BERM-5 presented the changing outlook of the AOAC International in recognizing the usefulness of incorporating RMs for use in conjunction with their methods validation protocol. 

Many of the more established techniques have been validated through collaborative studies which becomes of greater importance as laboratories seek to become accredited via ISO, EN or related systems where the use of official or well validated methods is mandatory. New instrumental techniques are constantly being reported in the literature but it often requires many years before procedures are introduced, validated and then applied within the food industry. Recent techniques that can be included in this category are capillary electrophoresis and liquid chromatography-mass spectrometry (LC-MS). In time procedures based on these techniques will also become accepted as routine methods and are likely to be adopted by some of the official international bodies like the AOAC International, CEN, ISO, etc. 

On the international level, we distinguish IUPAC, ISO, and the AOAC International. All three bodies develop validation and standardization frameworks for analytical chemistry. AOAC International introduced the AOAC Peer Verified Methods Program [62]. Different harmonized guidelines and protocols are developed by the IUPAC, ISO, and AOAC International together [4,8,63-67], in addition to a number of ISO standards [68-71]. The FDA, USP, and ICH developed guidelines specific for pharmaceutical and biotechnological methods [55,72-74]. 

IUPAC, ISO, and AOAC International International Union of Pure and Applied Chemistry, International Organisation for Standardization, Association of Official Chemists Method validation, Standardization, internal quality control, proficiency testing, accreditation 4,8, 62-71... 

Association of Official Analytical Chemists (AOAC) International (2000), Method validation programs (OMA/PVM Department), including Appendix D Guidelines for collaborative study procedures to validate characteristics of a method of analysis, available http //www.aoac.org/vmeth/devmethno.htm. 

In recent years the term qualimetrics has been coined to refer to the use of chemometrics for the purposes of quality control (Massart et al. 1997). ft relates particularly to the use of multivariate analysis of process control measurements. Other texts on quality assurance in chemical laboratories include the latest edition of Garfield s book published by AOAC International (Garfield et al. 2000), material published through the Valid Analytical Measurement program by the LGC (Prichard 1995), and books from the Royal Society of Chemistry (Parkany 1993,1995 Sargent and MacKay 1995). Wenclawiak et al. (2004) have edited a series of Microsoft PowerPoint presentations on aspects of quality assurance. 

The ideal validated method would be the one that has progressed fully through a collaborative study in accordance with international protocols for the design, conduct, and interpretation of method performance studies. A typical study of a determinative method conducted in accordance with the internationally harmonized International Organization for Standardization (ISO)/International Union for Pure and Applied Chemistry (IUPAC)/AOAC International (AOAC) protocol would require a minimum of up to five test materials including blind replicates or split-level samples to assess within-laboratory repeatability parameters, and eight participating laboratories (15). Included with the intended use should be recommended performance criteria for accuracy, precision and recovery. 

In cases in which tliis less stringent model cannot be used, alternative validation schemes may be used (17). These include a two-laboratory validation protocol similar to the AOAC International Peer Verified Method Protocol, or a singlelaboratory validation approach. With any of tlie alternative validation schemes, the Joint FAO/IAEA Expert Consultation on Validation of Analytical Methods... 

Reina, R.J., White, K.D. and Jahngen, E.G.E. (1997) Validated method for quantitation and identification of 4,4-desmethylsterols and triterpene diols in plant oils by thin-layer chromatography-high resolution gas chromatography-mass spectrometry. J. AOAC Intern., 80(6), 1272-1280. 

Due to the demand for reliable and comparable methods, performance requirements have been established at a national and international level for implementation of official methods, e.g. by European legislation, by the CEN or the Association of the Analytical Communities (AOAC) International, and worldwide by Codex Alimen-tarius (CAC). Thus any method proposed to be used for official purposes must be validated in a collaborative trial study, resulting in defined method performance characteristics [4], The framework for the design and conduct of such collaborative trial studies, as well as the statistical evaluation, are also defined in appropriate protocols [5]. Any method that has been successfully validated according to these protocols can be recognised as an official method for use in legal cases or for international trade control purposes. 

Food methods validated by a collaborative trial study and those validated using the single-laboratory approach have been adopted as national and international standards by, e.g. CEN, International Organisation for Standardisation (ISO), AOAC International and by the Joint FAO/WHO Codex Alimentarius Food Standards Programme. A number of EN Standards developed by CEN relate to the organisation of controls. It is however important to keep in mind that, in addition to the method performance criteria, economical and prevention strategy... 

Since its beginning in 1884, AOAC INTERNATIONAL has been truly dedicated to the validation of analytical methods through trials in multiple laboratories. An early undertaking of AOAC is still its most important business supporting the use of analytical methods used in multiple laboratories through validation by interlaboratory studies. 

Three method validation systems are operated by AOAC INTERNATIONAL ... 

At present, a special Task Force in AOAC INTERNATIONAL is studying the integration of the three methods validation systems. The reason for doing this is the increasing number of proprietary... 

AOAC, 1999. Qualitative and Quantitative Microbiology Guidelines for Methods Validation, Journal of AOAC International, 82(2). 

During the past 15 years, there has been a consolidation of vendors producing these test kits. Currently, there is only one vendor, Strategic Diagnostics, These kits are available for several OPs and CMs. Note that none of these kits have been validated to receive the PTM status from AOAC International. 

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

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

For example, a guideline approved in 2009 by the CAC defines a validated method as an accepted test method for which validation smdies have been completed to determine the accuracy and reliability of this method for a specific purpose, referencing a definition provided by the Interagency Coordinating Committee on the Validation of Alternative Methods (ICCVAM). This definition is similar in content to definitions used by Eurachem, AOAC International, the International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use (ICH), " and the VICH.19... 

Continued progress on the development of improved sample cleanup techniques with good recoveries has been observed. An example of the application of a new cleanup column was an improvement of a fluorometric test kit that determines AFL in almonds, allowing it to be validated by the AOAC International Research Institute as a Performance Tested certified kit (Romer Labs, 2007). 

Koll K, Reich E, Blatter A, and Veit M (2003) Validation of standardized high-performance thin-layer chromatographic methods for quahty control and stahihty testing of herhals. Journal of AOAC International 86(5) 909-915. 

LaCroix, D.E., Wolf, W.R., and Chase, Jr. G.W., 2002. Determination of niacin in infant formula by solid phase extraction/liquid chromatography peer-verified method performance validation. Journal of AOAC International. 85(3) 654-664. 

Campos-Gimenez, E.C., Trisconi, M-J., Kilinc, T., and Andrieux, P., 2010. Optimization and validation of an LC-FLD method for biotin in infant formula, infant cereals, cocoa-malt beverages and clinical nutrition products. Journal of AOAC International. 93 1494—1502. 

AOAC, Appendix D Guidelines for collaborative study procedures to validate characteristics of a method of analysis. Journal of AOAC International (2002). 

Two types of method validation can be distinguished. Full method validation, of interest to the general scientific community, is carried out through an interlaboratory method performance study. Where a method becomes more routinely used it is reasonable to expect that the method should be fully validated. Internal method validation (single-laboratory method validation) is a scientific and technical alternative. It consists of validation steps carried out within one laboratory, for instance, to validate a new method that has been developed in-house or to verify that a method adopted from some other source is applied sufficiently well. A single-laboratory validation cannot assess between-laboratory variation and will provide an optimistic assessment of interlaboratory variability (cfr. Chp. 6.2.3 and 6.2.4). In-house method validation is described in the lUPAC, AOAC International, and ISO guidance [65,66]. There are several types of internal laboratory validation ... 

Moreover, the international AO AC could constitute another source of official methods. This association develops or evaluates methods for substances or products that could be used by a large number of manufacturers. This group is supervising a validation programme intended to evaluate a method for use in various fields. Although most of these methods are used primarily in the area of foodstuffs, different analytical methods for cosmetics can be found in the official methods of analysis of AOAC International (Horwitz, 2005). The AO AC analytical methods regarding cosmetic products are listed in Table 2.1.12. 

By using the combination of specific method accreditation and generic accreditation it will be possible for laboratories to be accredited for all the analyses of which they are capable and competent to undertake. Method performance validation data demonstrating that the method was fit-for-purpose shall be demonstrated before the test result is released and method performance shall be monitored by on-going quality-control techniques where applicable. It will be necessary for laboratories to be able to demonstrate quality-control procedures to ensure compliance with the EN 45001 Standard,3 an example of which would be compliance with the ISO/AOAC/IUPAC Guidelines on Internal Quality Control in Analytical Chemistry Laboratories.12... 

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