AOAC-IUPAC

Analysts in industry prefer in many cases to maintain consistent methods for their analyses. Recommended ASTM analytical procedures are quite well developed in the rubber and polymer industry. As an example, we mention the standard test method for determination of phenolic antioxidants and erucamide slip additives in LDPE using liquid chromatography [76]. However, the current industry standard test methods (ASTM, AOAC, IUPAC, etc.) use a large number of solvents in vast... 

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... 

K Larsson, T Moller. Liquid chromatographic determination of ochratoxin A in barley, wheat bran, and rye by the AOAC/IUPAC/NMKL method NMKL collaborative study. J AOAC Int 79 1102— 1105, 1996. 

Another area where IAP is found to be beneficial is in the testing of afiatoxins. The development of Aflatest using IAP enrichment has allowed sample testing in minutes with limited laboratory facilities and without need for hazardous aflatoxin standards (135). An AOAC/IUPAC collaborative study was conducted to evaluate the effectiveness of the immunoaffinity column (Aflatest) for determination of aflatoxin. The method has been given official first action by the AOAC (128). 

For most regulatory applications, the method chosen will have been subjected to preliminary method development studies and a collaborative study, both carried out according to standard protocols. This process, and subsequent acceptance, forms the validation of the method. For example, the AOAC/IUPAC protocol [5, 6] provides guidelines for both method development and collaborative study. Typically, method development forms an iterative process of performance evaluation and refinement, using increasingly powerful tests as development progresses, and culminating in collaborative study. On the basis of the results of these studies,... 

The AOAC/IUPAC protocol recommends that steps 2,3 and 4 be carried out within a single laboratory, to optimise the method, before starting the collaborative trial. Tables 1 and 2 give a comparison of this part of the protocol [6] with an extract from corresponding parts of the EURACHEM Guide [3], The two procedures are very similar. Section 1.3.2 of the method vali-... 

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). 

In the common vernacular, the terms specificity and selectivity are often interchangeably used. More properly, a method is said to be specific if it provides a response for only a single analyte, while the term selective means that the method provides responses for a number of chemical entities that may be distinguished from each other. Selectivity also implies the ability to separate the analyte from degradation products, metabolites, and coadministrated drugs [12]. USP 28 [1] defines specificity as the ability to assess the analyte unequivocally in the presence of other components such as impurities, degradation products, and the matrix. IUPAC and AOAC have preferred the use of the term selectivity than specificity for methods that are completely selective, while USP, ICH, and FDA used the term specificity . Due to the very number of limited methods that respond to only one analyte, the term selectivity is usually more suitable, and this usage will be used in this work. 

ISO, IUPAC and AOAC INTERNATIONAL have co-operated to produce agreed protocols on the Design, Conduct and Interpretation of Collaborative Studies 14 and on the Proficiency Testing of [Chemical] Analytical Laboratories .11 The Working Group that produced these protocols has prepared a further protocol on the internal quality control of data produced in analytical laboratories. The document was finalised in 1994 and published in 1995 as the Harmonised Guidelines For Internal Quality Control In Analytical Chemistry Laboratories .12 The use of the procedures outlined in the Protocol should aid compliance with the accreditation requirements specified above. 

ISO/IUPAC/AOAC International Harmonised Protocol For Proficiency Testing of (Chemical) Analytical Laboratories... 

Precision is defined as the closeness of agreement between independent test results obtained under prescribed conditions.19 In a standard method the precision characteristics are obtained from a properly organised collaborative trial, i.e. a trial conforming to the requirements of an International Standard (the AOAC/ISO/IUPAC Harmonised Protocol or the ISO 5725 Standard). Because of the importance of collaborative trials, and the resource that is now being devoted to the assessment of precision characteristics of analytical methods before their acceptance, they are described in detail below. 

On the international level, relevant standards are available from the IUPAC, ISO, and AOAC International [4, 8,16,17] and from the Codex Alimentarius working group CCMAS [18-21]. Other helping guides have been published by the EAL [22] and ILAC [23] (see Table 1 for explanation of abbreviations). 

IUPAC, ISO, and AOAC International International Union of Pure and Applied Chemistry, International Organisation for Standardization, and Association of Official Analytical Chemists MU 4,8,16,17... 

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]. 

Use a top-down approach using reproducibility and repeatability standard deviations from an interlaboratory study by the Harmonized IUPAC/AOAC protocol (Horwitz 1995) or ISO 5725 (ISO 1994). 

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. 

The IUPAC Commission on Oils, Fats and Derivatives undertook the development of a method and collaborative study for the determination of triglycerides in vegetable oils by liquid chromatography. Three collaborative studies were conducted from 1985 to 1987. Refinements were made in the method after the first collaborative study, and the second and third collaborative studies demonstrated that the method produces acceptable results. Materials studied were soybean oil, almond oil, sunflower oil, olive oil, rapeseed oil, and blends of palm and sunflower oils and almond and sunflower oils. Six test samples were analyzed by 18 laboratories from 11 countries in the second study 4 test samples were analyzed by 16 laboratories from 12 countries in the third study. The method for the determination of triglycerides (by partition numbers) in vegetable oils by liquid chromatography was the first action adopted by AOAC INTERNATIONAL as an IUPAC-AOC-AOAC method (103). 

The International Standardising Organisations, AOAC, ISO and IUPAC, have co-operated to produce an agreed International Harmonised Protocol For... 

Recently there has been progress towards a universal acceptance of collaboratively tested methods and collaborative trial results and methods, no matter by whom these trials are organised. This has been aided by the publication of the IUPAC/ISO/AOAC Harmonisation Protocol on Collaborative Studies.14 That Protocol was developed under the auspices of the International Union of Pure and Applied Chemists (IUPAC) aided by representatives from the major organisations interested in conducting collaborative studies. In particular, from the food sector, the AO AC International, the International Organisation for Standardisation (ISO), the International Dairy Federation (IDF), the Collaborative International Analytical Council for Pesticides (CIPAC), the Nordic Analytical Committee (NMKL), the Codex Committee on Methods of... 

As for all other analytical methods, methods for the analysis of products derived from modern biotechnology need to be validated. This validation should follow international standards (e.g. ISO 5725) and comply with, The IUPAC/AOAC/ISO harmonized protocol of method validation [6] or the standards cited above. Validation of testing methods is greatly facilitated by the use and availability of the appropriate reference materials. The following paragraphs specify some important... 

Harmonised guidelines for the use of recovery information in analytical measurement, IUPAC, ISO, AOAC, EURACHEM, Technical Report (1998) Marschal A., Andrieux, Compagon P.A., Fabre H. (2002) Accred Qual Assur 7 42-49... 

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