Analytical methods Union

Assessment of residue analytical methods for crops, food, feed, and environmental samples the approach of the European Union... 

Validation of analytical methods for post-registration control and monitoring purposes in the European Union... 

Until 1991, manufacturers seeking authorizations for pesticides had to fulfil country-specific requirements of validation of enforcement methods. The term enforcement method means analytical methods which are developed for post-registration control and monitoring purposes. The harmonization of these requirements was initiated with the European Economic Community (EEC) Council Directive 91/414/EEC and temporarily finalized with the Guidance Document on Residue Analytical Methods SANCO/825/00 rev. 6, dated 20 June 2000 [Santd et Protection des Consommateurs (SANCO)]. The evaluation of validation studies by the competent authority is conducted by comparison of these European Union (EU) requirements with the study results and most often without any practical experience of the method. Some details of this evaluation are discussed below. 

Water for injection (WFI) is the most widely used solvent for parenteral preparations. The USP requirements for WFI and purified water have been recently updated to replace the traditional wet and colorimetric analytical methods with the more modern and cost-effective methods of conductivity and total organic carbon. Water for injection must be prepared and stored in a manner to ensure purity and freedom from pyrogens. The most common means of obtaining WFI is by the distillation of deionized water. This is the only method of preparation permitted by the European Pharmacopoeia (EP). In contrast, the USP and the Japanese Pharmacopeias also permit reverse osmosis to be used. The USP has also recently broadened its definition of source water to include not only the U.S. Environmental Protection Agency National Primary Drinking Water Standards, but also comparable regulations of the European Union or Japan. 

Seven laboratories participated in the interlaboratory evaluation within the framework of the PRISTINE, SANDRINE and INEXsPORT European Union Projects [6]. The results obtained for the analysis of diverse classes of surfactants by different analytical methods are listed in Table 4.5.1. The analytical strategies were based on LC coupled to either MS or FL detection in all cases with the exception of one laboratory using a test tube ELISA kit. Samples were spiked with the surfactants NPEO, CDEA, LAS, AEO, NPEO-SO4 and SAS. 

Consideration of the above requirements confirms that in future all methods must be fully validated if at all possible, i.e. have been subjected to a collaborative trial conforming to an internationally recognised protocol. In addition this, as described above, is now a legislative requirement in the food sector of the European Union. The concept of the valid analytical method in the food sector, and its requirements, is described below. 

Table 5.2 Summary of selected analytical methods for molecular environmental geochemistry. AAS Atomic absorption spectroscopy AFM Atomic force microscopy (also known as SFM) CT Computerized tomography EDS Energy dispersive spectrometry. EELS Electron energy loss spectroscopy EM Electron microscopy EPR Electron paramagnetic resonance (also known as ESR) ESR Electron spin resonance (also known as EPR) EXAFS Extended X-ray absorption fine structure FUR Fourier transform infrared FIR-TEM Fligh-resolution transmission electron microscopy ICP-AES Inductively-coupled plasma atomic emission spectrometry ICP-MS Inductively-coupled plasma mass spectrometry. Reproduced by permission of American Geophysical Union. O Day PA (1999) Molecular environmental geochemistry. Rev Geophysics 37 249-274. Copyright 1999 American Geophysical Union...

Table 26.1 Classification of Analytical Methods in the European Union According to their Validation Status...

Quality criteria for quantitative analytical methods, in general, have been proposed or arc lo be proposed by several international organizations including the Association of Official Analytical Chemists, the Food and Drug Administration, the Codex Committee for Residues of Veterinary Drugs in Food, the International Dairy Federation, and the European Union. The European Union, in particular, has laid down minimum quality criteria for quantitative drug residue methods,... 

Apart from the European Union quality criteria, uncertainty factors may be used for defining the reliability of a qualitative method. The European Union criteria lay down standards that have to be fulfilled only in the detection step of the method (18). However, every method is a combination of many analytical steps, including sample extraction, sample cleanup, and detection. Uncertainty factors simply represent qualitative values for the remaining uncertainty after use of a well-defined analytical method (25). 

Even using uncertainty factors, the problem of determining the reliability of qualitative methods has not be solved because the usual statistical approaches are often not applicable. In residue analysis, this problem is often amplified because concenftations frequently are in the low or even sub-ppb range. Most promising appears to be a model that helps in estimating, in arbitrary units, the overall selectivity of an analytical method on the basis of partial selectivity indices. Selectivity indices are nothing more than a combination of the above-mentioned tools with the experience obtained within the European Union from recognized laboratory experts (26). 

Although there are only a limited number of methods that have been validated specifically for soft drinks, there are around 80 validated methods available for the analysis of fruit juices, most of which would work equally well for soft drinks. These methods are published in the International Fruit Juice Union (IFU) handbook of analytical procedures, which offers the best reference collection of methods for the analysis of fruit juices in the world, with new methods added on a regular basis (Anon, 2004a). The IFU s collection of analytical methods covers most of the main procedures required to assess the quality and authenticity of fruit juices and nectars. The methods are hsted on the IFU s website (http //www.ifu-fruitjuice.com) at the time of writing they cannot be purchased directly from there, but they can be obtained from the Swiss Fruit Union, Zug, and details of how to do this are given on the website. It is possible that at some time the methods will be made available directly from the website. 

Anon (1985) Determination of glucose and fructose enzymatic No. 55, in International Federation of Fruit Juice Producers (IFU) Handbook of Analytical Methods, Swiss Fruit Juice Union, Zug, Switzerland. 

Anon (2004a) IFU Compendium of Analytical Methods for Fruit Juices and Nectars, Swiss Fiuit Juice Union, Zug, Switzerland. 

Under the auspices of the International Union of Pure and Applied Chemistry, an Analytical Methods Committee carried out a critical examination of some primary standards suggested for use in acid-base titrations, with a view to making recommendations concerning practical applications. Some of the findings of this committee were as follows (1) Benzoic acid as a primary standard is not recommended because... 

---