Standards validation with

On basis of systematie use of the prineiple of insignifieanee, aeeeptanee eriteria system of validation eharaeteristies was developed and standardized validation plan of pharmaeeutieal analysis proeedures was proposed, the latter plan found an applieation in the establishing of NSRS and PPT establishing. Have been developed and issued two editions of the SPU, whieh is harmonized with European Pharmaeopoeia and now is a sole national pharmaeopoeia in CIS. 

A system suitability test prescribes a relative standard deviation of not more than 1% for the procedure to be valid with Xmean = 173.5 this translates into Vr - (1.735)2 because the limit is imposed, this is equivalent to having no uncertainty about the numerical value, or in other words,/r = Since Si was determined to be 2.43 for n, = 1 ... 

Thanks to the efforts of a continuously increasing number of research groups, CE has by now been accepted as a highly efficient separation technique for qualitative purposes, with about 1500 CE-related documents appearing annually in analytical journals. However, CE has not yet been fully established as a quantification method, mainly due to the predominance of HPLC techniques applied in standard, validated analytical protocols. 

The problem has now been solved, and it is possible to measure the phase angle of the probe as the cells pass through the laser beam.09,40) While these measurements have not yet been applied to Ca2+, the method has been validated with standard beads and stained cells. In our opinion, this new flow cytometry parameter, and our increasing knowledge of lifetimes of probes, will result in the increased use of flow cytometry for studies of intracellular physiology, in addition to the current emphasis in immunology, cell activation, and ploidy. 

Monitoring the MMA/DMAAm reaction is challenging becanse both monomers have very similar NIR spectra, and because other interfering snbstances are present in the reaction mixtnre. The anthors prepared calibration samples gravimetrically and made the NIR measurements at reaction temperatnres. The calibration sets consisted of only five or six samples, which is considerably fewer than standard recommendations for NIR chemometric model development. The final models for MMA and DMAAm were validated with an internal validation set as well as an external reaction validation. The performance of the models is summarized in Table 15.6. This table inclndes a measurement of the standard deviation of an external GC method... 

For reliable quantification, the deuterium-labelled substrate (ds-phenylethyl-amine) was added to the matrix as internal standard. To circumvent the problem of crystal inhomogenities, 100 acceptable spectra were measured from seven to ten different positions of one sample spot and averaged. The MALDI-MS assay was validated with a gas chromatography-based quantification scheme and was found to be in good compliance. This methodology obviously allows a reliable quantification of the low molecular weight analytes of interest. Nevertheless, the need for isotopically labelled compounds as internal standards is still a bottleneck, as these are usually rather expensive or have to be laboriously synthesized. 

Nevertheless, the calculated standard potential given in Eq. (2) remains valid with a good precision. When pH value is higher than 12, the solubility of silicate ion grows rapidly and then corrosion process... 

Initial validation each stopper type should be tested once prior to and once after mnning the standard process with a loading of 100%. Revalidation once every 3 years... 

Cross-Validation. Cross-validation is a comparison of validation parameters when two or more bioanalytical methods are used to generate data within the same study or across different studies. An example of cross-validation would be a situation where an original validated bioanalytical method serves as the reference and the revised bioanalytical method is the comparator. The comparisons should be done both ways. When sample analyses within a single study are conducted at more than one site or more than one laboratory, cross-validation with spiked matrix standards and subject samples should be conducted at each site or laboratory... 

Analytical methods validation—As mentioned earlier, a good CVMP should allow the analytical method to develop concurrently with the product formulation, thus in the early stages of development, an analytical method may not be fully validated but may still be used for cleaning tests as the best available method. At the time of the PAI, however, and definitely by the time the formal cleaning validation occurs, a fully validated analytical method should be developed. This methods validation package should include all the standard parameters, with special attention to the sensitivity of the analytical method as expressed by the limit of detection (LOD) and... 

Other standardized/validated test methods reported in the literature include acute/chronic tests performed with algae (e.g, OECD, 2002a ISO, 2003), fish cells (Gagne and Blaise, 2001), invertebrates (Borgmann and Munawar, 1989 Trottier et al., 1997 Pereira et ah, 2000 OECD, 2001 a,b), Lemnaceae (OECD, 2002b), and with toxicity tests conducted at different trophic levels (Nebeker et ah, 1984 U.S. EPA, 2002a,b). 

Procedures—An underutilized practice in validation is the SOP, whereby repetitive activities can be defined. The use of SOPs increases reproducibility of execution and allows for further brevity in both protocols and reports. Procedures make everyone who is involved with the project substantially more efficient, and should be employed wherever possible. Practices such as calibration of instrumentation, biological indicator placement, sampling of validation batches, and microbial testing are clear candidates for inclusion in SOPs. Among the more innovative uses is the inclusion of standardized validation acceptance criteria for similar products. 

Standardized methods for surveillance of antifungal drug susceptibility have been a recent development (Rex et al, 1993). The M27 protocol of the National Committee for Clinical Laboratory Standards (NCCLS) for testing of yeasts focused on laboratory to laboratory reproducibility and became an approved standard in 1997 (National Committee for Clinical Laboratory Standards, 1997). A modification of M27 for testing of molds has recently been proposed as NCCLS document M38-P (National Committee for Clinical Laboratory Standards, 1998). With these tools, collaborative studies to validate the predictive power of these results have been possible. Interpretive breakpoints for... 

Most of the instrumental direct methods, which are employed in routine analyses, are highly matrix-dependent, therefore methods must be validated with certified standard reference materials. Standard plant reference materials (SRMs), with certified elemental contents can be obtained from NIST, National Institute of Standards and Technology of the United States Department of Commerce or from BCR, Community Bureau of Reference, Commission of the European Community (Colinet et al., 1982 Criepink, 1990 Horwitz and Albert, 1991). 

Toxic potency values are most often assessed from the most suitable small-scale smoke toxicity test (NIST radiant test, using rats as the animal model, but only for confirmatory purposes, standardized in ASTM E 1678192 and NFPA 269193). The results from this test have been well validated with regard to toxicity in full-scale fires. However, such validation cannot be done to a better approximation than a factor of 3. This is illustrated by the fact that the range of the toxic potency of the smoke of almost all materials is so small that it pales in comparison with the ranges of toxic potencies of... 

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