Method Documentation

A system of document control, including restricting unofficial copying, is required, in order to ensure that only authorized methods are used and that these are the latest revisions. This requires attention to details, such as revision number, who authorized the method, who has amended it, issue date, date of next revision, number of copies and who owns them, etc. A variety of documentation formats are available, but a standard format for method documentation is provided in ISO 78-2 1999 and a layout based on this Standard is provided in the Appendix to this chapter [18]. 

The following layout is based on ISO 78-2 [18]. Note that method documentation requires appropriate control (see Section 4.6.6). In addition to the headings described below, each page of the method should be marked with the page number, the total number of pages and the version number. 

Performance evaluations of the reference method Documentation regarding routine QC of reference laboratory methods can be very relevant for model evaluation, if the methods were used to generate reference (y) data for model development. 

There are several methods documented in the literature for the synthesis of gabapentin (1). Satzinger, Hartenstein, Herrmann, and Heldt disclosed the original synthesis in a 1976 Goe-decke A.-G. patent (Satzinger et al., 1976). The key intermediate 1,1-cyclohexanediacetic... 

The Canadian Acceptable Methods document [14] gives more or less a combination of the two definitions described above and considers 3 levels in the testing of the ruggedness of a method, with the third level being performed only rarely. Level one requires verification of the basic insensitivity of the method to minor changes in environmental and operational conditions and should include verification of reproducibility by a second analyst . The first part of this definition resembles the French Guide s definition. The second part is a check on the adequacy of the method description and should be done without input from the original analyst. 

From the definitions given above it can be seen that there are two approaches to ruggedness testing (also equal to levels 1 and 2 given in the Acceptable Methods document [14]). In the first approach factors to be examined are selected from the set of operating and environmental conditions that are or could be stipulated in the analytical procedure. This kind of factors can be called procedure related factors. 

The study is performed according to a plan approved (by dated signature) by the study director and verified for CLP compliance by the QA unit. Some countries also require formal approval by the test facility management and the sponsor. The plan should usually contain identification of the study, the test item and reference item, information concerning the sponsor and the test facility, dates, test methods, documents and materials to be retained, and other issues that have been identified. 

The Analytical Methods Committee s own compilation of official and standardised methods of analysis is widely used and respected within the analytical community. The importance of standardised formats for method documentation has been emphasised by the AMC s guidelines for achieving quality in trace analysis. They list 17 headings for inclusion in the documentation ... 

Let us examine what a protocol should accomplish. During an inspection of a given product or process, FDA will more times than not conduct a review of the process validation protocol. As mentioned earlier, the process entails everything used to manufacture the transdermal—procedures, personnel, methods, documents, and so on. Given the fact that the protocol will likely fall under FDA scrutiny at some point and that other documents used to complete the validation may as well, it should be easy to understand that the process validation protocol should be used to reference as many of these other supporting documents as possible. 

Full validation of a standard method is recommended where no information on type and results of validation can be found in the standard method documentation. 

If toxicity tests fulfill the scientific criteria set out by inter-calibration exercises, they can then be considered for the standardization process. If this process is followed, an official toxicity test method document is eventually produced that ensures proper conduct of biological tests (see Section 3.2.1). 

Test method standardization (TMS) calls for several actions that involve 1) preparation of a formal draft test method document for each bioassay intended for standardization, 2) a critical review by an expert subcommittee, 3) the preparation of a final draft test method, 4) an international peer review of each test method, 5) an inter-calibration exercise of the final draft test method, 6) finalization of each test method and 7) the formal publication of the toxicity test method document. Environment Canada (EC) has been particularly active in biological test method standardization and has thus far contributed 18 standardized aquatic and sediment... 

One final point, which needs emphasis, is that at the time of writing the methods documented are the most up to date in current use. However, judging by past experience, it is likely that these will be further improved and amended as sequencing objectives become more ambitious and complex. 

Analytical method the complete process used to determine an analyte or analytes in a sample. The analytical method documents all the individual steps in the process from sampling to reporting the results. 

Either method can be used as long as the operator does it consistently. Do not prepare mobile phases one way once and another way the second time. Also do not weigh one solvent and measure another volumetrically. If one method is used and results in too much variability in the chromatography, try the other method. The important point is to use one method, document it, and be consistent. 

The job is not complete until another chemist can independently run your method. I have transferred many methods over the years. Despite the use of comprehensive method documentation, problems often occur during start-up in a new laboratory, particularly when chemists new to CE are involved. These often minor problems are always solved through a dialogue with the operator. Even seemingly minor details can be befuddling. For example, be sure to specify the electrolyte reservoir size in your method. Using too small an electrolyte reservoir can cause precision problems, particularly when multiple runs are performed from a set of electrolytes. 

Calibration schedule Chain of custody Controlled documents Methods documentation Procedure Protocol... 

The criteria and methods document prepared by COT for the development of EEGLs and SPEGLs indicates that theoretical excess carcinogenic risk... 

OECD (1996). Final Report of the OECD Workshop on Harmonization of Validation and Acceptance Criteria for Alternative Toxicological Test Methods. Document ENV/MC/TG(96)9 (http //www. oecd. org/ehs/test/background. htm). 

GLP Federal Register, December 1978 also see Williams and Hottendorf, 1997). These define technical matters such as laboratory methods, documentation, data handling, instrument calibration and much more connected with the actual conduct of toxicology testing at the bench level. 

Because they are primarily growth processes, these applications require reduction in seed crystal size to prevent oversized crystals from limiting the surface area. The methods documented in these examples include sonication and wet milling. 

The method documentation package is typically extensive and should contain the following ... 

TBP curves are not usually determined directly by batch distillation since achieving complete fractionation in the laboratory is impractical. Instead, standardized batch distillation tests are conducted under closely dehned conditions. Several such tests are specihed by the American Society for Testing and Materials, including procedures D86, D1160, and D2887 (ASTM, 1990). These distillation curves are converted to TBP curves using the methods documented by the American Petroleum Institute (API, 1983). 

The endpoint of the first level is a method with complete internal validation for the intended purpose at the level of a single research laboratory. A method meeting the requirements of the second level can successfully be transferred to another laboratory possessing sufficient expertise and experience. Ranking the method at the third level means that the method possesses sufficient interlaboratory performance and is applicable for use at the level of routine laboratories. This also comprises the development and control of key aspects of method documentation and method usability. Having... 

The data of Table 3b have been computed by replacing the active space of the CASPT2 treatment by the CIPSI multireference space of the MRPT2 method documented in section 2.1. The selection of the components of the reference space by this technique enables us to reduce the gap between the Moller-Plesset and Epstein-Nesbet total energies to less than 0.01 a.u., and so to improve our evaluation of energy balances, disregarding a possible overestimation of the Moller-Plesset values due to intruder states, as it is the case in the ScNC system. 

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