Method description

METHOD 4 This is a P2P recipe that Strike has no hand in. Strike never even knew about it until Strike saw everybody talking about it on the net. But it seems to be extremely popular. Shulgin has written about it. Uncle Fester, Strike understands, has written about it. And there seems to be a lot of posts regarding its high success rates. Most people get started from the method description in the patent literature where they were first published. The following are some representative examples from the U.S. Patent 4,638,094 Process for Producing Phenylacetones ... 

Affine deformation method, description, 109 Agitated glass ampule method apparatus, 510,511/312 limitations, 515... 

BAC-MP4 method, description, 344-346 Band theory, crystal orbital method, 149 Be clusters, structures, 24-25 Bifurcation... 

Ktihne, R., Ebert, R-U., Schtitirmann, G. Model selection based on structural similarity - method description and application to water solubility prediction. f Chem. Inf Model. 2006, 46, 636-641. 

In the SMMT process, draft protocols are reviewed, and guidance provided to the sponsor to help ensure that the format and specifications are adequate. The protocol should be approved by CVM prior to the initiation of the method trial. Once the protocol and method description are acceptable to CVM, the methods are sent to the participating laboratories for review, and a method demonstration is scheduled. The method demonstration, attended by all participating laboratory analysts, involves review of the study protocol and method SOP and a laboratory demonstration of the method. Ideally, all revisions are completed by the end of the demonstration and the study protocol is signed. 

A standard format for the presentation of analytical methods is not obligatory. However, each study should contain such information normally present in complete method descriptions. The list of key points presented in the SANCO Guidance Document d may serve as a guide ... 

J. N. Hogsett, cf., method description in F. E. Critchfield, Organic Functional Group Analysis (International Series of Monographs on Analytical Chemistry, Vol. 8), Pergamon Press, Oxford, 1963, p. 95. 

The Student s (W.S. Gossett) /-lest is useful for comparisons of the means and standard deviations of different analytical test methods. Descriptions of the theory and use of this statistic are readily available in standard statistical texts including those in the references [1-6]. Use of this test will indicate whether the differences between a set of measurement and the true (known) value for those measurements is statistically meaningful. For Table 36-1 a comparison of METHOD B test results for each of the locations is compared to the known spiked analyte value for each sample. This statistical test indicates that METHOD B results are lower than the known analyte values for Sample No. 5 (Lab 1 and Lab 2), and Sample No. 6 (Lab 1). METHOD B reported value is higher for Sample No. 6 (Lab 2). Average results for this test indicate that METHOD B may result in analytical values trending lower than actual values. 

Where possible, the ASTM test method description and designation have been included. 

Forms should be self-contained, but should not try to repeat the content of the SOPs or method descriptions. 

Copy of the protocol/amendments (title of study purpose, including expected benefits obtained by doing the study participant selection criteria par ticipant exclusion criteria study design, including as needed, a discussion of the appropriateness of research methods description of methods performed)... 

The recovery of the main compound (100%) and all relevant impurities (spiked at, for example, the 0.5% wt/wt level) in a reference solution are calculated against a freshly prepared reference solution as described in the method description. This is done to demonstrate effects of the studied parameters on the recovery. 

DRAFT METHOD DESCRIPTION AND METHOD EVALUATION PHASE... 

All requirements described in the MDR are considered during method development. Either an intuitive or an experimental design approach may be applied when optimizing methods, resulting in an optimal separation of the main compound and all relevant impurities in a reasonable analysis time using typical CE conditions. The development activities are mainly performed by the AD lab (Method Development Phase). Before submitting the method it should be evaluated for robustness and daily lab-to-lab application performance (Method Evaluation Phase). Is the method doable in all the application labs Is the method description acceptable Are all customer needs accounted for ... 

For the current example, optimal conditions were selected at 5 mM a-CD, 2% wfv S- -CD, a buffer electrolyte concentration of lOmM, and a run voltage of lOkV. The resulting electropherogram obtained at the predicted optimal conditions is shown in Figure 9. These separation conditions were included in the draft test method description. 

The selectivity is demonstrated by analysis of a mixture of the relevant compounds, e.g., a selectivity batch/sample solution. The resulting electropherogram is compared with the selectivity electropherogram provided in the method description. The resolution between the critical peak pair(s) is determined. The target resolution should be >2.0 (the calculation... 

The method development and optimization phase is completed with test method description drafted according to the method development results. The following method evaluation tests will continue with direct involvement of the customer (receiving laboratory). The goal is to check whether the developed late phase method performs adequately in different labs. 

The development lab can benefit from valuable objective data to detect method shortcomings and to identify gaps in the method development process. The feedback on method performance should be discussed regularly. During the monitoring a number of key performance indicators are recorded and filled out in feedback sheets by the application labs (stability and operational labs) each time the method is applied. The method feedback sheet is sent together with the method description to the application labs at transfer. An example of such a feedback sheet is shown in Figure 22. 

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