International Conference quantitative method

The method was validated in accordance to the guidelines of the international conference on harmonization (ICH). Data with respect to accuracy, within- and between run precision, recovery, detection and quantitation limits were reported and found to be within the accepted international criteria. Neither endogeneous substances nor the commonly used dmgs were found to interfere with the retention times of the analytes. Standard solutions of the dmg and quality control preparations at high and low level concentrations were demonstrated to be stable at room temperature and/or -20°C for long and short periods of time. 

Quantitative CE—MS studies were scarcely reported. " This subject is however of prime importance, particularly for the pharmaceutical industry where the reliability of analytical data is essential. For this reason, method development is generally followed by an evaluation of quantitative performance using an appropriate validation procedure performed in agreement with criteria established by the International Conference on Harmonisation of technical requirements for registration of pharmaceuticals for human use (ICH) and the Food and Drug Administraction (FDA) guidelines, or Societe Franqaise des Sciences et Techniques Pharmaceutiques (SFSTP) commissions. ... 

In general, the detection and identification of impurities present in API and formulations play an integral role in the drug development process and methods need to be developed to adequately resolve these species and quantitate them. The International Conference on Harmonization (ICH) [3] has published a guidehnes on impurities in new drug substances and new drug products (see Table 8-1). The acceptable limit of the impurities in drug substances is dependent upon the maximum daily dose and the quahfication threshold however, lower thresholds are sometimes deemed necessary if the... 

Analytical method validation has developed within the pharmaceutical industry over the years in order to produce an assurance of the capabilities of an analytical method. A recent text on validation of analytical techniques has been published by the international Conference on Harmonisation (ICH) [19]. This discusses the four most common analytical procedures (1) identification test, (2) quantitative measurements for content of impurities, (3) limit test for the control of impurities and (4) quantitative measurement of the active moiety in samples of drug substance or drug product or other selected components of the drug product. As in any analytical method, the characteristics of the assay are determined and used to provide quantitative data which demonstrate the analytical validation. The reported validation data for CE are identical to those produced by an LC or GC method [11] and are derived from the same parameters, i.e. peak time and response. Those validation parameters featured by the ICH (Table 1) are derived from the peak data generated by the method. Table 1 also indicates those aspects of a CE method (instrumentation and chemistry), peculiar to the technique, which can affect the peak data and highlights factors which can assist the user in demonstrating the validation parameters. 

As required by regulatory authorities [1-3, 6] and International Conference on Harmonisation (ICH) guidelines [7], analytical method validation is especially important in establishing the assay methods and procedures of quantitative or semi-quantitative measurement of target substances or compounds. Among the specification items for drug products, assay, content uniformity, and dissolution are typical of those which require almost full analytical validation. The purity test, related... 

Hamza, W., Rashwan, M., and Afify, M. A quantitative method for modelling context in concatenative synthesis using large speech database. In Proceedings of the International Conference on Acoustics Speech and Signal Processing 2001 (2001). 

Prior to its use a method has to be validated. Validation is the formal proof that the method is suitable for the intended purpose. This requires that all steps and parameters of the method have been clearly specified in a written method description, any necessary equipment was qualified, and acceptance criteria for each validation point have been agreed upon. For quantitative methods the International Conference on Harmonization (ICH) has issued specific guidelines for setting up a validation protocol and for parameters that have to be validated for different applications. These include specificity, accuracy, precision, LOD, LOQ, linearity, and range as well as robustness. The only required validation parameter for qualitative methods is specificity. 

Figure 6.1 presents what may be referred to as the near-infrared method validahon pyramid. Ritchie and Cimczak [28] presented this idea at the 9th International Diffuse Reflectance Conference (Chambersburg, Pennsylvania) in 1998. The figure shows that a NIR result, whether generated from a qualitative or quantitative method, can be traced back to a calibrated instrument and a calibrated computer hardware and software system. In addition, it reveals that the result was generated using a method that was found suitable for its intended use. Observed in this manner. 

Wysocka, W., Brukwicki, T., Macioszek, E. and Wolski, W. 1988. The influence of the isolation method on the quantitative and qualitative composition of the alkaloids from Lupinus albus seeds. In Proceedings 5th International Lupin Conference, July 5-8, 1988 (Twardowski, T., ed.). Poznan, Polish Academy of Sciences, Institute of Bioorganic Chemistry. 

Recovery. In the 2000 Washington Conference final report it is clearly stated that knowledge of recovery is not essential to assay validation, but it does provide useful information about the real amount of analyte that is being analyzed. Assessment of recovery at every step of sample preparation and analysis in which losses may occur provides a powerful diagnostic tool to improve the method if needed. If a good internal standard has been chosen, the losses will have no impact on quantitation because they will be similar for analyte and internal standard and will thus annul each other. On the other hand, recovery is very important to verify if the internal standard really mimics and matches the analyte. The discovery of significant and inconsistent differences in recovery between analyte and internal standard at different steps of sample cleanup and analysis could indicate possible failure of the method during the validation. 

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