#Mestrenova peak assignment report manual

This approach has been derived from statistical mathematics. Another strategy for enhancing spectral resolution has been developed by using covariance data processing. In order to compensate for the low resolution of, e.g., NIR or compact bench-top 1H NMR spectrometers, suitable multivariate data analysis procedures have been devised and applied where univariate data processing did not prove sufficient. Hence, in-, on-, and at-line monitoring types usually provide results in real-time. For at-line analysis, a sample is taken from the reaction and treated before analysis. When the measurement is conducted on-line, a bypass is used. For in-line monitoring, a probe is inserted into the reaction vessel. Process monitoring can proceed in-line, on-line, at-line or-less desirable-off-line. Therefore, spectroscopic techniques providing even relatively lower resolution and sensitivity than those commonly required for structure elucidation purposes satisfy the requirements for process monitoring. During process monitoring, the information sought is most often the quantity of a compound at a given time. More recently, nuclear magnetic resonance (NMR) spectroscopy has grown into focus. Among them, Raman and near-infrared (NIR) play major roles. Spectroscopy, spectrometry, and chromatography represent highly specific methods. TodayвЂ™s process analytical tools comprise a variety of methodologies and take advantage of their inherent features. Meeting the customer demand for reproducible product quality is an important prerequisite for the competitiveness of a company, which requires using facilities, resources, and energy in the most economical way. The process may be improved towards efficiency, hence cost reduction, sustainability, and safety. It further enables process control and allows process optimization. The process knowledge obtained aims at ensuring a constant final product quality. Process understanding results from their application, which in fact is process monitoring. Thus, process analytical instruments are located in or nearby large-scale processes and reactors. It has established itself as an important element of industrial production processes. Since the joint initiative of regulatory authorities and the pharmaceutical industry, process analytical technology (PAT) has evolved from a mere production support discipline into a fast-growing research area.

#Mestrenova peak assignment report manual

While the manual integration of the 1H NMR spectra followed by univariate analysis allowed to establish a concentration profile of the final product isoamyl acetate hence revealing more details, multivariate analysis was found more suitable for process automation. The results of the univariate and multivariate approaches were comparable with regard to reaction rates and concentrations. An alternative, elegant, and fit-for-automation approach for the kinetic analysis of the spectra was demonstrated in using multivariate curve resolution (MCR). The data obtained were interpreted in terms of a first-order kinetic model, and corresponding reaction rate constants were extracted. By means of this purely mathematical statistical procedure, the relevant signals of the process media were assigned to educts and products and thus made applicable for univariate data evaluation. To facilitate the identification of signals suitable for the extraction of concentration-time ( c-t) graphs, 2D heterocorrelation spectra were generated through covariance transformations applied to 1D Raman, NIR, and NMR data. Compact 1H NMR, NIR, and Raman spectroscopy were used to monitor the biocatalyzed hydrolysis and esterification of acetic anhydride to isoamyl acetate using immobilized Candida antarctica lipase B (CALB) in a microreaction system in real-time. The combination of microreaction systems and spectroscopy proved suitable due to dimension and compound reduction and real-time monitoring capabilities. Process analytical technology aims at process knowledge and process improvement, efficiency, and sustainability.