Degradation analytical techniques

In the field of bio-inorganic chemistry the many advantages of over iR NMR have already been realized to good advantage. Moreover, biosynthetic studies involving labels have already demonstrated their superiority over degradative analytical techniques involving labels. 

Analytical techniques will need to encompass the identification of very low levels of site-specific systems and their degradation and metabolic products.)... 

Having said this, it was felt therefore that there is a need for a book addressing analysis and characterisation of polymers from the point of view of what we wish to call the primary analytical question. Many excellent textbooks and reference works exist which address one or more individual analytical techniques, see, for example, references [1-10]. These books form the basis of the knowledge of the technique expert. They also contain many excellent and varied examples on successful applications of analytical techniques to polymer analysis and characterisation. There are also books which address the multitude of analytical techniques applied in polymer analysis, see, for example, references [11-24], However, a synthetic chemist may wish to know the constitution of his/her polymer chain, a material scientist may want to find out the reasons why a fabricated sample had failed. What technique is best or optimal to study chain constitution will depend on the situation. Polymer failure may result from morphological features, which needs to be avoided, a contaminant, a surface property degradation, etc. When a sample has been processed, e.g., a film blown, molecular orientation may be the key parameter to be studied. A formulation scientist may wish to know why an additive from a different supplier performs differently. It is from such points of view that polymer analysis and characterisation is addressed in this book. 

The fact that mineralization does not always occur justifies the large number of studies published as an effort to characterize the degradation products. In some cases these products are detected in human or animal urine, which may reach WWTPs and/or different environmental compartments. Probably, in the coming years more sophisticated analytical techniques to detect and quantify these metabolites will be developed. 

As ToF-SIMS is a surface analytical technique, it is well suited to the study of surface interaction between a material and its environment or between a material and products applied to it. The surface modifications can then be studied, making it possible to establish links with degradation processes. Published papers on the study of natural fibres related to cultural heritage typically illustrate this aspect of ToF-SIMS analysis. 

For LC peaks at 0.1% level or less, a considerably long acquisition time may be required to achieve suitable signal-to-noise ratio. A couple of analytical techniques may be used to concentrate the degradants before the LC-NMR analysis, such as column switching or solid phase... 

The i.v. approach has the distinct advantage of measurements being carried out under the most physiological conditions. On the other hand, the caveats include confounding effects of peripheral metabolism, which may give rise to artifactual brain uptake of degradation products. To exclude such a possibility the application of suitable analytical techniques to tissue and plasma samples is required. 

A major consequence of using regulatory limits based on degradant formation, rather than absolute change of the API level in the drug product, is that it necessitates the application and routine use of very sensitive analytical techniques [ 10]. In addition, the need to resolve both structurally similar, as well as structurally diverse degradants of the API, mandates the use of analytical separation techniques, for example, HPLC, CE, often coupled with highly sensitive detection modes, for example, ultraviolet (UV) spectroscopy, fluorescence (F) spectroscopy, electrochemical detection (EC), mass spectroscopy (MS), tandem mass spectroscopy (MS-MS) and so forth. 

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