Pharmaceutical developments method types used

The weaknesses associated with the flow through an orifice and angle of repose measurements limit their application for powder flow studies and hopper designs. Consequently, several powder shear testers and methods that permit a more thorough and precisely defined assessment of powder flow characteristics were developed. Shear testers that measure the frictional characteristics of a powder bed under load yield valuable information with regard to powder flow in high-speed tablet equipment. A number of types of shear cell testers are available, but the most common types used in the pharmaceutical industry are the Jenike shear cell and the Schulze ring shear tester.61,62... 

The comprehensive profiling of drug substances and pharmaceutical excipients as to their physical and analytical characteristics remains at the core of pharmaceutical development. As a result, the compilation and publication of comprehensive summaries of physical and chemical data, analytical methods, routes of compound preparation, degration pathways, uses and applications, etc., has always been a vital function to both academia and industry. Historically, the Profiles series has always provided this type of information, and has striven to publish the highest quality available. 

Among the various types of atomic spectroscopy, only two, flame emission spectroscopy and atomic absorption spectroscopy, are widely used and accepted for quantitative pharmaceutical analysis. By far the majority of literature regarding pharmaceutical atomic spectroscopy is concerned with these two methods. However, the older method of arc emission spectroscopy is still a valuable tool for the qualitative detection of trace-metal impurities. The two most recently developed methods, furnace atomic absorption spectroscopy and inductively coupled plasma (ICP) emission spectroscopy, promise to become prominent in pharmaceutical analysis. The former is the most sensitive technique available to the analyst, while the latter offers simultaneous, multielemental analysis with the high sensitivity and precision of flame atomic absorption. 

ASE method development is very easy, as it requires the selection of the temperature and solvents, which govern the efficiency of the extraction. The other parameters that control the recovery of the extraction are the static time, the flushing volume and the number of static cycles used in the extraction. It is very interesting to note that the first application of this method was reported in the extraction of environmental pollutants [30-38]. Therefore, the ASE method has become very popular in the extraction of environmental samples [39]. Moreover, its use has been expanded for the extraction of many organic and inorganic substances from foodstuffs, polymers, pharmaceuticals and other types of sample. The application of the ASE technique for environmental samples is summarized in Table 5.3. 

A new brush-type CSP, the Whelk-0 1, was used by Blum et al. for the analytical and preparative-scale separations of racemic pharmaceutical compounds, including verapamil and ketoprofen. A comparison of LC and SFC revealed the superiority of SFC in terms of efficiency and speed of method development [50]. The Whelk-0 1 selector and its homologues have also been incorporated into polysiloxanes. The resulting polymers were coated on silica and thermally immobilized. Higher efficiencies were observed when these CSPs were used with sub- and supercritical fluids as eluents, and a greater number of compounds were resolved in SFC compared to LC. Compounds such as flurbiprofen, warfarin, and benzoin were enantioresolved with a modified CO, eluent [37]. 

Recently Turner and coworkers have sought to extend the deracemization method beyond a-amino acids to encompass chiral amines. Chiral amines are increasingly important building blocks for pharmaceutical compounds that are either in clinical development or currently licensed for use as drugs (Figure 5.7). At the outset of this work, it was known that type II monoamine oxidases were able to catalyze the oxidation of simple amines to imines in an analogous fashion to amino acid oxidases. However, monoamine oxidases generally possess narrow substrate specificity and moreover have been only documented to catalyze the oxidation of simple, nonchiral... 

NMR microscopy is ultimately an innovative method of research and it is not surprising that most of the commercially installed systems, approximately 80%, are installed in public scientific research centers, where new applications are continuously being developed. The method is not particularly widely distributed in industry, where standardized methods are more often used. However, NMR microscopy is mainly used in the pharmaceutical industry for the development of new drugs, in the food industry for the development of new types of food, in the chemical industry for creating and characterizing new materials and in the polymer industry, e.g., for creating new mixtures for tires. 

As can be seen in Fig. 3b, it is important to specify whether data are represented as a number distribution (obtained by a counting technique such as microscopy) or as a weight distribution (obtained by methods such as sieving), since the results will not be the same. Hatch and Choate [4] have developed equations for converting one type of diameter to another the relationships between them are summarized in Table 2. Note that caution should be exercised in using the Hatch-Choate conversions if the distributions do not closely fit the log-normal model. While this distribution is the most frequently used to describe pharmaceutical systems, other distribution functions have also been developed [2,5,6],... 

A preservative is a substance that prevents or inhibits microbial growth and extends the shelf life of the drug products. In most pharmaceutical drug products, only a few compounds are typically selected as preservatives. For efficiency, a generic method should be developed for the types of preservatives that are more commonly used. For example, butylated hydroxytoluene (BHT) is an antioxidant commonly used in many solid dosage formulations to retard oxidative degradation of the excipients. 

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