Analysis pharmaceuticals

Raman spectroscopy is emerging as a powerful analytical tool in the pharmaceutical industry, both in PAT and in qualitative and quantitative analyses of pharmaceuticals. Reviews of analyses of pharmaceuticals by Raman spectroscopy have been published.158 159 Applications include identification of raw materials, quantification of APIs in different formulations, polymorphic screening, and support of chemical development process scale-up. Recently published applications of Raman spectroscopy in high-throughput pharmaceutical analyses include determination of APIs in pharmaceutical liquids,160,161 suspensions,162 163 ointments,164 gel and patch formulations,165 and tablets and capsules.166-172... 

In summary, the use of RPLC is ideal for pharmaceutical analyses because of the broad range of commercially available stationary phases because the most common RPLC mobile phases (buffers with acetonitrile or methanol) have low UV cut-off wavelengths, which facilitate high sensitivity detection for quantitation of low-level impurities and because selectivity can readily be controlled via mobile phase optimization. Additionally, the samples generated for selectivity screening (as detailed above) are typically aqueous based. In subsequent phases of pharmaceutical development, aqueous-based sample solvents are ideal for sample preparation and are, under limited constraints, compatible with MS detection required to identify impurities and degradation products. 

Ions are highly charged species by nature and lend themselves well to analysis by capillary electrophoresis (CE). In pharmaceutical analyses, we usually deal with small organic and inorganic anions and small cations or aliphatic amines. 

For the above-described reasons, molecular spectroscopic techniques have become the most common choices for pharmaceutical analysis in addition to chromatography. The latter, however, are being gradually superseded by the former in some industrial pharmaceutical processes. Recent technological advances have led to the development of more reliable and robust equipment. The ubiquity of computers has enabled the implementation of highly powerful chemometric methods. All this has brought about radical, widespread changes in the way pharmaceutical analyses are conducted. 

One other important point in using NIR spectroscopy in pharmaceutical analyses is its limited sensitivity, which complicates the determination of analytes at low concentrations by effect of too small analyte signals... 

The analytical capability of MS has been evolving at an astounding rate as Nobel laureates and developers push what is an inherently powerful analytical technique to even higher levels of capability. During the last decade, numerous ionization and analyzer configurations have been commercialized. Some of the most recent developments have made MS the gold standard for many pharmaceutical analyses, and has made the biopharmaceutical industry the major purchaser of mass spectrometers (Cudiamat, 2005). 

Hsieh, Y., Fukuda, E., Wingate, J., and Korfmacher, W. A. (2006). Fast mass spectrometry-based methodologies for pharmaceutical analyses. Comb. Chem. High Throughput Screening 9 3-8. 

The significance of this fact is twofold. First LC/MS has, indeed, become the method of choice for many pharmaceutical analyses. Because the utilization of analysis technology in the pharmaceutical industry is highly dependent on perception, the breakthroughs and barriers that LC/MS has overcome provided opportunity for acceptance and a widened scope of application. Currently, LC/MS is widely perceived in the pharmaceutical industry to be a viable choice, as opposed to a necessary alternative, for analysis. Second, these events led to an increased understanding of LC/MS in such a way that practitioners and collaborators have become more diverse. The result of this diversity is a mutually shared sense of purpose... 

Because of their importance in pharmaceutical analyses, much attention has been focused on harmonizing the parameters necessary for the validation of chromatographic methods. While some of these parameters are applicable to other analytical techniques, it is the responsibility of the analytical chemist to select and tailor the appropriate parameters and acceptance criteria for the particular method to be validated. Since most analytical chemists are not experts on regulatory matters, it is essential for the regulatory affairs professional to understand the requirements of method validation and work closely with the analytical chemist to select appropriate validation parameters and meaningful acceptance criteria. 

N. Kikuchi and T. Ohhata, High-performance liquid chromatography for pharmaceutical analyses. II. Major components in commercial cold medications, Iwate-Ken Eisei Kenkyusho Nenpo, 26 61 (1983). 

Advances in the manufacture of flexible fused silica WCOT columns will almost certainly extend the applications of GC by virtue of their high-resolution capability, while the advent of sophisticated, computerized detectors forecast the improvement in sensitivity and specificity. The use of chiral stationary phases for the resolution of enantiomers is becoming an increasingly important topic in pharmaceutical analyses. The range and availability of various liquid phases for chiral analysis by GC is bound to make this technique extremely valuable for the assay of pharmaceutical raw materials as well as for use in biological fluids. 

Comparative studies have often found that high performance TLC (HPTLC) is superior to HPLC in terms of total cost and time required for pharmaceutical analyses. " The Bibliography contains sources of general information on the principles, theory, practice, instrumentation, and applications of TLC and HPTLC. Detailed information on the subjects mentioned above as well as on additional topics and applications that could not be covered because of lack of space will be found in these references. 

We confidently predict that NIRS will rapidly become an established and standard method for many types of pharmaceutical analyses. 

For pharmaceutical analyses, it is necessary to have reliable methods. Results obtained using ion-selective membrane electrodes are the best because of the simplicity, rapidity, and accuracy of direct and continuous measurement of the activity of the ions in the solution. Another very important reason for the selection of electrochemical sensors for pharmaceutical assay is non-interference of by-products when the purity of a raw material is to be determined. 

In all accurate pharmaceutical analyses, samples are weighed by difference that is, the weight of sample added to the flask is determined by subtraction of consecutive weighings of the sample container. The procedure adopted is as follows. 

In the example above, a reaction was chosen that was quick to carry out and was quantitative, i.e. it went to completion. In many pharmaceutical analyses this is not the case and a back titration has to be carried out. 

When the concentration of the sample is expressed in percentage weight in volume (% w/v) org/100 mL, the constant used is A1%, 1 cm, usually written as A, and is called the specific absorbance, with units of dL g 1 cm-1 although, again, the value is usually quoted without units. The A value is very useful in pharmacy and pharmaceutical analyses where the molecular weight of the sample may be unknown (e.g. when analysing a macro-... 

In the past century, there has been a tremendous growth in pharmaceutical analyses and the role the analytical group plays in the development of new products. The baton was passed from techniques such as gravimetry, titrimetry, spectroscopy after extraction, and thin-layer paper chromatography to HPLC, gas chromatography, and various autoanalyzers. Emphasis was on tests such as assay, content and blend uniformity, and determination of impurities and residual solvents. 

The capillary format of SFC is attractive because of the potential of interfacing with a wide array of detectors available when carbon dioxide is used as the mobile phase. Several advances, beyond the issue of mobile-phase polarity, are, however, required prior to the technique becoming viable for pharmaceutical analyses. Capillary SFC instrumentation has lacked the requisite analytical performance for pharmaceutical analyses, and difficulties are encountered due to the acidic nature of fused silica and the problem of measuring impurities while, at the same time, not overloading the stationary phase with the main component. ... 

Biological Fluids. The pharmaceutical analyses of biological fluids provide the information necessary for evaluating the safety, therapeutic effect, and mechanism of action of a variety of drugs (95). 

Emphasizes thermal measurement techniques and the interpretation of corresponding data, particularly in pharmaceutical analyses... 

Derivative spectra are literally the derivatives of the normal spectra. Their analytical advantage stems from the fact that the slopes of the spectra of substances of narrow spectral bandwidth are usually higher in magnitude than those of substances with broad spectral bandwidth. As a result, the analyses of substances with narrow spectral bandwidth can often be performed in the presence of substances with broad spectral bandwidth, where the spectrum of the analyte appears as a shoulder on the spectrum of the broad-bandwidth interferant. The differentiation procedure was initially carried out manually. However, electronic differentiation techniques developed more recently have simplified the application of the techniques to pharmaceutical analyses. It is worth noting that though higher derivatives appear to improve resolution, the spectra obtained are also significantly distorted by noise. A trade-off is therefore required. 

Redox titrations are among the most important types of analyses performed in many areas of application, for example, in food analyses, industrial analyses, and pharmaceutical analyses. Titration of sulfite in wine using iodine is a common example. Alcohol can be deteirnined by reacting with potassium dichromate. Examples in clinical laboratories are rare since most analyses are for traces, but these titrations are still extremely useful for standardizing reagents. You should be familiar with some of the more commonly used titrants. 

In contrast to the well-known difficulties of traditionally applied quantitative IR spectroscopy of mixtures in solid (powdered) samples, the near-infrared reflectance analysis (NIRA) technique [32] has gained importance over the last decade and can now be implemented on a variety of commercially available Instruments In a number of applications to Industrial, agricultural and pharmaceutical analyses. Both the NIRA instruments equipped with grating monochromators and those fitted with filter systems feature built—In microprocessors with software suited to the Intrinsic characteristics of this spectroscopic alternative. Filter Instruments generate raw optical data for only a few wave-... 

In most pharmaceutical analyses, the answer to these questions is quite simple. The separation method will have to satisfy all the above criteria, because by meeting this criteria, the ruggedness of the method is tested. The end-user is most likely the QC laboratory in a manufacturing facility, and the ease with which a separation method can be transferred in most cases, R D laboratories to a QC laboratory will be highly dependent on the method development strategy used [37]. 

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