Trends in Pharmaceutical Analysis

This chapter provides the novice and the more experienced analyst with an overview of HPLC instrumentation, operating principles and recent advances or trends that are pertinent to pharmaceutical analysis. 

The author acknowledges helpful ideas and suggestions from R. Ornaf, D. Barker, C. Davidson, J. Bonilla, C. Choi and G. Miller from Purdue Pharma. This chapter has been presented in parts in short courses on Advanced HPLC in Pharmaceutical Analysis at Eastern Analytical Symposium 2001-2002, HPLC 2002, and Pittcon 2003. Numerous comments and suggestions from the attendees of these short courses were incorporated during the development of this chapter. 

Holler, F. J. and Nieman T. A., Principles of Instrumental Analysis, 5th ed., Brooks Cole, Pacific Grove, CA, 1997. 

Snyder, L. R. and Kirkland, J. J., Introduction to Modern Liquid Chromatography, John Wiley Sons, New York, 1979. 

Adamovics, J. A., Chromatographic Analysis of Pharmaceuticals, 2nd ed., Marcel Dekker, New York, 1997. 

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XI. INSTRUMENTATION TRENDS IN PHARMACEUTICAL ANALYSIS MANUFACTURERS SUMMARY AND CONCLUSION ACKNOWLEDGMENTS REFERENCES... 

HPLC Method Development Trends in Pharmaceutical Analysis... 

HPLC INSTRUMENTATION IN PHARMACEUTICAL ANALYSIS STATUS, ADVANCES, AND TRENDS... 

With the trend toward using Fast LC and small-bore columns (3-and 2-mm i.d.) in pharmaceutical analysis, increasing demand is placed on reducing the system dispersion or IBW. Figure 15 shows the deleterious effect of IBW on the performance of a Fast LC column showing that... 

Vankeirsbilck, T. Vercauteren, A. Baeyens, W. eta . Applications of Raman Spectroscopy in Pharmaceutical Analysis TrAC, Trends Anal. Chem. 2002, 21, 869-877. 

Vankeirsbilck T, Vercauteren A, Baeyens W, et al. Applications of Raman spectroscopy in pharmaceutical analysis. Trends Anal Chem 2002 21(12) 869-877. 

Perez-Parada, A., Colazzo, M., BesU, N., Dellacassa, E., Cesio, V, Heinzen, H., and Femandez-Alba, A.R. 2011. Pesticide residues in natural products with pharmaceutical use occurrence, analytical advances and perspectives. In Pesticides in the Modem World-Trends in Pesticide Analysis, ed. L.M. Stoytcheva, InTech Publisher, Rijeka (CR), pp. 357-390. ISBN 978-953-307A37-5. 

An overview of HPLC instrumentation, operating principles, and recent advances or trends that are pertinent to pharmaceutical analysis is provided in Chapter 3 for the novice and the more experienced analyst. Modern liquid chromatographs have excellent performance and reliability because of the decades of refinements driven by technical advances and competition between manufacturers in a two billion-dollar-plus equipment market. References to HPLC textbooks, reference books, review articles, and training software have been provided in this chapter. Rather than summarizing the current literature, the goal is to provide the reader with a concise overview of HPLC instrumentation, operating principles, and recent advances or trends that lead to better analytical performance. Two often-neglected system parameters—dwell volume and instrumental bandwidth—are discussed in more detail because of their impact on fast LC and small-bore LC applications. 

Sample preparation (SP) is generally not given adequate attention in discussions of pharmaceutical analysis even though its proper execution is of paramount importance in achieving fast and accurate quantification (see Chapter 5). Non-robust SP procedures, poor techniques, or incomplete extraction are the major causes of out-of-trend and out-of-specification results. The common SP techniques have been reviewed with a strong focus on tablets or capsules, as they are the primary products of the pharmaceutical industry. Detailed descriptions of SP methods for assays and impurity testing are provided with selected case studies of single- and multi-component products. 

This chapter presents an overview of current trends in high-pressure liquid chromatography (HPLC) instrumentation focusing on recent advances and features relevant to pharmaceutical analysis. Operating principles of HPLC modules (pump, detectors, autosampler) are discussed with future trends. 

As stated earlier, the SP trend in the pharmaceutical analysis of solid dosage forms is dominated by manual batch techniques such as grinding, sonication, dilution in volumetric flask and filtration. The unique SP requirements for solid dosages in grinding and handling large volumetries are particularly difficult to automate. 

Altria KD, Kelly MA, Clark BJ. Current applications in the analysis of pharmaceuticals by capillary electrophoresis. I. Trends Anal Chem 1998 17 204-14. 

Rao RN, Nagaraju V. An overview of the recent trends in development of HPLC methods for determination of impurities in drugs. Journal of Pharmaceutical and Biomedical Analysis 33, 335-377, 2003. 

Paulekuhn, G. S., Dressman, I. B., Saal, C. Trends in Active Pharmaceutical Ingredient Salt Selection Based on Analysis of the Orange Book Database. J. Med. Chem. 2007, 50, 6665-6672. 

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