Pharmaceutical analysis HPLC

Other early food applications included the analysis of pesticide residues in fruits and vegetables, organic acids, lipids, amino acids, toxins (e.g., aflatox-ins in peanuts, ergot in rye), and contaminants. As with pharmaceutical analysis, HPLC provides the ability to analyze for vitamin content in food... 

FdPLC has contributed many successes in product development and in quality control for the pharmaceutical industry. The UV detector coupling with HPLC equipment is the most important analytical instrument for preformulation, QC/QA, and in-process control in pharmaceutical analysis. HPLC is a basic and reliable analytical tool for preformulation study because of the high-resolution capacity, accuracy, and reproducibility of the equipment. Its primary function includes search for and detection of impurities in drug substances, as well as stability evaluation of dosage forms in terms of detection and quantitation of degradation products. 

The official methods (pharmacopoeial methods) in this respect are different from the methods used in the industrial analysis. For example, in the United States Pharmacopoeia, HPLC is the primary method and TLC the second choice. Application of the methods used for purity testing in the British Pharmacopoeia is different TLC is the primary method, and HPLC is the second choice. But, both Pharmacopoeias are in agreement that conventional TLC is used without instrumentation. In the industrial pharmaceutical analysis, HPLC and instrumental TLC are more or less used equally and in many cases in conjunction. 

In a 1987 paper, Osborne investigated the use of NIR spectroscopy in the determination of nicotinamide in vitamin pre-mixes [32]. Although this was not specifically a tablet matrix, the study showed potential advantages of the method for pharmaceutical analysis. HPLC was the existing reference method for nicotinamide, requiring 3 days to analyze 36 samples. The proposed NIR method required only 30 min to analyze the same samples. 

However, compared with the traditional analytical methods, the adoption of chromatographic methods represented a signihcant improvement in pharmaceutical analysis. This was because chromatographic methods had the advantages of method specihcity, the ability to separate and detect low-level impurities. Specihcity is especially important for methods intended for early-phase drug development when the chemical and physical properties of the active pharmaceutical ingredient (API) are not fully understood and the synthetic processes are not fully developed. Therefore the assurance of safety in clinical trials of an API relies heavily on the ability of analytical methods to detect and quantitate unknown impurities that may pose safety concerns. This task was not easily performed or simply could not be carried out by classic wet chemistry methods. Therefore, slowly, HPLC and GC established their places as the mainstream analytical methods in pharmaceutical analysis. 

Ahuja S, Dong MW. Handbook of pharmaceutical analysis by HPLC, Amsterdam, Elsevier Academic, 2005. 

Szepesi, G., HPLC in Pharmaceutical Analysis. Vol. I. General Considerations, CRC Press, Boca Raton, FL, 1990, chap. 8. 

G. Lunn, HPLC Methods for Pharmaceutical Analysis, Vol. 4, Wiley-Interscience Publication, John Wiley Sons, Inc., New York, 2000, pp. 1250-1256. 

Separation-based techniques, especially high-performance liquid chromatography (HPLC) and gas chromatography (GC), have long been the work horses of pharmaceutical analysis laboratories. They are among the most powerful and versatile tools for the detection and quantitation of analytes (chemical components) in complex matrices frequently encountered in the course of PhR D. 

FIA has also found wide application in pharmaceutical analysis.214,215 Direct UV detection of active ingredients is the most popular pharmaceutical analysis application of FIA. For single component analysis of samples with little matrix interference such as dissolution and content uniformity of conventional dosage forms, many pharmaceutical chemists simply replace a column with suitable tubing between the injector and the detector to run FIA on standard HPLC instrumentation. When direct UV detection offers inadequate selectivity, simple online reaction schemes with more specific reagents including chemical, photochemical, and enzymatic reactions of derivatization are applied for flow injection determination of pharmaceuticals.216... 

S. Ahuja and M.W. Dong, Handbook of Pharmaceutical Analysis by HPLC, Elsevier, Amsterdam, The Netherlands, 2005. 

D Acquarica, L, New synthetic strategies for the preparation of novel chiral stationary phases for HPLC containing natural pool selectors, presented at 8 Int. Meeting on Recent Developments in Pharmaceutical Analysis, Roma, June 29-July 3, 1999, 37. 

The contents of this book have been highlighted below to provide the reader with an overview of pharmaceutical analysis by HPLC. 

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. 

Chiral separation of drng molecules and of their precursors, in the case of synthesis of enantiomerically pure drugs, is one of the important application areas of HPLC in pharmaceutical analysis. Besides HPLC, capillary electrophoresis (CE) is another technique of choice for chiral separations. Chapter 18 provides an overview of the different modes (e.g., direct and indirect ones) of obtaining a chiral separation in HPLC and CE. The direct approaches, i.e., those where the compound of interest is not derivatized prior to separation, are discussed in more detail since they are cnrrently the most frequently used techniques. These approaches require the use of the so-called chiral selectors to enable enantioselective recognition and enantiomeric separation. Many different molecnles have been nsed as chiral selectors, both in HPLC and CE. They can be classified into three different groups, based on their... 

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