Near-infrared spectroscopy product development

Brazier, D.W. (1981) Calorimetric studies of rubber vulcanization and rubber vulcanisates, in Grassie, N. (Ed.) Developments in Polymer Degradation - 3, London Applied Science. Brimmer, P. J., Monfre, S. L. Dethomas, F. A. (1992) Real-time monitoring for the production of polyurethane, in Murray, I. Cowe, LA. (Eds.) Making Light Work Advances in Near Infrared Spectroscopy, Weinheim VCH. 

In many ways, near-infrared spectroscopy is an ideal method for pharmaceutical process control, particularly for the analysis of intact dosage forms. As production costs, including analytical expenses, continue to increase, the advantages of NIR spectroscopy will become more attractive. With near-infrared spectroscopy, the pharmaceutical industry will move one step closer to zero-defect quality control, making the costs associated with the method s development well spent. 

M. M. Said, S. Gibbons, A. C. Moffat, and M. Zloh, A Novel Sample Selection Strategy by Near-Infrared Spectroscopy-Based High Throughput Tablet Tester for Content Uniformity in Early-Phase Pharmaceutical Product Development. Note missing reference J Pharm Sci. 2012 Jul 101(7) 2502-ll. doi 10.1002/jps.23153. Int.. Pharm., 415,102 (2011). 

Of the analytical techniques available for process analytical measmements, IR is one of the most versatile, where all physical forms of a sample may be considered - gases, liquids, solids and even mixed phase materials. A wide range of sample interfaces (sampling accessories) have been developed for infrared spectroscopy over the past 20 to 30 years and many of these can be adapted for either near-lme/at-lme production control or on-line process monitoring applications. For continuous on-line measurements applications may be limited to liquids and gases. However, for applications that have human interaction, such as near-line measurements, then all material types can be considered. For continuous measurements sample condition, as it exists within the process, may be an issue and factors such as temperature, pressure, chemical interfer-ants (such as solvents), and particulate matter may need to be addressed. In off-line applications this may be addressed by the way that the sample is handled, but for continuous on-line process applications this has to be accommodated by a sampling system. 

IR is a nondestructive technique suitable for the analysis of formulated products, and gives a considerable amount of information about the compounds present. Near-infrared (from 13 000 to 4000 cm ) and Fourier transform infrared (FTIR) (from 4000 to 400 cm ) spectroscopies are used. Qualitative analysis of the ethanol soluble fraction allows the identification of functional group types such as hydrotropes (xylenesulfonate and toluenesulfonate). In addition, zeolite, alkalis, polymers, and builders may be identified in the insoluble ethanol fraction. For quantitative analysis, method development is slow because a great number of calibration standards... 

H. Mark, G. E. Ritchie, R. W. Roller, E. W. Ciurczak, C. Tso, and S. A. MacDonald, Validation of a Near-Infrared Transmission Spectroscopic Procedure. Part A. Validation Protocols, /. Pharm. Biomed. Anal, 28,251 (2002). G. E. Ritchie, R. W. Roller, E. W. Ciurczak, H. Mark, C. Tso, and S. A. MacDonald, Validation of a Near-Infrared Transmission Spectroscopic Procedure. Part B. Application to Alternate Content Uniformity and Release Assay Methods for Pharmaceutical Solid Dosage Forms, /. Pharm. Biomed. Anal, 29,159 (2002). M. Blanco, M. Bautista, and M. Alcala, API Determination by NIR Spectroscopy across Pharmaceutical Production Process, AAPS PharmSciTech, 9,1130 (2008). A. Peinado, J. Hammond, and A. Scott, Development, Validation and Transfer of a Near Infrared Method to Determine In-Line the End Point of a Fluidised Drying Process for Commercial Production Batches of an Approved Oral Solid Dose Pharmaceutical Product, /. Pharm. Biomed. Anal, 54,13 (2011). 

Near-infrared reflectance spectroscopy has been traditionally developed in animal science to evaluate the chemical composition of forages (4, 5, 15). Compared with forages, little information is available on the suitability of NIR spectroscopy in the estimation of the chemical composition and nutritive value of by-product materials derived from livestock. The information available in the literature relates only to the use of NIR spectroscopy to determine gross chemical composition such as dry matter (DM), crude protein (CP), fat (oil), and amino acid content in a few livestock animal by-products. Examples of NIR applications in animal by-products are summarized in Tables 8.3.3 and 8.3.4. Good correlations were found for DM and CP in the different animal by-products. Although good correlations were found for some amino acids, Fontaine et al. (22) stated that the calibration for sulfur-containing amino acids are... 

Near-infrared (NIR) spectroscopy was initially used for measurements in low-moisture products. Its first application in dairy industry was mainly for the analysis of milk powders. Over the intervening years, developments both in hardware and in software have permitted analyses even of cheese and later of liquid milk. The transformation of milk into cheese or fermented milk is a very complex sequence of events, in which physical changes also take place, shifting from a basically liquid structure toward a solid or semisolid structure. 

CJ Frank, Raman spectroscopy for identity testing Applications from development to production in the pharmacetrical industry. In A Katzir, WS Grundfest, eds. Proceedings of the International Symposium on Biomedical Optics (BIOS 99). Bellingham, WA SPIE, 1999, Abstract 3608-08. AM Tudor, MC Davies, CD Melia, DC Lee, RC Mitchell, PJ Hendra, SJ Church. The application of near-infrared Fourier transform Raman spectroscopy to the analysis of polymorphic forms of cimetidine. Spectrochim Acta 47A 1389-1393, 1991. 

Therefore, during the past 30 years, numerous vibrational spectroscopic methods (near infrared, NIR infrared, IR and Raman spectroscopy) have been introduced as very efficient alternatives, which are widely used today to determine fats, proteins, and carbohydrates and also numerous secondary plant substances occurring in agricultural products. For authentication purposes, the mentioned spectroscopic techniques can provide the valuable data in a few minutes, allowing the discrimination of different agrofood samples. Also new developments of IR and Raman microscopes have considerably extended the field of application. These sophisticated techniques allow to perform point-by-point measurements (mapping) or to acquire simultaneously spectra (imaging) from a small sample area. 

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