Near-infrared spectroscopy validation process

Figure 1 presents what may be referred to as the near-infrared method validation pyramid. Ritchie [11] presented this idea at the Ninth International Diffuse Reflectance Conference (Chambersburg) in 1998. Since then, he has presented it at the Spectroscopy in Process and Quality Control Conference (SPQ) in 1999, the Eastern Analytical Symposium (EAS) in 1999, and the Pittsburgh Conference and Exposition on Analytical Chemistry and Applied Spectroscopy (PittCon) in 2000. 

The analytical method for moisture determination must be validated before use during process validation studies. There are numerous techniques for moisture analysis that range from physical methods, such as loss on drying, to chemical methods, such as Karl Fisher titration. A comparative review of the conventional techniques are presented in an overview [32], The measurement of residual moisture is lyophilized pharmaceuticals by near-infrared (NIR) spectroscopy has recently been expanded [33]. 

Pudelko-Koerner, C. (1998) Quantitative near-infrared reflectance spectroscopy of sennosides from Sennae fructus angustifoliae in in-process and quality control including method validation Pharmazeutische Industrie 60, 1007-1012. 

G. E. Ritchie and E. W. Ciurczak, Validating a Near-Infrared Spectroscopic Method, Proc. Spectroscopy in Process and Quality Control Conference, New Brunswick, NJ, October, 1999. 

C. Pudelko-Korner, Quantitative Near-Infrared-Reflection-Spectroscopy of Sennosides in Sennae fructus angustifoliae in Processing and Quality Control as well as Validation of these Methods, Pharma Technol. J., 19(1), 57-67 (1998). 

Ritchie, G. E. and Ciurczak, E. W. Validating a near-infrared spectroscopic method. In Spectroscopy in Process and Quality Control Conference Proceedings, East Brunswick NJ, 1999. 

Several applications can be found in literature regarding the use of NIR for the paediction of the main physical and rheological parameters of pasta and bread. De Temmerman et al. in 2007 proposed near-infrared (NIR) reflectance spectroscopy for in-line determination of moisture concentrations in semolina pasta immediately after the extrusion process. Several pasta samples with different moisture concentrations were extruded while the reflectance spectra between 308 and 1704 ran were measured. An adequate prediction model was developed based on the Partial Least Squares (PLS) method using leave-one-out cross-validation. Good results were obtained with R2 = 0,956 and very low level of RMSECV. This creates opportunities for measuring the moisture content with a low-cost sensor. 

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). 

PudeUco-Koerner, C., Quantitative Near-Infrared Reflectance Spectroscopy of Sennosides from Sennae fructus angustifoliae in In-Process and Quality Control Including Method Validation, Pharmazeutische Industrie, 60, 1007-1012 (1998). 

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