Near infrared spectroscopy method validation

N. Broad, P. Graham, P. Hailey, et al., Guidelines for the development and validation of near-infrared spectroscopic methods in the pharmaceutical industry. In Handbook of Vibrational Spectroscopy, vol. 5, J.M. Chalmers and PR. Griffiths (eds), John Wiley Sons Ltd, Chichester, 3590-3610, 2002. 

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. 

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. 

C. Kradjel and L. McDermott, Determinationof the Thickness of Plastic Sheets Used in Blister Packaging by Near infrared Spectroscopy Development and Validation of the Method, NiR Analysis of Polymers, in Handbook of Near-Infrared Analysis, 3rd ed., CRC Press, Boca Raton, FL, 2007. 

PLSR is commonly nsed to correlate different data sets to each other (e.g., sensory to chemical measmements), as well as for prediction purposes (i.e., substitution of various wet chemistry methods by a near-infrared spectroscopy (NIR)-based model). One example for the former case is the correlation of the sensory and instrumental flavor perception in ice creams with different flavor compounds and additionally also varying in fat levels [15]. A qnantitative and validated prediction model for fatty acid profile, fat and water content, retrogradation, and viscosity was developed by [ 16] for the characterization of potato, maize, wheat, rice, and tapioca starches for industrial purposes. 

M. Blanco, J. Coello, A. Eustaquio, H. Itturriaga and S. Maspoch, Development and validation of methods for the determination of miokamycin in various pharmaceutical preparations by use of near infrared reflectance spectroscopy, Analyst, 124, 1089-1092 (1999). 

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. 

Bradfield, K.B. Forbes, R.A. Development and validation of an analytical method for identification of granulated nicarbazin by near infrared reflectance spectroscopy. J. Near Infrared Spectrosc. 1997, 5, 41-65. 

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. 

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). 

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). 

M. Blanco,). Coello, A. Eustaquio,H. Itturriaga, andS. Maspoch, Development and Validation of Methods for the Determination of Miokamycin in Various Pharmaceutical Preparations by Use of Near Infrared Reflectance Spectroscopy, AnflZysf, 124(7), 1089 (1999). 

Although the pharmaceutical industry was slow in adopting this technique, a number of pharmaceutical applications of near-infrared (NIR) have been reported. This chapter will discuss the development, application, and validation of NIR spectroscopy for the pharmaceutical industry the software and multivariate methods used for this work are covered extensively in other chapters and will be mentioned in passing. 

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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