Moisture determination, near infrared

Infrared spectra of fats and oils are similar regardless of their composition. The principal absorption seen is the carbonyl stretching peak which is virtually identical for all triglyceride oils. The most common appHcation of infrared spectroscopy is the determination of trans fatty acids occurring in a partially hydrogenated fat (58,59). Absorption at 965 - 975 cm is unique to the trans functionaHty. Near infrared spectroscopy has been utilized for simultaneous quantitation of fat, protein, and moisture in grain samples (60). The technique has also been reported to be useful for instmmental determination of iodine value (61). 

Kamat, M. S., Lodder, R. A., De Luca, P. R Near-infrared spectroscopic determination of residual moisture in lyophilized sucrose through intact glass vials. Pharmaceutical Research 6, p. 961-965, 1989. Copyright 1989 Plenum Publishing Corp, New York, N. Y USA... 

X. Zhou, PA. Hines, K.C. White and M.W. Borer, Gas chromatography as a reference method for moisture determination by near-infrared spectroscopy, Anal. Chem., 70, 390-394 (1998). 

X. Zhou, P.A. Hines, and M.W. Borer, Moisture determination in hygroscopic drug substances by near infrared spectroscopy, J. Pharm. Biomed. Anal, 17, 219-225 (1998). 

O. Bemtsson, G. Zackrisson and G. Ostling, Determination of moisture in hard gelatin capsules using near-infrared spectroscopy applications to at-line process control of pharmaceutics, J. Pharm. Biomed. Anal, 15, 895-900 (1997). 

R.M. Leasure and M.K. Gangwer, Near-infrared spectroscopy for in-process moisture determination of a potent active pharmaceutical iugredieut. Am. Pharm. Rev., 5(1), 103-104, 106, 108-109 (2002). 

M. Savage, J. Torres, L. Franks, B. Masecar and J. Hotta, Determination of adequate moisture content for efficient dry-heat viral inactivation in lyophUized factor VIII by loss on drying and by near infrared, Biologicals, 26, 119-124 (1998). 

T. Moy, A. Calabria and C. Hsu, Near infrared a non-invasive method to determine residual moisture of lyophi-lized protein pharmaceuticals, American Chemical Society 221st National Meeting, BIOT-016. Meeting abstract, 2001. 

J.A. Jones, I.R. Last, B.R MacDonald and K.A. Prebble, Development and transferability of near-infrared methods for determination of moisture in a freeze-dried injection product, J. Pharm. Biomed. Anal. 11, 1227-1231 (1993). 

Reeves, J.B. Ill and Van Kessel, J.S. (2000) Determination of ammonium-N, moisture, total C and total N in dairy manures using a near infrared fibre-optic spectrometer. Journal of Near Infrared Spectroscopy 8, 151-160. 

Adams, M.J., Latham, K., Barnett, N. W., and Poynton, A. J. (1999). Calibration models for determining moisture and fat content of processed cheese using near-infrared spectrometry. J. Sci. Food Agric. 79,1232-1236. 

The optimal moisture content of the dried granulation needs to be determined. High moisture content can result in (1) tablet picking or sticking to tablet punch surfaces and (2) poor chemical stability as a result of hydrolysis. An overdried granulation could result in poor hardness and friability. Moisture content analysis can he performed using the conventional loss-on-drying techniques or such state-of-the-art techniques as near infrared (NIR) spectroscopy. 

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]. 

Lin and Hsu [1.85] described the determination of residual moisture in protein pharmaceuticals in sealed glass vials by near-infrared (NIR) spectroscopy. Five proteins were studied recombinant humanized monoclonal antibody (rhuMAb) E25, rhuM-Ab HER2, rhuMAb CDlla, TNKase and rt-PA. Higher moisture contents (RM) were obtained by adding appropriate amounts of MilliQ water to the wall of the vial in a... 

Iin, T.P., Hsu, Ch.C Determination of residual moisture in lyophilized protein pharmaceuticals using a rapid and non-invasive method near-infrared spectroscopy. PDA J. Pharm. Sci. Technol. 56, pp. 196-205, 2002... 

Last and Prebble [51 ] developed a near-infrared reflectance (NIR) method for the determination of moisture in an experimental freeze-dried injection product. NIR spectra were collected through the bases of unopened product vials using a horizontal instrument accessory. The samples in these vials were then used for Karl Fischer analysis to generate a standard curve for the analysis. The NIR data must be correlated with an accepted residual moisture technique in order to yield a meaningful result. This article states that NIR accuracy and precision in this application are not consistent with allowing the use of the current method in anything but a screening role. 

Near-Infrared Spectroscopy. Near-infrared (NIR) spectroscopy is a technique that has been around for some time but, like NMR spectroscopy, has only recently been improved and developed for on-line applications. Near-infrared analysis (NIRA) is a nondestructive technique that is versatile in the sense that it allows many constituents to be analyzed simultaneously 112, 113). The NIR spectrum of a sample depends upon the anharmonic bond vibrations of the constituent molecules. This condition means that the temperature, moisture content, bonding changes, and concentrations of various components in the sample can be determined simultaneously. In addition, scattering by particles such as sand and clay in the sample also allows (in principle) the determination of particle size distributions by NIRA. Such analyses can be used to determine the size of droplets in oil-water emulsions. 

Salsa, T. Pina, M.E. Teixeira-Dias, J.J.C. Crosslinking of gelatin in the reaction with formaldehyde an ftir spectroscopic study. Appl. Spectrosc. 1996, 50 (10), 1314—1318. Buice, R.G. Gold, T.B. Lodder, R.A. Digenis, G.A. Determination of moisture in intact gelatin capsules by near-infrared spectrophotometry. Pharm. Res. 1995,12 (1), 161-163. 

Another task often required is the determination of the water content. Quantification of moisture in hard gelan-tin capsules was described by Berntsson, Zackrisson, and Oestling who discussed its importance in monitoring for at-line process control. ° A sparse MLR calibration model with three optimized near-infrared wavelengths yielded an absolute prediction error of... 

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