We present a method for extracting the active component from granulated nar
asin samples using chloroform with subsequent quantitation by near-infrared
absorption spectroscopy (NIRS). A multiple linear regression (MLR) calibra
tion equation was developed using a set of 41 calibration samples. The pote
ncies obtained using NIR analysis exhibit no larger than an 8% (3.03 mg/g)
error when compared to results based on the primary HPLC reference method.
We estimate the detection limit using this method to be 400 ppm narasin (20
mg/g potency), and the standard deviation for five independent extractions
of the same sample is approximate to 24 ppm (approximate to 1.2 mg/g poten
cy or approximately 1%). We also present the results from a robustness stud
y based upon a full factorial experimental design in which we varied extrac
tion and measurement parameters. This study indicates that sample mass caus
es the most variation in the results. Bottle-to-bottle variations in the ch
loroform used for the extraction also proved significant. Variations in sam
ple batch, number of spectral scans, and the interactions between sample ba
tch*soneration time, no. Scans*time in NIR, and sample batch*sample mass we
re borderline significant. (C) 2001 Elsevier Science B.V. All lights reserv
ed.