title: Quantitation of active pharmaceutical ingredients and excipients in powder blends using designed multivariate calibration models by near-infrared spectroscopy.
abstract: This research note demonstrates the simultaneous quantitation of a pharmaceutical active ingredient and three excipients in a simulated powder blend containing acetaminophen, Prosolv and Crospovidone. An experimental design approach was used in generating a 5-level (%, w/w) calibration sample set that included 125 samples. The samples were prepared by weighing suitable amount of powders into separate 20-mL scintillation vials and were mixed manually. Partial least squares (PLS) regression was used in calibration model development. The models generated accurate results for quantitation of Crospovidone (at 5%, w/w) and magnesium stearate (at 0.5%, w/w). Further testing of the models demonstrated that the 2-level models were as effective as the 5-level ones, which reduced the calibration sample number to 50. The models had a small bias for quantitation of acetaminophen (at 30%, w/w) and Prosolv (at 64.5%, w/w) in the blend. The implication of the bias is discussed.
authors.affiliation: Global Analytical Development, Johnson & Johnson Pharmaceutical Research & Development, LLC 1000 Route 202, Raritan, NJ 08869, USA. wli1@prdus.jnj.com
authors.forename: Weiyong
authors.initials: W
authors.lastname: Li
authors.forename: Gregory D
authors.initials: GD
authors.lastname: Worosila
mesh_terms: D000082:Acetaminophen / Q000032:analysis; D002138:Calibration; D005079:Excipients / Q000032:analysis*; D015999:Multivariate Analysis; D011205:Povidone / Q000032:analysis; D011208:Powders / Q000032:analysis*; D019265:Spectroscopy, Near-Infrared; D013229:Stearic Acids / Q000032:analysis
chemical_list: D005079:Excipients; D011208:Powders; D013229:Stearic Acids; D000082:Acetaminophen; C031183:stearic acid; D011205:Povidone