FT-IR and Raman spectroscopic methods for identification and quantitation of orthorhombic and monoclinic paracetamol in powder mixes.
FT-IR and Raman spectroscopic methods are suggested for identification of orthorhombic (form II) and monoclinic (form I) paracetamol and for their quantitative determination in mixes. The intensity ratio of the 836 cm(-1) FT-IR band (attributed to the presence of both forms) to the 806 cm(-1) monoclinic band plotted against the inverse monoclinic molar fraction (X) yields a straight line: I(836)/I(806)=0.515/X+0.700, r=0.9965 for eight calibration points on the regression line. Similarly, the area under the 454 cm(-1) band in FT-Raman spectra (which is attributed to both forms) over the area under the 465 cm(-1) band of monoclinic form is inversely related to its molar fraction (X): A(454)/A(465)=0.482/X-0.324, r=0.9954 for eight calibration points. Precision (RSD%) was <5% for both methods. Linear regression analysis between content and intensity of characteristic XRD reflections for four different samples gave r=0.9964 at 4.62 A and r=0.9894 at 3.70 A, for form II. For the content of form I, r=0.9596 at 3.37 A. The limit of detection for monoclinic form was estimated to be 0.012 mole fraction for both methods.
Al-Zoubi
N
N
Department of Pharmaceutical Technology, School of Pharmacy, University of Thessaloniki, Thessaloniki 54124, Greece.
Koundourellis
J E
JE
Malamataris
S
S
D000082:Acetaminophen / Q000032:analysis* / Q000737:chemistry*; D018360:Crystallography, X-Ray; D004339:Drug Compounding; D011208:Powders; D017550:Spectroscopy, Fourier Transform Infrared / Q000379:methods*; D013059:Spectrum Analysis, Raman
D011208:Powders; D000082:Acetaminophen