title: Polarized spectroscopic elucidation of N-acetyl-L-cysteine, L-cysteine, L-cystine, L-ascorbic acid and a tool for their determination in solid mixtures.
abstract: Method of linear polarized vibrational (both IR- and Raman) spectroscopy of oriented colloids in nematic host is applied on N-acetyl-L-cysteine, L-cysteine, L-cystine and L-ascorbic acid with a view to obtain experimental bands assignment and local structural elucidation in solid-state. Structural results are compared with available crystallographic data for all of the systems studied. Scopes and limitations of the polarized method are shown. Discussion on the correlation between polarized spectroscopic data and the space group type as well as the number of the molecules in the unit cell (Z) is performed. Compounds with monoclinic space group P2(1), containing Z = 1 (N-acetyl-L-cysteine) and 2 (L-cysteine and L-ascorbic acid) are elucidated. One of the rare for organic molecules, hexagonal P6(1)22 space group and Z = 6 (L: -cystine) is also elucidated. Experimental assignment of the characteristics frequencies is obtained, explaining the typical for the crystals Fermi-resonance, Fermy-Davydov and Davydov splitting effects. For first time in the literature we are reported the orientation of the solid-mixture in nematic host, using the trade product ACC (Hexal, Germany), containing mainly N-acetyl-L-cysteine and L-ascorbic acid. Quantitative IR-spectroscopic approach for determination of solid mixtures is presented as well. The intensity ratio between 1,716 cm(-1) (characteristic for N-acetyl-L-cysteine) and 990 cm(-1), (attributed N-acethyl-cysteine and vitamin C) is used. Linear regression analysis between content and the peak ratio data for ten solid-binary mixtures, leads to straight-line plot y = 1.08(2) (+/-0.04(9)) + (-0.11(4) +/- 0.01(1))x, where x = 1/X ( i ). Factor r of 0.9641 and a reliability of 98.85% are obtained. The analysis of ACC 200 (Hexal, Germany) show that the IR measurements leads to standard deviation of 0.010 and 0.011 at P about 0.0500 for the systems and a confidence of >98.77(1)%.
authors.affiliation: Lehrstuhl für Analytische Chemie, Ruhr-Universität Bochum, Bochum, Germany. BKoleva@chem.uni-sofia.bg
authors.forename: Bojidarka
authors.initials: B
authors.lastname: Koleva
authors.forename: Michael
authors.initials: M
authors.lastname: Spiteller
authors.forename: Tsonko
authors.initials: T
authors.lastname: Kolev
mesh_terms: D000111:Acetylcysteine / Q000737:chemistry*; D001205:Ascorbic Acid / Q000737:chemistry*; D003545:Cysteine / Q000737:chemistry*; D003553:Cystine / Q000737:chemistry*; D015394:Molecular Structure; D013055:Spectrophotometry, Infrared / Q000379:methods*; D013059:Spectrum Analysis, Raman / Q000379:methods*
chemical_list: D003553:Cystine; D003545:Cysteine; D001205:Ascorbic Acid; D000111:Acetylcysteine