title: Standardless multicomponent qNMR analysis of compounds with overlapped resonances based on the combination of ICA and PULCON.
abstract: A fast and reliable nuclear magnetic resonance (NMR) method for quantitative analysis of targeted compounds with overlapped signals in complex mixtures has been established. The method is based on the combination of chemometric treatment for spectra deconvolution and the PULCON principle (pulse length based concentration determination) for quantification. Independent component analysis (ICA) (mutual information least dependent component analysis (MILCA) algorithm) was applied for spectra deconvolution in up to six component mixtures with known composition. The resolved matrices (independent components, ICs and ICA scores) were used for identification of analytes, calculating their relative concentrations and absolute integral intensity of selected resonances. The absolute analyte concentrations in multicomponent mixtures and authentic samples were then calculated using the PULCON principle. Instead of conventional application of absolute integral intensity in case of undisturbed signals, the multiplication of resolved IC absolute integral and its relative concentration in the mixture for each component was used. Correction factors that are required for quantification and are unique for each analyte were also estimated. The proposed method was applied for analysis of up to five components in lemon and orange juice samples with recoveries between 90% and 111%. The total duration of analysis is approximately 45 min including measurements, spectra decomposition and quantification. The results demonstrated that the proposed method is a promising tool for rapid simultaneous quantification of up to six components in case of spectral overlap and the absence of reference materials.
authors.affiliation: Institute of Chemistry, Saratov State University, Astrakhanskaya Street 83, 410012, Saratov, Russia.|Spectral Service AG, Emil-Hoffmann-Straße 33, 50996, Cologne, Germany.
authors.forename: Yulia B
authors.initials: YB
authors.lastname: Monakhova
authors.affiliation: Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, 76187, Karlsruhe, Germany.
authors.forename: Dirk W
authors.initials: DW
authors.lastname: Lachenmeier
authors.affiliation: Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, 76187, Karlsruhe, Germany.
authors.forename: Thomas
authors.initials: T
authors.lastname: Kuballa
authors.affiliation: Institute of Chemistry, Saratov State University, Astrakhanskaya Street 83, 410012, Saratov, Russia.
authors.forename: Svetlana P
authors.initials: SP
authors.lastname: Mushtakova
keywords: 1H NMR; PILCON principle; fruit juice; independent component analysis; standardless analysis