Abstract

An application of solid 13C nuclear magnetic resonance (NMR) spectroscopy for the determination of macronutrients, total polyphenols content, antioxidant activity, N C S elements, and pH in commercially available bee pollens is reported herein. Solid-state 13C NMR spectra were recorded for homogenized pollen granules without chemical treatment or dissolution of samples. By combining spectral data with the results of reference analyses, partial least squares models were constructed and validated separately for each of the studied parameters. To characterize and compare the models’ quality, the relative standard errors of prediction (RSEP) were calculated for calibration and validation sets. In the case of the analysis of protein, fat and reducing sugars, these errors were in the 1.8–2.5% range. Modeling the elemental composition of bee pollen on the basis of 13C NMR spectra resulted in RSEPcal/RSEPval values of 0.3/0.6% for the sum of NHCS elements, 0.3/0.4% for C, 1.8/1.9% for N, and 4.2/6.1% for S quantification. Analyses of total phenolics and ABTS antioxidant activity resulted in RSEP values in the 2.7–3.5% and 2.8–3.8% ranges, respectively, whereas they were 1.4–2.1% for pH. The obtained results demonstrate the usefulness of 13C solid-state NMR spectroscopy for direct determination of various important physiochemical parameters of bee pollen.

Highlights

  • 13 C nuclear magnetic resonance (NMR) SpectraSylwester Mazurek 1, *, Roman Szostak 1, * , Mateusz Kondratowicz 1 , Magdalena Weglińska 1 , Agnieszka Kita 2 and Agnieszka Nemś 2

  • 13 C nuclear magnetic resonance (NMR) spectra are considered less useful in the analysis of complex multicomponent systems compared to 1 H NMR spectra because of their noticeably lower sensitivity, we demonstrate their utility in the multivariate modeling of selected parameters of such a complicated system

  • The obtained results indicate that 13 C CPMAS NMR spectroscopy can be used to directly quantify nutrients and selected physiochemical parameters of bee pollen samples in their native state

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Summary

13 C NMR Spectra

Sylwester Mazurek 1, *, Roman Szostak 1, * , Mateusz Kondratowicz 1 , Magdalena Weglińska 1 , Agnieszka Kita 2 and Agnieszka Nemś 2.

Introduction
Experimental Material
Reference Analyzes
Chemicals and Reagents
Measurement Conditions
Multivariate Modeling
Software and Numerical Data Treatment
Results and Discussion
Solid-State NMR Spectra
Construction of PLS Models
Nutrients Content Modeling
Modeling of Total Polyphenols Content and Antioxidant Activity
Modeling of pH
Conclusions
Full Text
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