@article{AdelsElbersDiehletal.2023,
  author    = {Adels, Klaudia and Elbers, Gereon and Diehl, Bernd and Monakhova, Yulia},
  title     = {Multicomponent analysis of dietary supplements containing glucosamine and chondroitin: comparative low- and high-field NMR spectroscopic study},
  series = {Analytical Sciences},
  volume    = {2023},
  journal   = {Analytical Sciences},
  publisher = {Springer Verlag},
  address   = {Cham},
  issn      = {1348-2246 (Online)},
  doi       = {10.1007/s44211-023-00433-2},
  pages     = {13 Seiten},
  year      = {2023},
  abstract  = {With the prevalence of glucosamine- and chondroitin-containing dietary supplements for people with osteoarthritis in the marketplace, it is important to have an accurate and reproducible analytical method for the quantitation of these compounds in finished products. NMR spectroscopic method based both on low- (80 MHz) and high- (500-600 MHz) field NMR instrumentation was established, compared and validated for the determination of chondroitin sulfate and glucosamine in dietary supplements. The proposed method was applied for analysis of 20 different dietary supplements. In the majority of cases, quantification results obtained on the low-field NMR spectrometer are similar to those obtained with high-field 500-600 MHz NMR devices. Validation results in terms of accuracy, precision, reproducibility, limit of detection and recovery demonstrated that the developed method is fit for purpose for the marketed products. The NMR method was extended to the analysis of methylsulfonylmethane, adulterant maltodextrin, acetate and inorganic ions. Low-field NMR can be a quicker and cheaper alternative to more expensive high-field NMR measurements for quality control of the investigated dietary supplements. High-field NMR instrumentation can be more favorable for samples with complex composition due to better resolution, simultaneously giving the possibility of analysis of inorganic species such as potassium and chloride.},
  language  = {en}
}
@article{BlockMayWetzeletal.2023,
  author    = {Block, Franziska and May, Alexander and Wetzel, Katharina and Adels, Klaudia and Elbers, Gereon and Schulze, Margit and Monakhova, Yulia},
  title     = {What is the best spectroscopic method for simultaneous analysis of organic acids and (poly)saccharides in biological matrices: Example of Aloe vera extracts?},
  series = {Talanta Open},
  volume    = {7},
  journal   = {Talanta Open},
  number    = {Art. No. 100220},
  publisher = {Elsevier},
  address   = {Amsterdam},
  issn      = {2666-8319},
  doi       = {10.1016/j.talo.2023.100220},
  pages     = {1 -- 9},
  year      = {2023},
  abstract  = {Several species of (poly)saccharides and organic acids can be found often simultaneously in various biological matrices, e.g., fruits, plant materials, and biological fluids. The analysis of such matrices sometimes represents a challenging task. Using Aloe vera (A. vera) plant materials as an example, the performance of several spectro-scopic methods (80 MHz benchtop NMR, NIR, ATR-FTIR and UV-vis) for the simultaneous analysis of quality parameters of this plant material was compared. The determined parameters include (poly)saccharides such as aloverose, fructose and glucose as well as organic acids (malic, lactic, citric, isocitric, acetic, fumaric, benzoic and sorbic acids). 500 MHz NMR and high-performance liquid chromatography (HPLC) were used as the reference methods. UV-vis data can be used only for identification of added preservatives (benzoic and sorbic acids) and drying agent (maltodextrin) and semiquantitative analysis of malic acid. NIR and MIR spectroscopies combined with multivariate regression can deliver more informative overview of A. vera extracts being able to additionally quantify glucose, aloverose, citric, isocitric, malic, lactic acids and fructose. Low-field NMR measurements can be used for the quantification of aloverose, glucose, malic, lactic, acetic, and benzoic acids. The benchtop NMR method was successfully validated in terms of robustness, stability, precision, reproducibility and limit of detection (LOD) and quantification (LOQ), respectively. All spectroscopic techniques are useful for the screening of (poly)saccharides and organic acids in plant extracts and should be applied according to its availability as well as information and confidence required for the specific analytical goal. Benchtop NMR spectroscopy seems to be the most feasible solution for quality control of A. vera products.},
  language  = {en}
}
@article{MonakhovaDiehl2021,
  author    = {Monakhova, Yulia and Diehl, Bernd W. K.},
  title     = {A step towards optimization of the qNMR workflow: proficiency testing exercise at an GxP-accredited laboratory},
  series = {Applied Magnetic Resonance},
  volume    = {52},
  journal   = {Applied Magnetic Resonance},
  publisher = {Springer Nature},
  address   = {Wien},
  issn      = {1613-7507},
  doi       = {10.1007/s00723-021-01324-3},
  pages     = {581 -- 593},
  year      = {2021},
  abstract  = {Quantitative nuclear magnetic resonance (qNMR) is considered as a powerful tool for multicomponent mixture analysis as well as for the purity determination of single compounds. Special attention is currently paid to the training of operators and study directors involved in qNMR testing. To assure that only qualified personnel are used for sample preparation at our GxP-accredited laboratory, weighing test was proposed. Sixteen participants performed six-fold weighing of the binary mixture of dibutylated hydroxytoluene (BHT) and 1,2,4,5-tetrachloro-3-nitrobenzene (TCNB). To evaluate the quality of data analysis, all spectra were evaluated manually by a qNMR expert and using in-house developed automated routine. The results revealed that mean values are comparable and both evaluation approaches are free of systematic error. However, automated evaluation resulted in an approximately 20\% increase in precision. The same findings were revealed for qNMR analysis of 32 compounds used in pharmaceutical industry. Weighing test by six-fold determination in binary mixtures and automated qNMR methodology can be recommended as efficient tools for evaluating staff proficiency. The automated qNMR method significantly increases throughput and precision of qNMR for routine measurements and extends application scope of qNMR.},
  language  = {en}
}