@article{ZhantlessovaSavitskayaKistaubayevaetal.2022, author = {Zhantlessova, Sirina and Savitskaya, Irina and Kistaubayeva, Aida and Ignatova, Ludmila and Talipova, Aizhan and Pogrebnjak, Alexander and Digel, Ilya}, title = {Advanced "Green" prebiotic composite of bacterial cellulose/pullulan based on synthetic biology-powered microbial coculture strategy}, series = {Polymers}, volume = {14}, journal = {Polymers}, number = {15}, publisher = {MDPI}, address = {Basel}, issn = {2073-4360}, doi = {10.3390/polym14153224}, pages = {Artikel 3224}, year = {2022}, abstract = {Bacterial cellulose (BC) is a biopolymer produced by different microorganisms, but in biotechnological practice, Komagataeibacter xylinus is used. The micro- and nanofibrillar structure of BC, which forms many different-sized pores, creates prerequisites for the introduction of other polymers into it, including those synthesized by other microorganisms. The study aims to develop a cocultivation system of BC and prebiotic producers to obtain BC-based composite material with prebiotic activity. In this study, pullulan (PUL) was found to stimulate the growth of the probiotic strain Lactobacillus rhamnosus GG better than the other microbial polysaccharides gellan and xanthan. BC/PUL biocomposite with prebiotic properties was obtained by cocultivation of Komagataeibacter xylinus and Aureobasidium pullulans, BC and PUL producers respectively, on molasses medium. The inclusion of PUL in BC is proved gravimetrically by scanning electron microscopy and by Fourier transformed infrared spectroscopy. Cocultivation demonstrated a composite effect on the aggregation and binding of BC fibers, which led to a significant improvement in mechanical properties. The developed approach for "grafting" of prebiotic activity on BC allows preparation of environmentally friendly composites of better quality.}, language = {en} } @article{DallasSalphatiGomezZepedaetal.2016, author = {Dallas, Shannon and Salphati, Laurent and Gomez-Zepeda, David and Wanek, Thomas and Chen, Liangfu and Chu, Xiaoyan and Kunta, Jeevan and Mezler, Mario and Menet, Marie-Claude and Chasseigneaux, Stephanie and Decl{\`e}ves, Xavier and Langer, Oliver and Pierre, Esaie and DiLoreto, Karen and Hoft, Carolin and Laplanche, Loic and Pang, Jodie and Pereira, Tony and Andonian, Clara and Simic, Damir and Rode, Anja and Yabut, Jocelyn and Zhang, Xiaolin and Scheer, Nico}, title = {Generation and Characterization of a Breast Cancer Resistance Protein Humanized Mouse Model}, series = {Molecular Pharmacology}, volume = {89}, journal = {Molecular Pharmacology}, number = {5}, publisher = {ASPET}, address = {Bethesda, Md.}, issn = {1521-0111}, doi = {10.1124/mol.115.102079}, pages = {492 -- 504}, year = {2016}, abstract = {Breast cancer resistance protein (BCRP) is expressed in various tissues, such as the gut, liver, kidney and blood brain barrier (BBB), where it mediates the unidirectional transport of substrates to the apical/luminal side of polarized cells. Thereby BCRP acts as an efflux pump, mediating the elimination or restricting the entry of endogenous compounds or xenobiotics into tissues and it plays important roles in drug disposition, efficacy and safety. Bcrp knockout mice (Bcrp-/-) have been used widely to study the role of this transporter in limiting intestinal absorption and brain penetration of substrate compounds. Here we describe the first generation and characterization of a mouse line humanized for BCRP (hBCRP), in which the mouse coding sequence from the start to stop codon was replaced with the corresponding human genomic region, such that the human transporter is expressed under control of the murine Bcrp promoter. We demonstrate robust human and loss of mouse BCRP/Bcrp mRNA and protein expression in the hBCRP mice and the absence of major compensatory changes in the expression of other genes involved in drug metabolism and disposition. Pharmacokinetic and brain distribution studies with several BCRP probe substrates confirmed the functional activity of the human transporter in these mice. Furthermore, we provide practical examples for the use of hBCRP mice to study drug-drug interactions (DDIs). The hBCRP mouse is a promising model to study the in vivo role of human BCRP in limiting absorption and BBB penetration of substrate compounds and to investigate clinically relevant DDIs involving BCRP.}, language = {en} } @misc{DuweSchlegelTippkoetteretal.2014, author = {Duwe, A. and Schlegel, C. and Tippk{\"o}tter, Nils and Ulber, Roland}, title = {Sequentielle Extraktion von Cellulose zur effizienten Nutzung der Stoffstr{\"o}me in der Holzbioraffinerie}, series = {Chemie Ingenieur Technik}, volume = {86}, journal = {Chemie Ingenieur Technik}, number = {9}, publisher = {Wiley-VCH}, address = {Weinheim}, issn = {0009-286X}, doi = {10.1002/cite.201450308}, pages = {1400}, year = {2014}, abstract = {In der Reihe der nachwachsenden Rohstoffe besitzt Holz als erneuerbare und umweltfreundliche Ressource ein großes Potenzial. {\"U}ber 11 Mio. ha Holz, das laut der Fachagentur f{\"u}r nachwachsende Rohstoffe (FNR) auch f{\"u}r industrielle Zwecke genutzt werden kann, wuchsen im Jahr 2013 allein auf bundesdeutscher Fl{\"a}che. 56,8 Mio. m³ j{\"a}hrlicher Holzeinschlag in den letzten zehn Jahren wurde zu knapp der H{\"a}lfte stofflich und der Rest energetisch verwertet. Im Rahmen dieser Arbeit konnte auf der Basis vom Holz der Buche, die nach Fichte und Kiefer die dritth{\"a}ufigste Baumart in Deutschland ist und 15\% der deutschen Waldfl{\"a}che ausmacht, die Fraktionierung der polymeren Hauptbestandteile mit niedrigem energetischen Einsatz erreicht werden. Hierbei werden in einem nachgeschalteten Extraktionsprozess die beiden Komponenten Hemicellulose und Lignin in fl{\"u}ssiger Form von der finalen festen Cellulosefraktion abgetrennt. Die Extraktion der Hemicellulose erfolgt durch eine Liquid Hot Water (LHW)-Behandlung. Untersucht wird der katalytische Zusatz anorganischer S{\"a}uren wie H₃PO₄ und H₂SO₄. Im Hinblick auf die weitere Verwertung von Lignin zu aromatischen Synthesebausteinen kommt die Organosolv-Extraktion mit einem Ethanol/Wasser-Gemisch zum Einsatz. Von Vorteil ist die weitere Verwendung beider Stoffstr{\"o}me ohne F{\"a}llungsschritt und nachteiliger Verd{\"u}nnung der Hemicellulose.}, language = {en} } @incollection{HahnKellyMuffleretal.2011, author = {Hahn, Thomas and Kelly, Svenja and Muffler, Kai and Tippk{\"o}tter, Nils and Ulber, Roland}, title = {Extraction of lignocellulose and algae for the production of bulk and fine chemicals}, series = {Industrial scale natural products extraction}, booktitle = {Industrial scale natural products extraction}, editor = {Hans-J{\"o}rg, Bart and Pilz, Stephan}, publisher = {Wiley-VCH}, address = {Weinheim}, isbn = {978-3-527-32504-7 (Print)}, doi = {10.1002/9783527635122}, pages = {221 -- 245}, year = {2011}, language = {en} } @misc{HeringUlberTippkoetter2016, author = {Hering, T. and Ulber, Roland and Tippk{\"o}tter, Nils}, title = {Antimikrobielle Oberfl{\"a}chenmodifikation durch Mikropartikel}, series = {Chemie Ingenieur Technik}, volume = {88}, journal = {Chemie Ingenieur Technik}, number = {9}, publisher = {Wiley-VCH}, address = {Weinheim}, doi = {10.1002/cite.201650084}, pages = {1302}, year = {2016}, abstract = {Die Ausbildung von Biofilmen in technischen Anlagen, wie z. B. K{\"u}hlkreisl{\"a}ufen, Wasseraufbereitungssystemen und Bioreaktoren, f{\"u}hren zu Materialsch{\"a}den (Biofouling) und stark erh{\"o}htem Energieaufwand. Im Rahmen der aktuellen Forschungsarbeiten erfolgen aktive sowie passive Bio-Modifikationen auf funktionalisierten magnetischen Mikropartikelober-fl{\"a}chen. Um die verschiedenen funktionalisierten magnetischen Mikropartikel zu analysieren und ihre antimikrobielle Wirkung zu testen, wird der Einsatz einer 3D-gedruckten, magnetischen Plattform f{\"u}r ein Fluoreszenz-basiertes Screening-System untersucht. F{\"u}r den Oberfl{\"a}chenschutz wurden verschiedene, antimikrobiell funktionalisierte Partikelkombinationen mit dem Mikroorganismus Escherichia coli GFPmut2 in Bezug auf aktiven Oberfl{\"a}chenschutz verglichen. Um die antimikrobielle Oberfl{\"a}cheneffekte von synergistischen Kombinationen unterschiedlich funktionalisierter Partikel zu bestimmen, werden Oberfl{\"a}chen einem Magnetfeld ausgesetzt, das die Mikropartikel als definierte Schicht auf ihnen zur{\"u}ck h{\"a}lt. Diese modifizierten Oberfl{\"a}chen k{\"o}nnen sowohl durch Fluoreszenzspektroskopie als auch -mikroskopie analysiert werden.}, language = {de} } @article{Berndt1979, author = {Berndt, Heinz}, title = {Synthese der Sequenz 71—86 des Humanproinsulins, I : Synthese der Sequenz 71—86 als monomeres cyclisches Biscystinpeptidderivat und als Tetra-S-tritylderivat}, series = {Hoppe-Seyler's Zeitschrift f{\"u}r physiologische Chemie}, volume = {360}, journal = {Hoppe-Seyler's Zeitschrift f{\"u}r physiologische Chemie}, number = {1}, issn = {1437-4315}, doi = {10.1515/bchm2.1979.360.1.747}, pages = {747 -- 760}, year = {1979}, language = {de} } @misc{EngelTippkoetter2016, author = {Engel, M. and Tippk{\"o}tter, Nils}, title = {Einfluss eines Phenazin-Mediators und elektrischen Potenzials auf die Aceton-Butanol-Ethanol-Fermentation}, series = {Chemie Ingenieur Technik}, volume = {88}, journal = {Chemie Ingenieur Technik}, number = {9}, publisher = {Wiley-VCH}, address = {Weinheim}, issn = {0009-286X}, doi = {10.1002/cite.201650105}, pages = {1254}, year = {2016}, abstract = {In den letzten Jahren haben nachhaltige, biotechnologische Prozesse zunehmend an Bedeutung gewonnen. Die Aceton-Butanol-Ethanol-Fermentation (ABE-Fermentation) mit dem anaeroben Bakterium Clostridium acetobutylicum zur Gewinnung von Biobutanol k{\"o}nnte in diesem Zusammenhang eine M{\"o}glichkeit der nachhaltigen Kraftstoffproduktion darstellen. In dieser Arbeit wird der Einfluss zus{\"a}tzlich verf{\"u}gbarer Elektronen durch den Einsatz des Phenazin-Farbstoffs Neutralrot als Redoxmediator sowie das Anlegen eines elektrischen Potenzials w{\"a}hrend der ABE-Fermentation untersucht. Es wird gezeigt, dass das Neutralrot keinen Einfluss auf die Leerlaufspannung von ca. 500 mV vs. Ag/AgCl w{\"a}hrend der Fermentation hat. Der Mediator bewirkt allerdings eine fr{\"u}here Butanolbildung sowie h{\"o}here Butanolkonzentrationen. Wird zudem die Mediatorkonzentration von 125 mM auf 250 mM angehoben, wird dabei auch die maximale Butanolkonzentration um 36 \% ± 1,8 \% innerhalb von28 Stunden gesteigert.}, language = {de} } @misc{SiekerTippkoetterUlber2010, author = {Sieker, T. and Tippk{\"o}tter, Nils and Ulber, Roland}, title = {Simultane Vorbehandlung, Hydrolyse und Fermentation bei der Nutzung von gr{\"u}ner Biomasse zur Produktion von Bioethanol}, series = {Chemie Ingenieur Technik}, volume = {82}, journal = {Chemie Ingenieur Technik}, number = {9}, publisher = {Wiley-VCH}, address = {Weinheim}, issn = {0009-286X}, doi = {10.1002/cite.201050319}, pages = {1601}, year = {2010}, abstract = {Gr{\"a}ser sind in der Lage, einen großen Teil der f{\"u}r eine biobasierte Wirtschaft ben{\"o}tigten Biomasse zur Verf{\"u}gung zu stellen. Wie bei anderen lignocellulosehaltigen nachwachsenden Rohstoffen erfordert die Verwertung der im Gras enthaltenen Polysaccharide einen mehrstufigen Prozess aus Vorbehandlung, Hydrolyse und Fermentation. In Gr{\"a}sern ist die Hemicellulose mitP henolcarbons{\"a}uren wie Ferula- und p-Coumars{\"a}ure verestert, die die enzymatische Hydrolyse der Cellulose und Hemicellulose ebenso effektiv behindern wie Lignin. Anders als bei holzigen Rohstoffen erm{\"o}glicht dieser Aufbau aber eine enzymatische Vorbehandlung, mit der die Phenolcarbons{\"a}uren abgespalten werden k{\"o}nnen. Da die bei der Vorbehandlung eingesetzten Enzyme in ihrer nat{\"u}rlichen Funktion synergistisch mit cellulytischen Enzymen zusammenarbeiten, besitzen sie {\"a}hnliche Optima wie die f{\"u}r die Hydrolyse der Polysaccharide eingesetzten Cellulasen und Hemicellulasen. Diese Eigenschaft erm{\"o}glicht die Integration von Vorbehandlung und Hydrolyse in einem einzigen Verfahrensschritt. Durch die Einf{\"u}hrung der enzymatischen Vorbehandlung konnte das in der Literatur bekannte SSF-Verfahren f{\"u}r die Herstellung von Ethanol aus Gr{\"a}sern um die Vorbehandlungsstufe erweitert werden. Das so realisierte simultaneous pretreatment, saccharification and fermentation (SPSF)-Verfahren stellt eine vollst{\"a}ndige Integration der drei f{\"u}r die Nutzung von Lignocellulose n{\"o}tigen Verfahrensschritte in der gr{\"u}nen Bioraffinerie dar.}, language = {de} } @article{AlKaidyDuweHusteretal.2014, author = {Al-Kaidy, Huschyar and Duwe, Anna and Huster, Manuel and Muffler, Kai and Schlegel, Christin and Sieker, Tim and Stadtm{\"u}ller, Ralf and Tippk{\"o}tter, Nils and Ulber, Roland}, title = {Biotechnologie und Bioverfahrenstechnik - Vom ersten Ullmanns Artikel bis hin zu aktuellen Forschungsthemen}, series = {Chemie Ingenieur Technik}, volume = {86}, journal = {Chemie Ingenieur Technik}, number = {12}, publisher = {Wiley-VCH}, address = {Weinheim}, issn = {0009-286X}, doi = {10.1002/cite.201400083}, pages = {2215 -- 2225}, year = {2014}, abstract = {Biotechnologie und die mit ihr verbundenen technischen Prozesse pr{\"a}gen seit Jahrtausenden die Entwicklung der Menschheit. Ausgehend von empirischen Verfahren, insbesondere zur Herstellung von Lebensmitteln und t{\"a}glichen Gebrauchsg{\"u}tern, haben sich diese Disziplinen zu einem der innovativsten Zukunftsfelder entwickelt. Durch das immer detailliertere Verst{\"a}ndnis zellul{\"a}rer Vorg{\"a}nge k{\"o}nnen mittlerweile Produktionsst{\"a}mme gezielt optimiert werden. Im Zusammenspiel mit moderner Prozesstechnik k{\"o}nnen so eine Vielzahl von Bulk- und Feinchemikalien sowie Pharmazeutika effizient hergestellt werden. In diesem Artikel werden exemplarisch einige der aktuellen Trends vorgestellt.}, language = {de} } @article{UndenBeckerBongaertsetal.1994, author = {Unden, G. and Becker, S. and Bongaerts, Johannes and Schirawski, J. and Six, S.}, title = {Oxygen regulated gene expression in facultatively anaerobic bacteria}, series = {Antonie van Leeuwenhoek}, volume = {Vol. 66}, journal = {Antonie van Leeuwenhoek}, number = {Iss. 1-3}, issn = {0003-6072 (Print) ; 1572-9699 (online)}, pages = {3 -- 22}, year = {1994}, language = {en} } @article{PasteurTippkoetterKampeisetal.2014, author = {Pasteur, Aline and Tippk{\"o}tter, Nils and Kampeis, Percy and Ulber, Roland}, title = {Optimization of high gradient magnetic separation filter units for the purification of fermentation products}, series = {IEEE TRANSACTIONS ON MAGNETICS}, volume = {50}, journal = {IEEE TRANSACTIONS ON MAGNETICS}, number = {10}, publisher = {IEEE}, address = {New York, NY}, issn = {0018-9464}, doi = {10.1109/TMAG.2014.2325535}, pages = {Artikel 5000607}, year = {2014}, abstract = {High gradient magnetic separation (HGMS) has been established since the early 1970s. A more recent application of these systems is the use in bioprocesses. To integrate the HGMS in a fermentation process, it is necessary to optimize the separation matrix with regard to the magnetic separation characteristics and permeability of the non-magnetizable components of the fermentation broth. As part of the work presented here, a combined fluidic and magnetic force finite element model simulation was created using the software COMSOL Multiphysics and compared with separation experiments. Finally, as optimal lattice orientation of the separation matrix, a transversal rhombohedral arrangement was defined. The high suitability of the new filter matrix has been verified by separation experiments.}, language = {en} } @article{UlberTippkoetter2009, author = {Ulber, Roland and Tippk{\"o}tter, Nils}, title = {Nitratfreie Molke}, series = {Rundschau f{\"u}r Fleischhygiene und Lebensmittel{\"u}berwachung}, journal = {Rundschau f{\"u}r Fleischhygiene und Lebensmittel{\"u}berwachung}, number = {4}, pages = {150 -- 152}, year = {2009}, language = {de} } @misc{AlKaidyTippkoetterUlber2013, author = {Al-Kaidy, Huschyar and Tippk{\"o}tter, Nils and Ulber, Roland}, title = {A system and a method for the implementation of chemical, biological or physical reactions [Europ{\"a}ische Patentanmeldung]}, publisher = {Europ{\"a}isches Patentamt}, address = {Den Hague}, pages = {16 Seiten}, year = {2013}, abstract = {The invention relates to a system for the implementation of chemical, biological or physical reactions, consisting of - one or more magnetic micro-reactors, each comprising a shell made of hydrophobic magnetic nanoparticles encapsulating an aqueous core, - a plane platform comprising a surface to receive the micro-reactors, - a source that generates a magnetic field above or underneath the platform for manipulating the one or more hydrophobic magnetic micro-reactors, or for moving them along the surface of the platform from one position to another position, characterized in that the aqueous core of the one or more magnetic micro-reactors contains a reaction solution or buffer, and wherein the magnetic field generated by the source correlates to a defined position on the surface of the platform.}, language = {en} } @article{WiesenTippkoetterMuffleretal.2015, author = {Wiesen, Sebastian and Tippk{\"o}tter, Nils and Muffler, Kai and Suck, Kirstin and Sohling, Ulrich and Ruf, Friedrich and Ulber, Roland}, title = {Adsorption of fatty acids to layered double hydroxides in aqueous systems}, series = {Adsorption}, volume = {21}, journal = {Adsorption}, number = {6-7}, publisher = {Springer}, address = {Berlin}, pages = {459 -- 466}, year = {2015}, abstract = {Due to their anion exchange characteristics, layered double hydroxides (LDHs) are suitable for the detoxification of aqueous, fatty acid containing fermentation substrates. The aim of this study is to examine the adsorption mechanism, using crude glycerol from plant oil esterification as a model system. Changes in the intercalation structure in relation to the amount of fatty acids adsorbed are monitored by X-ray diffraction and infra-red spectroscopy. Additionally, calcination of LDH is investigated in order to increase the binding capacity for fatty acids. Our data propose that, at ambient temperature, fatty acids can be bound to the hydrotalcite by adsorption or in addition by intercalation, depending on fatty acid concentration. The adsorption of fatty acids from crude glycerol shows a BET-like behavior. Above a fatty acid concentration of 3.5 g L-1, intercalation of fatty acids can be shown by the appearance of an increased interlayer spacing. This observation suggests a two phase adsorption process. Calcination of LDHs allows increasing the binding capacity for fatty acids by more than six times, mainly by reduction of structural CO32-.}, language = {en} } @article{MuesgenanntKoersPrevostPaulssenetal.2023, author = {Mues genannt Koers, Lucas and Prevost, David and Paulßen, Elisabeth and Hoehr, Cornelia}, title = {Density reduction effects on the production of [11C]CO2 in Nb-body targets on a medical cyclotron}, volume = {199}, number = {Art. 110911}, publisher = {Elsevier}, address = {Amsterdam}, doi = {10.1016/j.apradiso.2023.110911}, year = {2023}, abstract = {Medical isotope production of 11C is commonly performed in gaseous targets. The power deposition of the proton beam during the irradiation decreases the target density due to thermodynamic mixing and can cause an increase of penetration depth and divergence of the proton beam. In order to investigate the difference how the target-body length influences the operation conditions and the production yield, a 12 cm and a 22 cm Nb-target body containing N2/O2 gas were irradiated using a 13 MeV proton cyclotron. It was found that the density reduction has a large influence on the pressure rise during irradiation and the achievable radioactive yield. The saturation activity of [11C]CO2 for the long target (0.083 Ci/μA) is about 10\% higher than in the short target geometry (0.075 Ci/μA).}, language = {en} } @article{BergsMonakhovaDiehletal.2021, author = {Bergs, Michel and Monakhova, Yulia and Diehl, Bernd W. and Konow, Christopher and V{\"o}lkering, Georg and Pude, Ralf and Schulze, Margit}, title = {Lignins isolated via catalyst-free organosolv pulping from Miscanthus x giganteus, M. sinensis, M. robustus and M. nagara: a comparative study}, series = {Molecules}, volume = {26}, journal = {Molecules}, number = {4}, publisher = {MDPI}, address = {Basel}, issn = {1420-3049}, doi = {10.3390/molecules26040842}, year = {2021}, abstract = {As a low-input crop, Miscanthus offers numerous advantages that, in addition to agricultural applications, permits its exploitation for energy, fuel, and material production. Depending on the Miscanthus genotype, season, and harvest time as well as plant component (leaf versus stem), correlations between structure and properties of the corresponding isolated lignins differ. Here, a comparative study is presented between lignins isolated from M. x giganteus, M. sinensis, M. robustus and M. nagara using a catalyst-free organosolv pulping process. The lignins from different plant constituents are also compared regarding their similarities and differences regarding monolignol ratio and important linkages. Results showed that the plant genotype has the weakest influence on monolignol content and interunit linkages. In contrast, structural differences are more significant among lignins of different harvest time and/or season. Analyses were performed using fast and simple methods such as nuclear magnetic resonance (NMR) spectroscopy. Data was assigned to four different linkages (A: β-O-4 linkage, B: phenylcoumaran, C: resinol, D: β-unsaturated ester). In conclusion, A content is particularly high in leaf-derived lignins at just under 70\% and significantly lower in stem and mixture lignins at around 60\% and almost 65\%. The second most common linkage pattern is D in all isolated lignins, the proportion of which is also strongly dependent on the crop portion. Both stem and mixture lignins, have a relatively high share of approximately 20\% or more (maximum is M. sinensis Sin2 with over 30\%). In the leaf-derived lignins, the proportions are significantly lower on average. Stem samples should be chosen if the highest possible lignin content is desired, specifically from the M. x giganteus genotype, which revealed lignin contents up to 27\%. Due to the better frost resistance and higher stem stability, M. nagara offers some advantages compared to M. x giganteus. Miscanthus crops are shown to be very attractive lignocellulose feedstock (LCF) for second generation biorefineries and lignin generation in Europe.}, language = {en} } @article{BurgerRumpfDoetal.2021, author = {Burger, Ren{\´e} and Rumpf, Jessica and Do, Xuan Tung and Monakhova, Yulia and Diehl, Bernd W. K. and Rehahn, Matthias and Schulze, Margit}, title = {Is NMR combined with multivariate regression applicable for the molecular weight determination of randomly cross-linked polymers such as lignin?}, series = {ACS Omega}, volume = {6}, journal = {ACS Omega}, number = {44}, publisher = {ACS Publications}, address = {Washington, DC}, issn = {2470-1343}, doi = {10.1021/acsomega.1c03574}, pages = {29516 -- 29524}, year = {2021}, abstract = {The molecular weight properties of lignins are one of the key elements that need to be analyzed for a successful industrial application of these promising biopolymers. In this study, the use of 1H NMR as well as diffusion-ordered spectroscopy (DOSY NMR), combined with multivariate regression methods, was investigated for the determination of the molecular weight (Mw and Mn) and the polydispersity of organosolv lignins (n = 53, Miscanthus x giganteus, Paulownia tomentosa, and Silphium perfoliatum). The suitability of the models was demonstrated by cross validation (CV) as well as by an independent validation set of samples from different biomass origins (beech wood and wheat straw). CV errors of ca. 7-9 and 14-16\% were achieved for all parameters with the models from the 1H NMR spectra and the DOSY NMR data, respectively. The prediction errors for the validation samples were in a similar range for the partial least squares model from the 1H NMR data and for a multiple linear regression using the DOSY NMR data. The results indicate the usefulness of NMR measurements combined with multivariate regression methods as a potential alternative to more time-consuming methods such as gel permeation chromatography.}, language = {en} } @article{MonakhovaDiehl2022, author = {Monakhova, Yulia and Diehl, Bernd W.K.}, title = {Nuclear magnetic resonance spectroscopy as an elegant tool for a complete quality control of crude heparin material}, series = {Journal of Pharmaceutical and Biomedical Analysis}, volume = {219}, journal = {Journal of Pharmaceutical and Biomedical Analysis}, number = {Article number: 114915}, publisher = {Elsevier}, address = {New York, NY}, issn = {0731-7085}, doi = {10.1016/j.jpba.2022.114915}, year = {2022}, abstract = {Nuclear magnetic resonance (NMR) spectrometric methods for the quantitative analysis of pure heparin in crude heparin is proposed. For quantification, a two-step routine was developed using a USP heparin reference sample for calibration and benzoic acid as an internal standard. The method was successfully validated for its accuracy, reproducibility, and precision. The methodology was used to analyze 20 authentic porcine heparinoid samples having heparin content between 4.25 w/w \% and 64.4 w/w \%. The characterization of crude heparin products was further extended to a simultaneous analysis of these common ions: sodium, calcium, acetate and chloride. A significant, linear dependence was found between anticoagulant activity and assayed heparin content for thirteen heparinoids samples, for which reference data were available. A Diffused-ordered NMR experiment (DOSY) can be used for qualitative analysis of specific glycosaminoglycans (GAGs) in heparinoid matrices and, potentially, for quantitative prediction of molecular weight of GAGs. NMR spectrometry therefore represents a unique analytical method suitable for the simultaneous quantitative control of organic and inorganic composition of crude heparin samples (especially heparin content) as well as an estimation of other physical and quality parameters (molecular weight, animal origin and activity).}, language = {en} } @article{MonakhovaDiehl2021, author = {Monakhova, Yulia and Diehl, Bernd W. K.}, title = {Simplification of NMR Workflows by Standardization Using 2H Integral of Deuterated Solvent as Applied to Aloe vera Preparations}, series = {Applied Magnetic Resonance}, volume = {52}, journal = {Applied Magnetic Resonance}, number = {11}, publisher = {Springer}, address = {Cham}, issn = {1613-7507}, doi = {10.1007/s00723-021-01393-4}, pages = {1591 -- 1600}, year = {2021}, abstract = {In this study, a recently proposed NMR standardization approach by 2H integral of deuterated solvent for quantitative multicomponent analysis of complex mixtures is presented. As a proof of principle, the existing NMR routine for the analysis of Aloe vera products was modified. Instead of using absolute integrals of targeted compounds and internal standard (nicotinamide) from 1H-NMR spectra, quantification was performed based on the ratio of a particular 1H-NMR compound integral and 2H-NMR signal of deuterated solvent D2O. Validation characteristics (linearity, repeatability, accuracy) were evaluated and the results showed that the method has the same precision as internal standardization in case of multicomponent screening. Moreover, a dehydration process by freeze drying is not necessary for the new routine. Now, our NMR profiling of A. vera products needs only limited sample preparation and data processing. The new standardization methodology provides an appealing alternative for multicomponent NMR screening. In general, this novel approach, using standardization by 2H integral, benefits from reduced sample preparation steps and uncertainties, and is recommended in different application areas (purity determination, forensics, pharmaceutical analysis, etc.).}, language = {en} } @article{AdelsMonakhova2024, author = {Adels, Klaudia and Monakhova, Yulia}, title = {Low-field NMR spectroscopic study of e-cigarettes: Is determination of only nicotine and organic carrier solvents possible?}, series = {Microchemical Journal}, volume = {203}, journal = {Microchemical Journal}, publisher = {Elsevier}, address = {Amsterdam}, issn = {1095-9149}, doi = {10.1016/j.microc.2024.110859}, pages = {9 Seiten}, year = {2024}, abstract = {Electronic cigarettes (e-cigarettes) have become popular worldwide with the market growing exponentially in some countries. The absence of product standards and safety regulations requires urgent development of analytical methodologies for the holistic control of the growing diversity of such products. An approach based on low-field nuclear magnetic resonance (LF-NMR) at 80 MHz is presented for the simultaneous determination of key parameters: carrier solvents (vegetable glycerine (VG), propylene glycol (PG) and water), total nicotine as well as free-base nicotine fraction. Moreover, qualitative and quantitative determination of fourteen weak organic acids deliberately added to enhance sensory characteristics of e-cigarettes was possible. In most cases these parameters can be rapidly and conveniently determined without using any sample manipulation such as dilution, extraction or derivatization steps. The method was applied for 37 authentic e-cigarettes samples. In particular, eight different organic acids with the content up to 56 mg/mL were detected. Due to its simplicity, the method can be used in routine regulatory control as well as to study release behaviour of nicotine and other e-cigarettes constituents in different products.}, language = {en} }