@article{RothTippkoetter2016, author = {Roth, Jasmine and Tippk{\"o}tter, Nils}, title = {Evaluation of lignocellulosic material for butanol production using enzymatic hydrolysate medium}, series = {Cellulose Chemistry and Technology}, volume = {50}, journal = {Cellulose Chemistry and Technology}, number = {3-4}, publisher = {Editura Academiei Romane}, address = {Bukarest}, pages = {405 -- 410}, year = {2016}, abstract = {Butanol is a promising gasoline additive and platform chemical that can be readily produced via acetone-butanolethanol (ABE) fermentation from pretreated lignocellulosic materials. This article examines lignocellulosic material from beech wood for ABE fermentation, using Clostridium acetobutylicum. First, the utilization of both C₅₋ (xylose) and C₆₋ (glucose) sugars as sole carbon source was investigated in static cultivation, using serum bottles and synthetic medium. The utilization of pentose sugar resulted in a solvent yield of 0.231 g·g_sugar⁻¹, compared to 0.262 g·g_sugar⁻¹ using hexose. Then, the Organosolv pretreated crude cellulose fibers (CF) were enzymatically decomposed, and the resulting hydrolysate medium was analyzed for inhibiting compounds (furans, organic acids, phenolics) and treated with ionexchangers for detoxification. Batch fermentation in a bioreactor using CF hydrolysate medium resulted in a total solvent yield of 0.20 gABE·g_sugar⁻¹.}, language = {en} } @article{BechtSchollmayerMonakhovaetal.2021, author = {Becht, Alexander and Schollmayer, Curd and Monakhova, Yulia and Holzgrabe, Ulrike}, title = {Tracing the origin of paracetamol tablets by near-infrared, mid-infrared, and nuclear magnetic resonance spectroscopy using principal component analysis and linear discriminant analysis}, series = {Analytical and Bioanalytical Chemistry}, volume = {413}, journal = {Analytical and Bioanalytical Chemistry}, publisher = {Springer Nature}, issn = {1618-2650}, doi = {10.1007/s00216-021-03249-z}, pages = {3107 -- 3118}, year = {2021}, abstract = {Most drugs are no longer produced in their own countries by the pharmaceutical companies, but by contract manufacturers or at manufacturing sites in countries that can produce more cheaply. This not only makes it difficult to trace them back but also leaves room for criminal organizations to fake them unnoticed. For these reasons, it is becoming increasingly difficult to determine the exact origin of drugs. The goal of this work was to investigate how exactly this is possible by using different spectroscopic methods like nuclear magnetic resonance and near- and mid-infrared spectroscopy in combination with multivariate data analysis. As an example, 56 out of 64 different paracetamol preparations, collected from 19 countries around the world, were chosen to investigate whether it is possible to determine the pharmaceutical company, manufacturing site, or country of origin. By means of suitable pre-processing of the spectra and the different information contained in each method, principal component analysis was able to evaluate manufacturing relationships between individual companies and to differentiate between production sites or formulations. Linear discriminant analysis showed different results depending on the spectral method and purpose. For all spectroscopic methods, it was found that the classification of the preparations to their manufacturer achieves better results than the classification to their pharmaceutical company. The best results were obtained with nuclear magnetic resonance and near-infrared data, with 94.6\%/99.6\% and 98.7/100\% of the spectra of the preparations correctly assigned to their pharmaceutical company or manufacturer.}, language = {en} } @article{LindnerBurgerRutledgeetal.2022, author = {Lindner, Simon and Burger, Ren{\´e} and Rutledge, Douglas N. and Do, Xuan Tung and Rumpf, Jessica and Diehl, Bernd W. K. and Schulze, Margit and Monakhova, Yulia}, title = {Is the calibration transfer of multivariate calibration models between high- and low-field NMR instruments possible? A case study of lignin molecular weight}, series = {Analytical chemistry}, volume = {94}, journal = {Analytical chemistry}, number = {9}, publisher = {ACS Publications}, address = {Washington, DC}, isbn = {1520-6882}, doi = {10.1021/acs.analchem.1c05125}, pages = {3997 -- 4004}, year = {2022}, abstract = {Although several successful applications of benchtop nuclear magnetic resonance (NMR) spectroscopy in quantitative mixture analysis exist, the possibility of calibration transfer remains mostly unexplored, especially between high- and low-field NMR. This study investigates for the first time the calibration transfer of partial least squares regressions [weight average molecular weight (Mw) of lignin] between high-field (600 MHz) NMR and benchtop NMR devices (43 and 60 MHz). For the transfer, piecewise direct standardization, calibration transfer based on canonical correlation analysis, and transfer via the extreme learning machine auto-encoder method are employed. Despite the immense resolution difference between high-field and low-field NMR instruments, the results demonstrate that the calibration transfer from high- to low-field is feasible in the case of a physical property, namely, the molecular weight, achieving validation errors close to the original calibration (down to only 1.2 times higher root mean square errors). These results introduce new perspectives for applications of benchtop NMR, in which existing calibrations from expensive high-field instruments can be transferred to cheaper benchtop instruments to economize.}, language = {en} } @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{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} }