@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{CheenakulaPaulsenOttetal.2023, author = {Cheenakula, Dheeraja and Paulsen, Svea and Ott, Fabian and Gr{\"o}mping, Markus}, title = {Operational window of a deammonifying sludge for mainstream application in a municipal wastewater treatment plant}, series = {Water and Environment Journal}, volume = {38}, journal = {Water and Environment Journal}, number = {1}, publisher = {Wiley}, address = {Chichester}, issn = {1747-6593}, doi = {10.1111/wej.12898}, pages = {59 -- 70}, year = {2023}, abstract = {The present work aimed to study the mainstream feasibility of the deammonifying sludge of side stream of municipal wastewater treatment plant (MWWTP) in Kaster, Germany. For this purpose, the deammonifying sludge available at the side stream was investigated for nitrogen (N) removal with respect to the operational factors temperature (15-30°C), pH value (6.0-8.0) and chemical oxygen demand (COD)/N ratio (≤1.5-6.0). The highest and lowest N-removal rates of 0.13 and 0.045 kg/(m³ d) are achieved at 30 and 15°C, respectively. Different conditions of pH and COD/N ratios in the SBRs of Partial nitritation/anammox (PN/A) significantly influenced both the metabolic processes and associated N-removal rates. The scientific insights gained from the current work signifies the possibility of mainstream PN/A at WWTPs. The current study forms a solid basis of operational window for the upcoming semi-technical trails to be conducted prior to the full-scale mainstream PN/A at WWTP Kaster and WWTPs globally.}, language = {en} } @article{PourshahidiEngelmannOffenhaeusseretal.2022, author = {Pourshahidi, Ali Mohammad and Engelmann, Ulrich M. and Offenh{\"a}usser, Andreas and Krause, Hans-Joachim}, title = {Resolving ambiguities in core size determination of magnetic nanoparticles from magnetic frequency mixing data}, series = {Journal of Magnetism and Magnetic Materials}, volume = {563}, journal = {Journal of Magnetism and Magnetic Materials}, number = {In progress, Art. No. 169969}, publisher = {Elsevier}, address = {Amsterdam}, issn = {0304-8853}, doi = {10.1016/j.jmmm.2022.169969}, year = {2022}, abstract = {Frequency mixing magnetic detection (FMMD) has been widely utilized as a measurement technique in magnetic immunoassays. It can also be used for the characterization and distinction (also known as "colourization") of different types of magnetic nanoparticles (MNPs) based on their core sizes. In a previous work, it was shown that the large particles contribute most of the FMMD signal. This leads to ambiguities in core size determination from fitting since the contribution of the small-sized particles is almost undetectable among the strong responses from the large ones. In this work, we report on how this ambiguity can be overcome by modelling the signal intensity using the Langevin model in thermodynamic equilibrium including a lognormal core size distribution fL(dc,d0,σ) fitted to experimentally measured FMMD data of immobilized MNPs. For each given median diameter d0, an ambiguous amount of best-fitting pairs of parameters distribution width σ and number of particles Np with R2 > 0.99 are extracted. By determining the samples' total iron mass, mFe, with inductively coupled plasma optical emission spectrometry (ICP-OES), we are then able to identify the one specific best-fitting pair (σ, Np) one uniquely. With this additional externally measured parameter, we resolved the ambiguity in core size distribution and determined the parameters (d0, σ, Np) directly from FMMD measurements, allowing precise MNPs sample characterization.}, 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{RabehiGarlanAchtsnichtetal.2018, author = {Rabehi, Amine and Garlan, Benjamin and Achtsnicht, Stefan and Krause, Hans-Joachim and Offenh{\"a}usser, Andreas and Ngo, Kieu and Neveu, Sophie and Graff-Dubois, Stephanie and Kokabi, Hamid}, title = {Magnetic detection structure for Lab-on-Chip applications based on the frequency mixing technique}, series = {Sensors}, volume = {18}, journal = {Sensors}, number = {6}, publisher = {MDPI}, address = {Basel}, issn = {1424-8220}, doi = {10.3390/s18061747}, pages = {14 Seiten}, year = {2018}, abstract = {A magnetic frequency mixing technique with a set of miniaturized planar coils was investigated for use with a completely integrated Lab-on-Chip (LoC) pathogen sensing system. The system allows the detection and quantification of superparamagnetic beads. Additionally, in terms of magnetic nanoparticle characterization ability, the system can be used for immunoassays using the beads as markers. Analytical calculations and simulations for both excitation and pick-up coils are presented; the goal was to investigate the miniaturization of simple and cost-effective planar spiral coils. Following these calculations, a Printed Circuit Board (PCB) prototype was designed, manufactured, and tested for limit of detection, linear response, and validation of theoretical concepts. Using the magnetic frequency mixing technique, a limit of detection of 15 µg/mL of 20 nm core-sized nanoparticles was achieved without any shielding.}, language = {en} } @article{AchtsnichtNeuendorfFassbenderetal.2019, author = {Achtsnicht, Stefan and Neuendorf, Christian and Faßbender, Tobias and N{\"o}lke, Greta and Offenh{\"a}usser, Andreas and Krause, Hans-Joachim and Schr{\"o}per, Florian}, title = {Sensitive and rapid detection of cholera toxin subunit B using magnetic frequency mixing detection}, series = {Plos One}, volume = {14}, journal = {Plos One}, number = {7}, publisher = {Plos}, address = {San Francisco}, issn = {1932-6203}, doi = {10.1371/journal.pone.0219356}, pages = {e0219356}, year = {2019}, abstract = {Cholera is a life-threatening disease caused by the cholera toxin (CT) as produced by some Vibrio cholerae serogroups. In this research we present a method which directly detects the toxin's B subunit (CTB) in drinking water. For this purpose we performed a magnetic sandwich immunoassay inside a 3D immunofiltration column. We used two different commercially available antibodies to capture CTB and for binding to superparamagnetic beads. ELISA experiments were performed to select the antibody combination. The beads act as labels for the magnetic frequency mixing detection technique. We show that the limit of detection depends on the type of magnetic beads. A nonlinear Hill curve was fitted to the calibration measurements by means of a custom-written python software. We achieved a sensitive and rapid detection of CTB within a broad concentration range from 0.2 ng/ml to more than 700 ng/ml.}, language = {en} } @article{AchtsnichtSchoenenbornOffenhaeusseretal.2019, author = {Achtsnicht, Stefan and Sch{\"o}nenborn, Kristina and Offenh{\"a}usser, Andreas and Krause, Hans-Joachim}, title = {Measurement of the magnetophoretic velocity of different superparamagnetic beads}, series = {Journal of Magnetism and Magnetic Materials}, volume = {477}, journal = {Journal of Magnetism and Magnetic Materials}, number = {1}, publisher = {Elsevier}, address = {Amsterdam}, issn = {0304-8853}, doi = {10.1016/j.jmmm.2018.10.066}, pages = {244 -- 248}, year = {2019}, abstract = {The movement of magnetic beads due to a magnetic field gradient is of great interest in different application fields. In this report we present a technique based on a magnetic tweezers setup to measure the velocity factor of magnetically actuated individual superparamagnetic beads in a fluidic environment. Several beads can be tracked simultaneously in order to gain and improve statistics. Furthermore we show our results for different beads with hydrodynamic diameters between 200 and 1000 nm from diverse manufacturers. These measurement data can, for example, be used to determine design parameters for a magnetic separation system, like maximum flow rate and minimum separation time, or to select suitable beads for fixed experimental requirements.}, language = {en} } @article{SildatkeKarwanniKraftetal.2023, author = {Sildatke, Michael and Karwanni, Hendrik and Kraft, Bodo and Z{\"u}ndorf, Albert}, title = {A distributed microservice architecture pattern for the automated generation of information extraction pipelines}, series = {SN Computer Science}, journal = {SN Computer Science}, number = {4, Article number: 833}, publisher = {Springer Singapore}, address = {Singapore}, issn = {2661-8907}, doi = {10.1007/s42979-023-02256-4}, pages = {19 Seiten}, year = {2023}, abstract = {Companies often build their businesses based on product information and therefore try to automate the process of information extraction (IE). Since the information source is usually heterogeneous and non-standardized, classic extract, transform, load techniques reach their limits. Hence, companies must implement the newest findings from research to tackle the challenges of process automation. They require a flexible and robust system that is extendable and ensures the optimal processing of the different document types. This paper provides a distributed microservice architecture pattern that enables the automated generation of IE pipelines. Since their optimal design is individual for each input document, the system ensures the ad-hoc generation of pipelines depending on specific document characteristics at runtime. Furthermore, it introduces the automated quality determination of each available pipeline and controls the integration of new microservices based on their impact on the business value. The introduced system enables fast prototyping of the newest approaches from research and supports companies in automating their IE processes. Based on the automated quality determination, it ensures that the generated pipelines always meet defined business requirements when they come into productive use.}, 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} }