TY - JOUR A1 - Monakhova, Yulia A1 - Diehl, Bernd W.K. T1 - Novel approach of qNMR workflow by standardization using 2H integral: Application to any intrinsic calibration standard JF - Talanta N2 - Quantitative nuclear magnetic resonance (qNMR) is routinely performed by the internal or external standardization. The manuscript describes a simple alternative to these common workflows by using NMR signal of another active nuclei of calibration compound. For example, for any arbitrary compound quantification by NMR can be based on the use of an indirect concentration referencing that relies on a solvent having both 1H and 2H signals. To perform high-quality quantification, the deuteration level of the utilized deuterated solvent has to be estimated. In this contribution the new method was applied to the determination of deuteration levels in different deuterated solvents (MeOD, ACN, CDCl3, acetone, benzene, DMSO-d6). Isopropanol-d6, which contains a defined number of deuterons and protons, was used for standardization. Validation characteristics (precision, accuracy, robustness) were calculated and the results showed that the method can be used in routine practice. Uncertainty budget was also evaluated. In general, this novel approach, using standardization by 2H integral, benefits from reduced sample preparation steps and uncertainties, and can be applied in different application areas (purity determination, forensics, pharmaceutical analysis, etc.). KW - qNMR KW - Deuterium NMR KW - Deuterated solvents KW - Standardization Y1 - 2021 SN - 0039-9140 U6 - https://doi.org/10.1016/j.talanta.2020.121504 VL - 222 IS - Article number: 121504 PB - Elsevier ER - TY - JOUR A1 - Burmistrova, Natalia A. A1 - Soboleva, Polina M. A1 - Monakhova, Yulia T1 - Is infrared spectroscopy combined with multivariate analysis a promising tool for heparin authentication? JF - Journal of Pharmaceutical and Biomedical Analysis N2 - The investigation of the possibility to determine various characteristics of powder heparin (n = 115) was carried out with infrared spectroscopy. The evaluation of heparin samples included several parameters such as purity grade, distributing company, animal source as well as heparin species (i.e. Na-heparin, Ca-heparin, and heparinoids). Multivariate analysis using principal component analysis (PCA), soft independent modelling of class analogy (SIMCA), and partial least squares – discriminant analysis (PLS-DA) were applied for the modelling of spectral data. Different pre-processing methods were applied to IR spectral data; multiplicative scatter correction (MSC) was chosen as the most relevant. Obtained results were confirmed by nuclear magnetic resonance (NMR) spectroscopy. Good predictive ability of this approach demonstrates the potential of IR spectroscopy and chemometrics for screening of heparin quality. This approach, however, is designed as a screening tool and is not considered as a replacement for either of the methods required by USP and FDA. KW - IR spectroscopy KW - Heparin KW - Authenticity KW - Principal component analysis KW - Soft independent modeling of class analogy Y1 - 2021 SN - 0731-7085 U6 - https://doi.org/10.1016/j.jpba.2020.113811 VL - 194 IS - Article number: 113811 PB - Elsevier CY - Amsterdam ER - TY - JOUR A1 - Monakhova, Yulia A1 - Diehl, Bernd W. K. T1 - Simplification of NMR Workflows by Standardization Using 2H Integral of Deuterated Solvent as Applied to Aloe vera Preparations JF - Applied Magnetic Resonance N2 - 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.). Y1 - 2021 U6 - https://doi.org/10.1007/s00723-021-01393-4 SN - 1613-7507 VL - 52 IS - 11 SP - 1591 EP - 1600 PB - Springer CY - Cham ER - TY - JOUR A1 - Burger, René A1 - Rumpf, Jessica A1 - Do, Xuan Tung A1 - Monakhova, Yulia A1 - Diehl, Bernd W. K. A1 - Rehahn, Matthias A1 - Schulze, Margit T1 - Is NMR combined with multivariate regression applicable for the molecular weight determination of randomly cross-linked polymers such as lignin? JF - ACS Omega N2 - 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. Y1 - 2021 U6 - https://doi.org/10.1021/acsomega.1c03574 SN - 2470-1343 VL - 6 IS - 44 SP - 29516 EP - 29524 PB - ACS Publications CY - Washington, DC ER - TY - JOUR A1 - Tran, Ngoc Trinh A1 - Staat, Manfred T1 - Direct plastic structural design under random strength and random load by chance constrained programming JF - European Journal of Mechanics - A/Solids Y1 - 2021 U6 - https://doi.org/10.1016/j.euromechsol.2020.104106 SN - 0997-7538 VL - 85 IS - Article 104106 PB - Elsevier CY - Amsterdam ER - TY - JOUR A1 - Seefeldt, Patric A1 - Dachwald, Bernd T1 - Temperature increase on folded solar sail membranes JF - Advances in Space Research Y1 - 2021 U6 - https://doi.org/10.1016/j.asr.2020.09.026 SN - 0273-1177 VL - 67 IS - 9 SP - 2688 EP - 2695 PB - Elsevier CY - Amsterdam ER - TY - JOUR A1 - Oliveira, Danilo A. A1 - Molinnus, Denise A1 - Beging, Stefan A1 - Siqueira Jr, José R. A1 - Schöning, Michael Josef T1 - Biosensor Based on Self-Assembled Films of Graphene Oxide and Polyaniline Using a Field-Effect Device Platform JF - physica status solidi (a) applications and materials science N2 - A new functionalization method to modify capacitive electrolyte–insulator–semiconductor (EIS) structures with nanofilms is presented. Layers of polyallylamine hydrochloride (PAH) and graphene oxide (GO) with the compound polyaniline:poly(2-acrylamido-2-methyl-1-propanesulfonic acid) (PANI:PAAMPSA) are deposited onto a p-Si/SiO2 chip using the layer-by-layer technique (LbL). Two different enzymes (urease and penicillinase) are separately immobilized on top of a five-bilayer stack of the PAH:GO/PANI:PAAMPSA-modified EIS chip, forming a biosensor for detection of urea and penicillin, respectively. Electrochemical characterization is performed by constant capacitance (ConCap) measurements, and the film morphology is characterized by atomic force microscopy (AFM) and scanning electron microscopy (SEM). An increase in the average sensitivity of the modified biosensors (EIS–nanofilm–enzyme) of around 15% is found in relation to sensors, only carrying the enzyme but without the nanofilm (EIS–enzyme). In this sense, the nanofilm acts as a stable bioreceptor onto the EIS chip improving the output signal in terms of sensitivity and stability. KW - capacitive electrolyte–insulator–semiconductor sensors KW - graphene oxide KW - layer-by-layer technique KW - nanomaterials KW - polyaniline Y1 - 2021 U6 - https://doi.org/10.1002/pssa.202000747 SN - 1862-6319 N1 - Corresponding author: José R. Siqueira Jr & Michael J. Schöning VL - 218 IS - 13 SP - 1 EP - 9 PB - Wiley-VCH CY - Weinheim ER - TY - JOUR A1 - Welden, Rene A1 - Nagamine Komesu, Cindy A. A1 - Wagner, Patrick H. A1 - Schöning, Michael Josef A1 - Wagner, Torsten T1 - Photoelectrochemical enzymatic penicillin biosensor: A proof-of-concept experiment JF - Electrochemical Science Advances N2 - Photoelectrochemical (PEC) biosensors are a rather novel type of biosensors thatutilizelighttoprovideinformationaboutthecompositionofananalyte,enablinglight-controlled multi-analyte measurements. For enzymatic PEC biosensors,amperometric detection principles are already known in the literature. In con-trast, there is only a little information on H+-ion sensitive PEC biosensors. Inthis work, we demonstrate the detection of H+ions emerged by H+-generatingenzymes, exemplarily demonstrated with penicillinase as a model enzyme on atitanium dioxide photoanode. First, we describe the pH sensitivity of the sensorand study possible photoelectrocatalytic reactions with penicillin. Second, weshow the enzymatic PEC detection of penicillin. KW - enzymatic biosensor KW - penicillin KW - penicillinase KW - photoelectrochemistry KW - titanium dioxide photoanode Y1 - 2021 U6 - https://doi.org/10.1002/elsa.202100131 SN - 2698-5977 N1 - Corresponding author: Michael J. Schöning VL - 2 IS - 4 SP - 1 EP - 5 PB - Wiley-VCH CY - Weinheim ER - TY - JOUR A1 - Jablonski, Melanie A1 - Poghossian, Arshak A1 - Keusgen, Michael A1 - Wege, Christina A1 - Schöning, Michael Josef T1 - Detection of plant virus particles with a capacitive field-effect sensor JF - Analytical and Bioanalytical Chemistry N2 - Plant viruses are major contributors to crop losses and induce high economic costs worldwide. For reliable, on-site and early detection of plant viral diseases, portable biosensors are of great interest. In this study, a field-effect SiO2-gate electrolyte-insulator-semiconductor (EIS) sensor was utilized for the label-free electrostatic detection of tobacco mosaic virus (TMV) particles as a model plant pathogen. The capacitive EIS sensor has been characterized regarding its TMV sensitivity by means of constant-capacitance method. The EIS sensor was able to detect biotinylated TMV particles from a solution with a TMV concentration as low as 0.025 nM. A good correlation between the registered EIS sensor signal and the density of adsorbed TMV particles assessed from scanning electron microscopy images of the SiO2-gate chip surface was observed. Additionally, the isoelectric point of the biotinylated TMV particles was determined via zeta potential measurements and the influence of ionic strength of the measurement solution on the TMV-modified EIS sensor signal has been studied. KW - Plant virus KW - Capacitive field-effect sensor KW - Tobacco mosaic virus (TMV) KW - Label-free detection KW - Zeta potential Y1 - 2021 U6 - https://doi.org/10.1007/s00216-021-03448-8 SN - 1618-2650 N1 - Corresponding authors: Arshak Poghossian & Michael J. Schöning VL - 413 SP - 5669 EP - 5678 PB - Springer Nature CY - Cham ER - TY - JOUR A1 - Richter, Charlotte A1 - Braunstein, Bjoern A1 - Staeudle, Benjamin A1 - Attias, Julia A1 - Suess, Alexander A1 - Weber, Tobias A1 - Mileva, Katya N. A1 - Rittweger, Joern A1 - Green, David A. A1 - Albracht, Kirsten T1 - Contractile behavior of the gastrocnemius medialis muscle during running in simulated hypogravity JF - npj Microgravity N2 - Vigorous exercise countermeasures in microgravity can largely attenuate muscular degeneration, albeit the extent of applied loading is key for the extent of muscle wasting. Running on the International Space Station is usually performed with maximum loads of 70% body weight (0.7 g). However, it has not been investigated how the reduced musculoskeletal loading affects muscle and series elastic element dynamics, and thereby force and power generation. Therefore, this study examined the effects of running on the vertical treadmill facility, a ground-based analog, at simulated 0.7 g on gastrocnemius medialis contractile behavior. The results reveal that fascicle−series elastic element behavior differs between simulated hypogravity and 1 g running. Whilst shorter peak series elastic element lengths at simulated 0.7 g appear to be the result of lower muscular and gravitational forces acting on it, increased fascicle lengths and decreased velocities could not be anticipated, but may inform the development of optimized running training in hypogravity. However, whether the alterations in contractile behavior precipitate musculoskeletal degeneration warrants further study. Y1 - 2021 U6 - https://doi.org/10.1038/s41526-021-00155-7 SN - 2373-8065 N1 - Corresponding author: Charlotte Richter VL - 7 IS - Article number: 32 PB - Springer Nature CY - New York ER - TY - JOUR A1 - Hunker, Jan L. A1 - Gossmann, Matthias A1 - Raman, Aravind Hariharan A1 - Linder, Peter T1 - Artificial neural networks in cardiac safety assessment: Classification of chemotherapeutic compound effects on hiPSC-derived cardiomyocyte contractility JF - Journal of Pharmacological and Toxicological Methods Y1 - 2021 U6 - https://doi.org/10.1016/j.vascn.2021.107044 SN - 1056-8719 VL - 111 IS - Article number 107044 PB - Elsevier CY - New York ER - TY - JOUR A1 - Heiligers, Jeannette A1 - Schoutetens, Frederic A1 - Dachwald, Bernd T1 - Photon-sail equilibria in the alpha centauri system JF - Journal of Guidance, Control, and Dynamics Y1 - 2021 U6 - https://doi.org/10.2514/1.G005446 SN - 1533-3884 SN - 0731-5090 SN - 0162-3192 VL - 44 IS - 5 SP - 1053 EP - 1061 ER - TY - JOUR A1 - German, Laura A1 - Mikucki, Jill A. A1 - Welch, Susan A. A1 - Welch, Kathleen A. A1 - Lutton, Anthony A1 - Dachwald, Bernd A1 - Kowalski, Julia A1 - Heinen, Dirk A1 - Feldmann, Marco A1 - Francke, Gero A1 - Espe, Clemens A1 - Lyons, W. Berry T1 - Validation of sampling antarctic subglacial hypersaline waters with an electrothermal ice melting probe (IceMole) for environmental analytical geochemistry JF - International Journal of Environmental Analytical Chemistry N2 - Geochemical characterisation of hypersaline waters is difficult as high concentrations of salts hinder the analysis of constituents at low concentrations, such as trace metals, and the collection of samples for trace metal analysis in natural waters can be easily contaminated. This is particularly the case if samples are collected by non-conventional techniques such as those required for aquatic subglacial environments. In this paper we present the first analysis of a subglacial brine from Taylor Valley, (~ 78°S), Antarctica for the trace metals: Ba, Co, Mo, Rb, Sr, V, and U. Samples were collected englacially using an electrothermal melting probe called the IceMole. This probe uses differential heating of a copper head as well as the probe’s sidewalls and an ice screw at the melting head to move through glacier ice. Detailed blanks, meltwater, and subglacial brine samples were collected to evaluate the impact of the IceMole and the borehole pump, the melting and collection process, filtration, and storage on the geochemistry of the samples collected by this device. Comparisons between melt water profiles through the glacier ice and blank analysis, with published studies on ice geochemistry, suggest the potential for minor contributions of some species Rb, As, Co, Mn, Ni, NH4+, and NO2−+NO3− from the IceMole. The ability to conduct detailed chemical analyses of subglacial fluids collected with melting probes is critical for the future exploration of the hundreds of deep subglacial lakes in Antarctica. Y1 - 2021 U6 - https://doi.org/10.1080/03067319.2019.1704750 SN - 0306-7319 VL - 101 IS - 15 SP - 2654 EP - 2667 PB - Taylor & Francis CY - London ER - TY - JOUR A1 - Spietz, Peter A1 - Spröwitz, Tom A1 - Seefeldt, Patric A1 - Grundmann, Jan Thimo A1 - Jahnke, Rico A1 - Mikschl, Tobias A1 - Mikulz, Eugen A1 - Montenegro, Sergio A1 - Reershemius, Siebo A1 - Renger, Thomas A1 - Ruffer, Michael A1 - Sasaki, Kaname A1 - Sznajder, Maciej A1 - Tóth, Norbert A1 - Ceriotti, Matteo A1 - Dachwald, Bernd A1 - Macdonald, Malcolm A1 - McInnes, Colin A1 - Seboldt, Wolfgang A1 - Quantius, Dominik A1 - Bauer, Waldemar A1 - Wiedemann, Carsten A1 - Grimm, Christian D. A1 - Hercik, David A1 - Ho, Tra-Mi A1 - Lange, Caroline A1 - Schmitz, Nicole T1 - Paths not taken – The Gossamer roadmap’s other options JF - Advances in Space Research KW - Solar sail KW - Small spacecraft KW - DLR-ESTEC GOSSAMER roadmap for solar sailing KW - GOSSAMER-1 Y1 - 2021 U6 - https://doi.org/10.1016/j.asr.2021.01.044 SN - 0273-1177 VL - 67 IS - 9 SP - 2912 EP - 2956 PB - Elsevier CY - Amsterdam ER - TY - JOUR A1 - Olbertz, Klaus T1 - Die Dienstreisezeit als Arbeitszeit – oder doch nicht? : Zur arbeitgeberfreundlichen Bewertung von Dienstreisezeiten durch das Bundesarbeitsgericht JF - NWB - Steuer- und Wirtschaftsrecht N2 - Der arbeitsrechtlich richtige Umgang mit Zeiten einer Dienstreise kann in der betrieblichen Praxis Probleme bereiten. Ob die Reisezeiten als solche Arbeitszeit i. S. des Arbeitszeitgesetzes (ArbZG ) darstellen, also bspw. auf die tägliche Höchstarbeitszeit angerechnet werden müssen oder nicht, ist oftmals genauso unklar wie die Frage, ob und inwieweit Reisezeiten vergütungspflichtig sind. Aber auch, ob ein Arbeitnehmer überhaupt zur Durchführung einer Dienstreise verpflichtet werden kann, ist ein möglicher Anlass von Streitigkeiten zwischen den Arbeitsvertragsparteien, wie verschiedene Gerichtsentscheidungen zeigen. Der nachfolgende Beitrag beantwortet die aufgeworfenen Fragen und gibt hierzu einen praxisorientierten Überblick. Y1 - 2021 SN - 0028-3460 IS - 1 SP - 38 EP - 44 ER - TY - JOUR A1 - Alexyuk, Madina A1 - Bogoyavlenskiy, Andrey A1 - Alexyuk, Pavel A1 - Moldakhanov, Yergali A1 - Berezin, Vladimir A1 - Digel, Ilya T1 - Epipelagic microbiome of the Small Aral Sea: Metagenomic structure and ecological diversity JF - MicrobiologyOpen N2 - Microbial diversity studies regarding the aquatic communities that experienced or are experiencing environmental problems are essential for the comprehension of the remediation dynamics. In this pilot study, we present data on the phylogenetic and ecological structure of microorganisms from epipelagic water samples collected in the Small Aral Sea (SAS). The raw data were generated by massive parallel sequencing using the shotgun approach. As expected, most of the identified DNA sequences belonged to Terrabacteria and Actinobacteria (40% and 37% of the total reads, respectively). The occurrence of Deinococcus-Thermus, Armatimonadetes, Chloroflexi in the epipelagic SAS waters was less anticipated. Surprising was also the detection of sequences, which are characteristic for strict anaerobes—Ignavibacteria, hydrogen-oxidizing bacteria, and archaeal methanogenic species. We suppose that the observed very broad range of phylogenetic and ecological features displayed by the SAS reads demonstrates a more intensive mixing of water masses originating from diverse ecological niches of the Aral-Syr Darya River basin than presumed before. KW - ecological structure KW - metagenomics KW - microbial diversity KW - shotgun sequencing KW - Small Aral Sea Y1 - 2021 U6 - https://doi.org/10.1002/mbo3.1142 SN - 2045-8827 N1 - Corresponding author: Ilya Digel VL - 10 IS - 1 SP - 1 EP - 10 PB - Wiley CY - Weinheim ER - TY - JOUR A1 - Heinke, Lars N. A1 - Knicker, Axel J. A1 - Albracht, Kirsten T1 - Test-retest reliability of the internal shoulder rotator muscles' stretch reflex in healthy men JF - Journal of Electromyography and Kinesiology N2 - Until now the reproducibility of the short latency stretch reflex of the internal rotator muscles of the glenohumeral joint has not been identified. Twenty-three healthy male participants performed three sets of external shoulder rotation stretches with various pre-activation levels on two different dates of measurement to assess test-retest reliability. All stretches were applied with a dynamometer acceleration of 104°/s2 and a velocity of 150°/s. Electromyographical response was measured via surface EMG. Reflex latencies showed a pre-activation effect (ƞ2 = 0,355). ICC ranged from 0,735 to 0,909 indicating an overall “good” relative reliability. SRD 95% lay between ±7,0 to ±12,3 ms.. The reflex gain showed overall poor test-retest reproducibility. The chosen methodological approach presented a suitable test protocol for shoulder muscles stretch reflex latency evaluation. A proof-of-concept study to validate the presented methodical approach in shoulder involvement including subjects with clinically relevant conditions is recommended. KW - stretch reflex KW - shoulder KW - test-retest reliability KW - intraclass correlation coefficient KW - standard error of measurement Y1 - 2021 U6 - https://doi.org/10.1016/j.jelekin.2021.102611 SN - 1050-6411 VL - 62 IS - Article 102611 PB - Elsevier CY - Amsterdam ER - TY - JOUR A1 - Heel, Mareike van A1 - Dikta, Gerhard A1 - Braekers, Roel T1 - Bootstrap based goodness‑of‑fit tests for binary multivariate regression models JF - Journal of the Korean Statistical Society N2 - We consider a binary multivariate regression model where the conditional expectation of a binary variable given a higher-dimensional input variable belongs to a parametric family. Based on this, we introduce a model-based bootstrap (MBB) for higher-dimensional input variables. This test can be used to check whether a sequence of independent and identically distributed observations belongs to such a parametric family. The approach is based on the empirical residual process introduced by Stute (Ann Statist 25:613–641, 1997). In contrast to Stute and Zhu’s approach (2002) Stute & Zhu (Scandinavian J Statist 29:535–545, 2002), a transformation is not required. Thus, any problems associated with non-parametric regression estimation are avoided. As a result, the MBB method is much easier for users to implement. To illustrate the power of the MBB based tests, a small simulation study is performed. Compared to the approach of Stute & Zhu (Scandinavian J Statist 29:535–545, 2002), the simulations indicate a slightly improved power of the MBB based method. Finally, both methods are applied to a real data set. Y1 - 2021 U6 - https://doi.org/10.1007/s42952-021-00142-4 SN - 2005-2863 (Online) SN - 1226-3192 (Print) N1 - Corresponding author: Mareike van Heel VL - 51 PB - Springer Nature CY - Singapur ER - TY - JOUR A1 - Timme, Michael T1 - Rechtsprechungsübersicht zum Wohnraummietrecht JF - Monatsschrift für Deutsches Recht Y1 - 2021 U6 - https://doi.org/10.9785/mdtr-2021-750113 SN - 2194-4202 VL - 75 IS - 1 SP - 6 EP - 11 PB - Verlag Dr. Otto Schmidt CY - Köln ER - TY - JOUR A1 - Kezerashvili, Roman Ya A1 - Dachwald, Bernd T1 - Preface: Solar sailing: Concepts, technology, and missions II JF - Advances in Space Research Y1 - 2021 U6 - https://doi.org/10.1016/j.asr.2021.01.037 SN - 0273-1177 VL - 67 IS - 9 SP - 2559 EP - 2560 PB - Elsevier CY - Amsterdam ER -