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 - Monakhova, Yulia A1 - Diehl, Bernd W. K. T1 - A step towards optimization of the qNMR workflow: proficiency testing exercise at an GxP-accredited laboratory JF - Applied Magnetic Resonance N2 - 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. Y1 - 2021 U6 - https://doi.org/10.1007/s00723-021-01324-3 SN - 1613-7507 N1 - Corresponding author: Yulia Monakhova VL - 52 SP - 581 EP - 593 PB - Springer Nature CY - Wien ER - TY - JOUR A1 - Engelmann, Ulrich M. A1 - Shalaby, Ahmed A1 - Shasha, Carolyn A1 - Krishnan, Kannan M. A1 - Krause, Hans-Joachim T1 - Comparative modeling of frequency mixing measurements of magnetic nanoparticles using micromagnetic simulations and Langevin theory JF - Nanomaterials N2 - Dual frequency magnetic excitation of magnetic nanoparticles (MNP) enables enhanced biosensing applications. This was studied from an experimental and theoretical perspective: nonlinear sum-frequency components of MNP exposed to dual-frequency magnetic excitation were measured as a function of static magnetic offset field. The Langevin model in thermodynamic equilibrium was fitted to the experimental data to derive parameters of the lognormal core size distribution. These parameters were subsequently used as inputs for micromagnetic Monte-Carlo (MC)-simulations. From the hysteresis loops obtained from MC-simulations, sum-frequency components were numerically demodulated and compared with both experiment and Langevin model predictions. From the latter, we derived that approximately 90% of the frequency mixing magnetic response signal is generated by the largest 10% of MNP. We therefore suggest that small particles do not contribute to the frequency mixing signal, which is supported by MC-simulation results. Both theoretical approaches describe the experimental signal shapes well, but with notable differences between experiment and micromagnetic simulations. These deviations could result from Brownian relaxations which are, albeit experimentally inhibited, included in MC-simulation, or (yet unconsidered) cluster-effects of MNP, or inaccurately derived input for MC-simulations, because the largest particles dominate the experimental signal but concurrently do not fulfill the precondition of thermodynamic equilibrium required by Langevin theory. KW - Magnetic nanoparticles KW - Frequency mixing magnetic detection KW - Langevin theory KW - Micromagnetic simulation KW - Nonequilibrium dynamics Y1 - 2021 SN - 2079-4991 U6 - https://doi.org/10.3390/nano11051257 N1 - This article belongs to the Special Issue Applications and Properties of Magnetic Nanoparticles VL - 11 IS - 5 SP - 1 EP - 16 PB - MDPI CY - Basel ER - TY - JOUR A1 - Saretzki, Charlotte A1 - Bergmann, Ole A1 - Dahmann, Peter A1 - Janser, Frank A1 - Keimer, Jona A1 - Machado, Patricia A1 - Morrison, Audry A1 - Page, Henry A1 - Pluta, Emil A1 - Stübing, Felix A1 - Küpper, Thomas T1 - Are small airplanes safe with regards to COVID-19 transmission? JF - Journal of Travel Medicine Y1 - 2021 U6 - https://doi.org/10.1093/jtm/taab105 SN - 1708-8305 VL - 28 IS - 7 PB - Oxford University Press CY - Oxford ER - TY - JOUR A1 - Karschuck, Tobias A1 - Kaulen, Corinna A1 - Poghossian, Arshak A1 - Wagner, Patrick H. A1 - Schöning, Michael Josef T1 - Gold nanoparticle-modified capacitive field-effect sensors: Studying the surface density of nanoparticles and coupling of charged polyelectrolyte macromolecules JF - Electrochemical Science Advances N2 - The coupling of ligand-stabilized gold nanoparticles with field-effect devices offers new possibilities for label-free biosensing. In this work, we study the immobilization of aminooctanethiol-stabilized gold nanoparticles (AuAOTs) on the silicon dioxide surface of a capacitive field-effect sensor. The terminal amino group of the AuAOT is well suited for the functionalization with biomolecules. The attachment of the positively-charged AuAOTs on a capacitive field-effect sensor was detected by direct electrical readout using capacitance-voltage and constant capacitance measurements. With a higher particle density on the sensor surface, the measured signal change was correspondingly more pronounced. The results demonstrate the ability of capacitive field-effect sensors for the non-destructive quantitative validation of nanoparticle immobilization. In addition, the electrostatic binding of the polyanion polystyrene sulfonate to the AuAOT-modified sensor surface was studied as a model system for the label-free detection of charged macromolecules. Most likely, this approach can be transferred to the label-free detection of other charged molecules such as enzymes or antibodies. KW - polystyrene sulfonate KW - gold nanoparticles KW - field-effect sensor KW - detection of charged macromolecules KW - capacitive EIS sensor Y1 - 2021 U6 - https://doi.org/10.1002/elsa.202100179 SN - 0938-5193 VL - 2 IS - 5 PB - Wiley-VCH CY - Weinheim ER - TY - JOUR A1 - Hackl, Michael A1 - Buess, Eduard A1 - Kammerlohr, Sandra A1 - Nacov, Julia A1 - Staat, Manfred A1 - Leschinger, Tim A1 - Müller, Lars P. A1 - Wegmann, Kilian T1 - A "comma sign"-directed subscapularis repair in anterosuperior rotator cuff tears yields biomechanical advantages in a cadaveric model JF - The american journal of sports medicine N2 - Background: Additional stabilization of the “comma sign” in anterosuperior rotator cuff repair has been proposed to provide biomechanical benefits regarding stability of the repair. Purpose: This in vitro investigation aimed to investigate the influence of a comma sign–directed reconstruction technique for anterosuperior rotator cuff tears on the primary stability of the subscapularis tendon repair. Study Design: Controlled laboratory study. Methods: A total of 18 fresh-frozen cadaveric shoulders were used in this study. Anterosuperior rotator cuff tears (complete full-thickness tear of the supraspinatus and subscapularis tendons) were created, and supraspinatus repair was performed with a standard suture bridge technique. The subscapularis was repaired with either a (1) single-row or (2) comma sign technique. A high-resolution 3D camera system was used to analyze 3-mm and 5-mm gap formation at the subscapularis tendon-bone interface upon incremental cyclic loading. Moreover, the ultimate failure load of the repair was recorded. A Mann-Whitney test was used to assess significant differences between the 2 groups. Results: The comma sign repair withstood significantly more loading cycles than the single-row repair until 3-mm and 5-mm gap formation occurred (P≤ .047). The ultimate failure load did not reveal any significant differences when the 2 techniques were compared (P = .596). Conclusion: The results of this study show that additional stabilization of the comma sign enhanced the primary stability of subscapularis tendon repair in anterosuperior rotator cuff tears. Although this stabilization did not seem to influence the ultimate failure load, it effectively decreased the micromotion at the tendon-bone interface during cyclic loading. Clinical Relevance: The proposed technique for stabilization of the comma sign has shown superior biomechanical properties in comparison with a single-row repair and might thus improve tendon healing. Further clinical research will be necessary to determine its influence on the functional outcome. Y1 - 2021 U6 - https://doi.org/10.1177/03635465211031506 SN - 1552-3365 SN - 0363-5465 VL - 49 IS - 12 SP - 3212 EP - 3217 PB - Sage CY - London ER - TY - JOUR A1 - Gaigall, Daniel T1 - Test for Changes in the Modeled Solvency Capital Requirement of an Internal Risk Model JF - ASTIN Bulletin N2 - In the context of the Solvency II directive, the operation of an internal risk model is a possible way for risk assessment and for the determination of the solvency capital requirement of an insurance company in the European Union. A Monte Carlo procedure is customary to generate a model output. To be compliant with the directive, validation of the internal risk model is conducted on the basis of the model output. For this purpose, we suggest a new test for checking whether there is a significant change in the modeled solvency capital requirement. Asymptotic properties of the test statistic are investigated and a bootstrap approximation is justified. A simulation study investigates the performance of the test in the finite sample case and confirms the theoretical results. The internal risk model and the application of the test is illustrated in a simplified example. The method has more general usage for inference of a broad class of law-invariant and coherent risk measures on the basis of a paired sample. KW - Bootstrap KW - Empirical process KW - Functional Delta Method KW - Hadamard differentiability KW - Paired sample Y1 - 2021 U6 - https://doi.org/10.1017/asb.2021.20 SN - 1783-1350 VL - 51 IS - 3 SP - 813 EP - 837 PB - Cambridge Univ. Press CY - Cambridge ER - TY - JOUR A1 - Poghossian, Arshak A1 - Welden, Rene A1 - Buniatyan, Vahe V. A1 - Schöning, Michael Josef T1 - An Array of On-Chip Integrated, Individually Addressable Capacitive Field-Effect Sensors with Control Gate: Design and Modelling JF - Sensors N2 - The on-chip integration of multiple biochemical sensors based on field-effect electrolyte-insulator-semiconductor capacitors (EISCAP) is challenging due to technological difficulties in realization of electrically isolated EISCAPs on the same Si chip. In this work, we present a new simple design for an array of on-chip integrated, individually electrically addressable EISCAPs with an additional control gate (CG-EISCAP). The existence of the CG enables an addressable activation or deactivation of on-chip integrated individual CG-EISCAPs by simple electrical switching the CG of each sensor in various setups, and makes the new design capable for multianalyte detection without cross-talk effects between the sensors in the array. The new designed CG-EISCAP chip was modelled in so-called floating/short-circuited and floating/capacitively-coupled setups, and the corresponding electrical equivalent circuits were developed. In addition, the capacitance-voltage curves of the CG-EISCAP chip in different setups were simulated and compared with that of a single EISCAP sensor. Moreover, the sensitivity of the CG-EISCAP chip to surface potential changes induced by biochemical reactions was simulated and an impact of different parameters, such as gate voltage, insulator thickness and doping concentration in Si, on the sensitivity has been discussed. KW - equivalent circuit KW - multianalyte detection KW - control gate KW - on-chip integrated addressable EISCAP sensors KW - capacitive field-effect sensor Y1 - 2021 U6 - https://doi.org/10.3390/s21186161 SN - 1424-8220 N1 - This article belongs to the Special Issue "Field-Effect Sensors: From pH Sensing to Biosensing" VL - 21 IS - 18 SP - 17 PB - MDPI CY - Basel ER - TY - CHAP A1 - Engelmann, Ulrich M. A1 - Shasha, Carolyn A1 - Slabu, Ioana T1 - Magnetic nanoparticle relaxation in biomedical application: focus on simulating nanoparticle heating T2 - Magnetic nanoparticles in human health and medicine Y1 - 2021 SN - 978-1-119-75467-1 SP - 327 EP - 354 PB - Wiley-Blackwell CY - Hoboken, New Jeersey ER - TY - JOUR A1 - Gorzalka, Philip A1 - Schmiedt, Jacob Estevam A1 - Schorn, Christian T1 - Automated Generation of an Energy Simulation Model for an Existing Building from UAV Imagery JF - Buildings N2 - An approach to automatically generate a dynamic energy simulation model in Modelica for a single existing building is presented. It aims at collecting data about the status quo in the preparation of energy retrofits with low effort and costs. The proposed method starts from a polygon model of the outer building envelope obtained from photogrammetrically generated point clouds. The open-source tools TEASER and AixLib are used for data enrichment and model generation. A case study was conducted on a single-family house. The resulting model can accurately reproduce the internal air temperatures during synthetical heating up and cooling down. Modelled and measured whole building heat transfer coefficients (HTC) agree within a 12% range. A sensitivity analysis emphasises the importance of accurate window characterisations and justifies the use of a very simplified interior geometry. Uncertainties arising from the use of archetype U-values are estimated by comparing different typologies, with best- and worst-case estimates showing differences in pre-retrofit heat demand of about ±20% to the average; however, as the assumptions made are permitted by some national standards, the method is already close to practical applicability and opens up a path to quickly estimate possible financial and energy savings after refurbishment. KW - Modelica KW - heat transfer coefficient KW - heat demand KW - building energy modelling KW - building energy simulation Y1 - 2021 U6 - https://doi.org/10.3390/buildings11090380 SN - 2075-5309 N1 - This article belongs to the Special Issue "Application of Computer Technology in Buildings" VL - 11 IS - 9 PB - MDPI CY - Basel ER -