TY - JOUR A1 - Haeger, Gerrit A1 - Bongaerts, Johannes A1 - Siegert, Petra T1 - A convenient ninhydrin assay in 96-well format for amino acid-releasing enzymes using an air-stable reagent JF - Analytical Biochemistry N2 - An improved and convenient ninhydrin assay for aminoacylase activity measurements was developed using the commercial EZ Nin™ reagent. Alternative reagents from literature were also evaluated and compared. The addition of DMSO to the reagent enhanced the solubility of Ruhemann's purple (RP). Furthermore, we found that the use of a basic, aqueous buffer enhances stability of RP. An acidic protocol for the quantification of lysine was developed by addition of glacial acetic acid. The assay allows for parallel processing in a 96-well format with measurements microtiter plates. Y1 - 2022 U6 - https://doi.org/10.1016/j.ab.2022.114819 SN - 1096-0309 IS - 624 PB - Elsevier CY - Amsterdam ER - TY - JOUR A1 - Zhantlessova, Sirina A1 - Savitskaya, Irina A1 - Kistaubayeva, Aida A1 - Ignatova, Ludmila A1 - Talipova, Aizhan A1 - Pogrebnjak, Alexander A1 - Digel, Ilya T1 - Advanced “Green” prebiotic composite of bacterial cellulose/pullulan based on synthetic biology-powered microbial coculture strategy JF - Polymers N2 - 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. KW - coculture KW - pullulan KW - exopolysaccharides KW - prebiotic KW - bacterial cellulose Y1 - 2022 U6 - https://doi.org/10.3390/polym14153224 SN - 2073-4360 N1 - This article belongs to the Special Issue "Cellulose Based Composites" VL - 14 IS - 15 PB - MDPI CY - Basel ER - TY - JOUR A1 - Ojovan, Michael I. A1 - Steinmetz, Hans-Jürgen T1 - Approaches to Disposal of Nuclear Waste JF - Energies N2 - We present a concise mini overview on the approaches to the disposal of nuclear waste currently used or deployed. The disposal of nuclear waste is the end point of nuclear waste management (NWM) activities and is the emplacement of waste in an appropriate facility without the intention to retrieve it. The IAEA has developed an internationally accepted classification scheme based on the end points of NWM, which is used as guidance. Retention times needed for safe isolation of waste radionuclides are estimated based on the radiotoxicity of nuclear waste. Disposal facilities usually rely on a multi-barrier defence system to isolate the waste from the biosphere, which comprises the natural geological barrier and the engineered barrier system. Disposal facilities could be of a trench type, vaults, tunnels, shafts, boreholes, or mined repositories. A graded approach relates the depth of the disposal facilities’ location with the level of hazard. Disposal practices demonstrate the reliability of nuclear waste disposal with minimal expected impacts on the environment and humans. KW - borehole disposal KW - geological disposal KW - disposal facility KW - retention time KW - nuclear waste Y1 - 2022 U6 - https://doi.org/10.3390/en15207804 SN - 1996-1073 N1 - This article belongs to the Special Issue "Treatment of Radioactive Waste and Sustainability Energy" VL - 15 IS - 20 PB - MDPI CY - Basel ER - TY - JOUR A1 - Burger, René A1 - Lindner, Simon A1 - Rumpf, Jessica A1 - Do, Xuan Tung A1 - Diehl, Bernd W.K. A1 - Rehahn, Matthias A1 - Monakhova, Yulia A1 - Schulze, Margit T1 - Benchtop versus high field NMR: Comparable performance found for the molecular weight determination of lignin JF - Journal of Pharmaceutical and Biomedical Analysis N2 - Lignin is a promising renewable biopolymer being investigated worldwide as an environmentally benign substitute of fossil-based aromatic compounds, e.g. for the use as an excipient with antioxidant and antimicrobial properties in drug delivery or even as active compound. For its successful implementation into process streams, a quick, easy, and reliable method is needed for its molecular weight determination. Here we present a method using 1H spectra of benchtop as well as conventional NMR systems in combination with multivariate data analysis, to determine lignin’s molecular weight (Mw and Mn) and polydispersity index (PDI). A set of 36 organosolv lignin samples (from Miscanthus x giganteus, Paulownia tomentosa and Silphium perfoliatum) was used for the calibration and cross validation, and 17 samples were used as external validation set. Validation errors between 5.6% and 12.9% were achieved for all parameters on all NMR devices (43, 60, 500 and 600 MHz). Surprisingly, no significant difference in the performance of the benchtop and high-field devices was found. This facilitates the application of this method for determining lignin’s molecular weight in an industrial environment because of the low maintenance expenditure, small footprint, ruggedness, and low cost of permanent magnet benchtop NMR systems. KW - NMR KW - PLS-regression KW - Molecular weight determination KW - Chemometrics KW - Biomass Y1 - 2022 SN - 0731-7085 U6 - https://doi.org/10.1016/j.jpba.2022.114649 VL - 212 IS - Article number: 114649 PB - Elsevier CY - New York, NY ER - TY - GEN A1 - Braun, Lena A1 - Krafft, Simone A1 - Tippkötter, Nils T1 - Combined supercritical carbon dioxide extraction and chromatography of the algae fatty linoleic and linolenic acid T2 - Chemie Ingenieur Technik N2 - A method for the integrated extraction and separation of fatty acids from algae using supercritical CO2 is presented. Desmodesmus obliquus and Chlorella sorokiniana were used as algae. First, a method for chromatographic separation of fatty acids of different degrees of saturation was established and optimized. Then, an integrated method for supercritical extraction was developed for both algal species. It was also verified whether prior cell disruption was beneficial for extraction. In developing the method for chromatographic separation, statistical experimental design was used to determine the optimal parameter settings. The methanol content in the mobile phase proved to be the most important parameter for successful separation of the three unsaturated fatty acids oleic acid, linoleic acid, and linolenic acid. Supercritical extraction with dried algae showed that about four times more fatty acids can be extracted from C. sorokiniana relative to the dry mass used. Y1 - 2022 U6 - https://doi.org/10.1002/cite.202255308 SN - 0009-286X SN - 1522-2640 (eISSN) N1 - ProcessNet and DECHEMA‐BioTechNet Jahrestagungen 2022 together with 13th ESBES Symposium 2022, 12. - 15. September 2022, Eurogress Aachen VL - 94 IS - 9 SP - 1304 PB - Wiley-VCH CY - Weinheim ER - TY - JOUR A1 - Welden, Melanie A1 - Severins, Robin A1 - Poghossian, Arshak A1 - Wege, Christina A1 - Bongaerts, Johannes A1 - Siegert, Petra A1 - Keusgen, Michael A1 - Schöning, Michael Josef T1 - Detection of acetoin and diacetyl by a tobacco mosaic virus-assisted field-effect biosensor JF - Chemosensors N2 - Acetoin and diacetyl have a major impact on the flavor of alcoholic beverages such as wine or beer. Therefore, their measurement is important during the fermentation process. Until now, gas chromatographic techniques have typically been applied; however, these require expensive laboratory equipment and trained staff, and do not allow for online monitoring. In this work, a capacitive electrolyte–insulator–semiconductor sensor modified with tobacco mosaic virus (TMV) particles as enzyme nanocarriers for the detection of acetoin and diacetyl is presented. The enzyme acetoin reductase from Alkalihalobacillus clausii DSM 8716ᵀ is immobilized via biotin–streptavidin affinity, binding to the surface of the TMV particles. The TMV-assisted biosensor is electrochemically characterized by means of leakage–current, capacitance–voltage, and constant capacitance measurements. In this paper, the novel biosensor is studied regarding its sensitivity and long-term stability in buffer solution. Moreover, the TMV-assisted capacitive field-effect sensor is applied for the detection of diacetyl for the first time. The measurement of acetoin and diacetyl with the same sensor setup is demonstrated. Finally, the successive detection of acetoin and diacetyl in buffer and in diluted beer is studied by tuning the sensitivity of the biosensor using the pH value of the measurement solution. Y1 - 2022 U6 - https://doi.org/10.3390/chemosensors10060218 SN - 2227-9040 N1 - This article belongs to the Special Issue "Nanostructured Devices for Biochemical Sensing" VL - 10 IS - 6 PB - MDPI CY - Basel ER - TY - JOUR A1 - Lindner, Simon A1 - Burger, René A1 - Rutledge, Douglas N. A1 - Do, Xuan Tung A1 - Rumpf, Jessica A1 - Diehl, Bernd W. K. A1 - Schulze, Margit A1 - Monakhova, Yulia T1 - Is the calibration transfer of multivariate calibration models between high- and low-field NMR instruments possible? A case study of lignin molecular weight JF - Analytical chemistry N2 - 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. Y1 - 2022 SN - 1520-6882 U6 - https://doi.org/10.1021/acs.analchem.1c05125 VL - 94 IS - 9 SP - 3997 EP - 4004 PB - ACS Publications CY - Washington, DC ER - TY - GEN A1 - Rothkranz, Berit A1 - Krafft, Simone A1 - Tippkötter, Nils T1 - Media optimization for sustainable fuel production: How to produce biohydrogen from renewable resources with Thermotoga neapolitana T2 - Chemie Ingenieur Technik N2 - Hydrogen is playing an increasingly important role in research and politics as an energy carrier of the future. Since hydrogen has commonly been produced from methane by steam reforming, the need for climate-friendly, alternative production routes is emerging. In addition to electrolysis, fermentative routes for the production of so-called biohydrogen are "green" alternatives. The application of microorganisms offers the advantage of sustainable production from renewable resources using easily manageable technologies. In this project, the hyperthermophilic, anaerobic microorganism Thermotoga neapolitana is used for the productio nof biohydrogen from renewable resources. The enzymatically hydrolyzed resources were used in fermentation leading to yield coefficients of 1.8 mole H₂ per mole glucose when using hydrolyzed straw and ryegrass supplemented with medium, respectively. These results are similar to the hydrogen yields when using Thermotoga basal medium with glucose (TBGY) as control group. In order to minimize the supplementation of the hydrolysate and thus increase the economic efficiency of the process, the essential media components were identified. The experiments revealed NaCl, KCl, and glucose as essential components for cell growth as well as biohydrogen production. When excluding NaCl, a decrease of 96% in hydrogen production occured. Y1 - 2022 U6 - https://doi.org/10.1002/cite.202255305 SN - 0009-286X SN - 1522-2640 (eISSN) N1 - ProcessNet and DECHEMA‐BioTechNet Jahrestagungen 2022 together with 13th ESBES Symposium 2022, 12. - 15. September 2022, Eurogress Aachen VL - 94 IS - 9 SP - 1298 EP - 1299 PB - Wiley-VCH CY - Weinheim ER - TY - JOUR A1 - Monakhova, Yulia A1 - Diehl, Bernd W.K. T1 - Multinuclear NMR screening of pharmaceuticals using standardization by 2H integral of a deuterated solvent JF - Journal of Pharmaceutical and Biomedical Analysis N2 - NMR standardization approach that uses the 2H integral of deuterated solvent for quantitative multinuclear analysis of pharmaceuticals is described. As a proof of principle, the existing NMR procedure for the analysis of heparin products according to US Pharmacopeia monograph is extended to the determination of Na+ and Cl- content in this matrix. Quantification is performed based on the ratio of a 23Na (35Cl) NMR integral and 2H NMR signal of deuterated solvent, D2O, acquired using the specific spectrometer hardware. As an alternative, the possibility of 133Cs standardization using the addition of Cs2CO3 stock solution is shown. Validation characteristics (linearity, repeatability, sensitivity) are evaluated. A holistic NMR profiling of heparin products can now also be used for the quantitative determination of inorganic compounds in a single analytical run using a single sample. In general, the new standardization methodology provides an appealing alternative for the NMR screening of inorganic and organic components in pharmaceutical products. KW - NMR spectroscopy KW - Inorganic ions KW - Heparin KW - Standardization Y1 - 2022 SN - 0731-7085 U6 - https://doi.org/10.1016/j.jpba.2021.114530 VL - 209 IS - Article number: 114530 PB - Elsevier ER - TY - JOUR A1 - Monakhova, Yulia A1 - Diehl, Bernd W.K. T1 - Nuclear magnetic resonance spectroscopy as an elegant tool for a complete quality control of crude heparin material JF - Journal of Pharmaceutical and Biomedical Analysis N2 - 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). KW - NMR spectroscopy KW - Heparin KW - Crude heparin KW - USP KW - Ions Y1 - 2022 U6 - https://doi.org/10.1016/j.jpba.2022.114915 SN - 0731-7085 VL - 219 IS - Article number: 114915 PB - Elsevier CY - New York, NY ER -