@article{GerigkMaassTakorsetal.2000, author = {Gerigk, M. and Maaß, D. and Takors, Ralf and Kreutzer, A. and Wandrey, Christian and Bongaerts, Johannes and Wubbolts, Marcel}, title = {Fermentative Herstellung von L-Phenylalanin im Fed-Batch Verfahren mit E. coli unter Einbindung eines integrierten Aufarbeitungsverfahrens}, series = {Chemie-Ingenieur-Technik (CIT)}, volume = {Vol. 72}, journal = {Chemie-Ingenieur-Technik (CIT)}, number = {Iss. 9}, issn = {1522-2640 (E-Journal); 0009-286X (Print)}, pages = {926 -- 927}, year = {2000}, language = {de} } @misc{SchumannRoginSchneideretal.2012, author = {Schumann, C. and Rogin, S. and Schneider, H. and Oster, J. and Tippk{\"o}tter, Nils and Kampeis, P.}, title = {Steuerung von HGMS-Prozessen mittels Durchflusszytometrie}, series = {Chemie Ingenieur Technik}, volume = {84}, journal = {Chemie Ingenieur Technik}, number = {8}, publisher = {Wiley-VCH}, address = {Weinheim}, issn = {0009-286X}, doi = {10.1002/cite.201250125}, pages = {1370}, year = {2012}, abstract = {Die Hochgradientenmagnetseparation (HGMS) ist eine Methode zur Aufreinigung von biopharmazeutischen Produkten. Mit dieser Methode l{\"a}sst sich in nur einem Schritt eine Fest/Fest/Fl{\"u}ssig-Trennung erzielen, was zu einer erheblichen Zeit- und Kostenersparnis im Downstreaming f{\"u}hrt. Dennoch steht ihr industrieller Einsatz noch aus, was u. a. am Mangel an Analysenmethoden liegt, um die HGMS quantifizierbar zu machen. Gerade in der Pharmaproduktion werden Prozesse gebraucht, die gem{\"a}ß den einschl{\"a}gigen Vorschriften (cGMP) validiert und deren verfahrenstechnische Anlagenteile qualifiziert werden k{\"o}nnen. Die Schwierigkeit ist die Messung der magnetischen Mikrosorbentien in der Suspension, in der auch Zellen oder Zelltr{\"u}mmer vorliegen. Im Rahmen eines Forschungsprojektes im „Zentralen Innovationsprogramm Mittelstand" des BMWi wurden verschiedene Analysenmethoden untersucht. Die Durchflusszytometrie erm{\"o}glicht eine Charakterisierung von Partikeln und eine simultane quantitative Messung. Durch die multiparametrige Messung kann zwischen Zellen, Zelltr{\"u}mmern und Magnetpartikeln unterschieden werden. Die At-line-Einbindung des Durchflusszytometers ist durch den Einsatz einer externen Pumpe m{\"o}glich. {\"U}ber eine automatisierte Messwertanalyse kann der HGMS-Prozess mittels der Durchflusszytometrie gesteuert werden.}, language = {de} } @article{BongaertsZoschkeWeidneretal.1995, author = {Bongaerts, Johannes and Zoschke, Sascha and Weidner, Uwe and Linden, Gottfried}, title = {Transcriptional regulation of the proton translocating NADH}, series = {Molecular microbiology}, volume = {Vol. 16}, journal = {Molecular microbiology}, number = {Iss. 3}, issn = {1365-2958 (E-Journal); 0950-382x (Print)}, pages = {521 -- 534}, year = {1995}, language = {en} } @article{MonakhovaDiehl2021, author = {Monakhova, Yulia and Diehl, Bernd W.K.}, title = {Novel approach of qNMR workflow by standardization using 2H integral: Application to any intrinsic calibration standard}, series = {Talanta}, volume = {222}, journal = {Talanta}, number = {Article number: 121504}, publisher = {Elsevier}, isbn = {0039-9140}, doi = {10.1016/j.talanta.2020.121504}, year = {2021}, abstract = {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.).}, language = {en} } @article{MonakhovaDiehl2022, author = {Monakhova, Yulia and Diehl, Bernd W.K.}, title = {Multinuclear NMR screening of pharmaceuticals using standardization by 2H integral of a deuterated solvent}, series = {Journal of Pharmaceutical and Biomedical Analysis}, volume = {209}, journal = {Journal of Pharmaceutical and Biomedical Analysis}, number = {Article number: 114530}, publisher = {Elsevier}, isbn = {0731-7085}, doi = {10.1016/j.jpba.2021.114530}, year = {2022}, abstract = {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.}, language = {en} } @article{BlockMayWetzeletal.2023, author = {Block, Franziska and May, Alexander and Wetzel, Katharina and Adels, Klaudia and Elbers, Gereon and Schulze, Margit and Monakhova, Yulia}, title = {What is the best spectroscopic method for simultaneous analysis of organic acids and (poly)saccharides in biological matrices: Example of Aloe vera extracts?}, series = {Talanta Open}, volume = {7}, journal = {Talanta Open}, number = {Art. No. 100220}, publisher = {Elsevier}, address = {Amsterdam}, issn = {2666-8319}, doi = {10.1016/j.talo.2023.100220}, pages = {1 -- 9}, year = {2023}, abstract = {Several species of (poly)saccharides and organic acids can be found often simultaneously in various biological matrices, e.g., fruits, plant materials, and biological fluids. The analysis of such matrices sometimes represents a challenging task. Using Aloe vera (A. vera) plant materials as an example, the performance of several spectro-scopic methods (80 MHz benchtop NMR, NIR, ATR-FTIR and UV-vis) for the simultaneous analysis of quality parameters of this plant material was compared. The determined parameters include (poly)saccharides such as aloverose, fructose and glucose as well as organic acids (malic, lactic, citric, isocitric, acetic, fumaric, benzoic and sorbic acids). 500 MHz NMR and high-performance liquid chromatography (HPLC) were used as the reference methods. UV-vis data can be used only for identification of added preservatives (benzoic and sorbic acids) and drying agent (maltodextrin) and semiquantitative analysis of malic acid. NIR and MIR spectroscopies combined with multivariate regression can deliver more informative overview of A. vera extracts being able to additionally quantify glucose, aloverose, citric, isocitric, malic, lactic acids and fructose. Low-field NMR measurements can be used for the quantification of aloverose, glucose, malic, lactic, acetic, and benzoic acids. The benchtop NMR method was successfully validated in terms of robustness, stability, precision, reproducibility and limit of detection (LOD) and quantification (LOQ), respectively. All spectroscopic techniques are useful for the screening of (poly)saccharides and organic acids in plant extracts and should be applied according to its availability as well as information and confidence required for the specific analytical goal. Benchtop NMR spectroscopy seems to be the most feasible solution for quality control of A. vera products.}, language = {en} } @article{AdelsElbersDiehletal.2023, author = {Adels, Klaudia and Elbers, Gereon and Diehl, Bernd and Monakhova, Yulia}, title = {Multicomponent analysis of dietary supplements containing glucosamine and chondroitin: comparative low- and high-field NMR spectroscopic study}, series = {Analytical Sciences}, volume = {2023}, journal = {Analytical Sciences}, publisher = {Springer Verlag}, address = {Cham}, issn = {1348-2246 (Online)}, doi = {10.1007/s44211-023-00433-2}, pages = {13 Seiten}, year = {2023}, abstract = {With the prevalence of glucosamine- and chondroitin-containing dietary supplements for people with osteoarthritis in the marketplace, it is important to have an accurate and reproducible analytical method for the quantitation of these compounds in finished products. NMR spectroscopic method based both on low- (80 MHz) and high- (500-600 MHz) field NMR instrumentation was established, compared and validated for the determination of chondroitin sulfate and glucosamine in dietary supplements. The proposed method was applied for analysis of 20 different dietary supplements. In the majority of cases, quantification results obtained on the low-field NMR spectrometer are similar to those obtained with high-field 500-600 MHz NMR devices. Validation results in terms of accuracy, precision, reproducibility, limit of detection and recovery demonstrated that the developed method is fit for purpose for the marketed products. The NMR method was extended to the analysis of methylsulfonylmethane, adulterant maltodextrin, acetate and inorganic ions. Low-field NMR can be a quicker and cheaper alternative to more expensive high-field NMR measurements for quality control of the investigated dietary supplements. High-field NMR instrumentation can be more favorable for samples with complex composition due to better resolution, simultaneously giving the possibility of analysis of inorganic species such as potassium and chloride.}, language = {en} } @article{TrappLammersEngudaretal.2023, author = {Trapp, Svenja and Lammers, Tom and Engudar, Gokce and Hoehr, Cornelia and Denkova, Antonia G. and Paulßen, Elisabeth and de Kruijff, Robin M.}, title = {Membrane-based microfluidic solvent extraction of Ga-68 from aqueous Zn solutions: towards an automated cyclotron production loop}, series = {EJNMMI Radiopharmacy and Chemistry}, volume = {2023}, journal = {EJNMMI Radiopharmacy and Chemistry}, number = {8, Article number: 9}, publisher = {Springer Nature}, issn = {2365-421X}, doi = {10.1186/s41181-023-00195-2}, pages = {1 -- 14}, year = {2023}, language = {en} } @article{MonakhovaDiehl2021, author = {Monakhova, Yulia and Diehl, Bernd W. K.}, title = {A step towards optimization of the qNMR workflow: proficiency testing exercise at an GxP-accredited laboratory}, series = {Applied Magnetic Resonance}, volume = {52}, journal = {Applied Magnetic Resonance}, publisher = {Springer Nature}, address = {Wien}, issn = {1613-7507}, doi = {10.1007/s00723-021-01324-3}, pages = {581 -- 593}, year = {2021}, abstract = {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.}, language = {en} } @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} }