Validated Multimethod Approach for Full Characterization of 2'-Fucosyl-d-lactose as an Industrially Produced Human Milk Oligosaccharide.

Human milk oligosaccharides are of high interest as active ingredients in infant formulas and dietary food supplements. Full characterization of members of this compound class is challenging due to the intrinsic complexity of byproducts during synthesis by fermentation. Moreover, when method validation is targeted for a regulated environment, a robust chromatographic separation of the highly polar oligosaccharides needs to be addressed, including isomers and compounds relevant for potential product adulteration.

Self-assembly of Co/Pt stripes with current-induced domain wall motion towards 3D racetrack devices.

Modification of the magnetic properties under the induced strain and curvature is a promising avenue to build three-dimensional magnetic devices, based on the domain wall motion. So far, most of the studies with 3D magnetic structures were performed in the helixes and nanowires, mainly with stationary domain walls. In this study, we demonstrate the impact of 3D geometry, strain and curvature on the current-induced domain wall motion and spin-orbital torque efficiency in the heterostructure, realized via a self-assembly rolling technique on a polymeric platform.

Direct imaging of nanoscale field-driven domain wall oscillations in Landau structures.

Linear oscillatory motion of domain walls (DWs) in the kHz and MHz regime is crucial when realizing precise magnetic field sensors such as giant magnetoimpedance devices. Numerous magnetically active defects lead to pinning of the DWs during their motion, affecting the overall behavior. Thus, the direct monitoring of the domain wall's oscillatory behavior is an important step to comprehend the underlying micromagnetic processes and to improve the magnetoresistive performance of these devices.

Size-Specific Magnetic Configurations in Electrodeposited Epitaxial Iron Nanocuboids: From Landau Pattern to Vortex and Single Domain States.

As the size of magnetic devices continuously decreases, the creation of three-dimensional nanomagnets and the understanding of their magnetic configurations become increasingly important for modern applications. Here, by progressive nucleation during epitaxial nanoelectrodeposition, we synthesize single-crystal iron nanocuboids with sizes ranging 10 to 200 nm on one sample. The size-dependent magnetic configurations of these nanocuboids are studied by quantitative magnetic force microscopy and electron holography.

Creating Ferroic Micropatterns through Geometrical Transformation.

The functionality of a ferroic device is intimately coupled to the configuration of domains, domain boundaries, and the possibility for tailoring them. Exemplified with a ferromagnetic system, we present a novel approach which allows the creation of new, metastable multidomain patterns with tailored wall configurations through a self-assembled geometrical transformation. By preparing a magnetic layer system on a polymeric platform including swelling layer, a repeated self-assembled rolling into a multiwinding tubular structure and unrolling of the functional membrane is obtained.

Modal Frustration and Periodicity Breaking in Artificial Spin Ice.

Here, an artificial spin ice lattice is introduced that exhibits unique Ising and non-Ising behavior under specific field switching protocols because of the inclusion of coupled nanomagnets into the unit cell. In the Ising regime, a magnetic switching mechanism that generates a uni- or bimodal distribution of states dependent on the alignment of the field is demonstrated with respect to the lattice unit cell. In addition, a method for generating a plethora of randomly distributed energy states across the lattice, consisting of Ising and Landau states, is investigated through magnetic force microscopy and micromagnetic modeling.

Stress-Actuated Spiral Microelectrode for High-Performance Lithium-Ion Microbatteries.

Miniaturization of batteries lags behind the success of modern electronic devices. Neither the device volume nor the energy density of microbatteries meets the requirement of microscale electronic devices. The main limitation for pushing the energy density of microbatteries arises from the low mass loading of active materials.

An extraordinary chiral exchange-bias phenomenon: engineering the sign of the bias field in orthogonal bilayers by a magnetically switchable response mechanism.

Isothermal tuning of both the magnitude and the sign of the bias field has been achieved by exploiting a new phenomenon in a system consisting of two orthogonally coupled films: SmCo5 (out-of-plane anisotropy)-CoFeB (in-plane anisotropy). This has been achieved by using the large dipolar magnetic field of the SmCo5 layer resulting in the pinning of one of the branches of the hysteresis loop (either the ascending or the descending branch) at a fixed field value while the second one is modulated along the field axis by varying the orientation of an externally applied magnetic field. This means the possibility of controlling the sign of the bias field in a manner not reported to date.

Determination of tip transfer function for quantitative MFM using frequency domain filtering and least squares method.

Magnetic force microscopy has unsurpassed capabilities in analysis of nanoscale and microscale magnetic samples and devices. Similar to other Scanning Probe Microscopy techniques, quantitative analysis remains a challenge. Despite large theoretical and practical progress in this area, present methods are seldom used due to their complexity and lack of systematic understanding of related uncertainties and recommended best practice.

Metrological large range magnetic force microscopy.

A new metrological large range magnetic force microscope (Met. LR-MFM) has been developed. In its design, the scanner motion is measured by using three laser interferometers along the x, y, and z axes.

Epitaxial hard magnetic SmCo MFM tips - a new approach to advanced magnetic force microscopy imaging.

Cantilever based scanning force sensors, which probe a specific tip-sample interaction through a functional tip coating, are limited by the material performance achievable in the coating process. In case of the wide spread magnetic force microscopy (MFM) technique, the magnetic performance of MFM tips, especially the response to magnetic fields and the coercivity, fall far behind the quality known from permanent magnet films prepared with optimized process conditions on appropriate substrates. We resolve this limitation by starting from an optimized thin film architecture - a highly anisotropic SmCo5 film grown epitaxially on MgO(110) substrates - from which a tip is separated by focused ion beam and is attached to a cantilever.

Calibration of multi-layered probes with low/high magnetic moments.

We present a comprehensive method for visualisation and quantification of the magnetic stray field of magnetic force microscopy (MFM) probes, applied to the particular case of custom-made multi-layered probes with controllable high/low magnetic moment states. The probes consist of two decoupled magnetic layers separated by a non-magnetic interlayer, which results in four stable magnetic states: ±ferromagnetic (FM) and ±antiferromagnetic (A-FM). Direct visualisation of the stray field surrounding the probe apex using electron holography convincingly demonstrates a striking difference in the spatial distribution and strength of the magnetic flux in FM and A-FM states.

Magnetite Core-Shell Nanoparticles in Nondestructive Flaw Detection of Polymeric Materials.

Nondestructive flaw detection in polymeric materials is important but difficult to achieve. In this research, the application of magnetite nanoparticles (MNPs) in nondestructive flaw detection is studied and realized, to the best of our knowledge, for the first time. Superparamagnetic and highly magnetic (up to 63 emu/g) magnetite core-shell nanoparticles are prepared by grafting bromo-end-group-functionalized poly(glycidyl methacrylate) (Br-PGMA) onto surface-modified FeO NPs.

Ultrahigh-performance liquid chromatography-ultraviolet absorbance detection-high-resolution-mass spectrometry combined with automated data processing for studying the kinetics of oxidative thermal degradation of thyroxine in the solid state.

Levothyroxine as active pharmaceutical ingredient of formulations used for the treatment of hypothyroidism is distributed worldwide and taken by millions of people. An important issue in terms of compound stability is its capability to react with ambient oxygen, especially in case of long term compound storage at elevated temperature. In this study we demonstrate that ultrahigh-performance liquid chromatography coupled to UV spectrometry and high-resolution mass spectrometry (UHPLC-UV-HRMS) represent very useful approaches to investigate the influence of ambient oxygen on the degradation kinetics of levothyroxine in the solid state at enhanced degradation conditions.

Magnetic domain pattern in hierarchically twinned epitaxial Ni-Mn-Ga films.

Magnetic shape memory alloys exhibit a hierarchically twinned microstructure, which has been examined thoroughly in epitaxial Ni-Mn-Ga films. Here we analyze the consequences of this 'twin within twins' microstructure on the magnetic domain pattern. Atomic and magnetic force microscopy are used to probe the correlation between the martensitic microstructure and magnetic domains.

Development and characterization of a capillary gap sampler as new microfluidic device for fast and direct analysis of low sample amounts by ESI-MS.

Direct hyphenation of miniaturized sampling devices to electrospray ionization-mass spectrometry (ESI-MS) is attractive because ESI-MS is compatible with microfluidics and allows comprehensive sample analysis, yielding information that is orthogonal to that available from optical methods. We present a "capillary gap sampler" as a platform for directly connecting microfluidics to μ-ESI-MS. The sampler was designed to be robust, light and compact, and to allow precise and fast liquid handling.

Rapid and comprehensive impurity profiling of synthetic thyroxine by ultrahigh-performance liquid chromatography-high-resolution mass spectrometry.

Rapid and efficient quality control according to the public authority regulations is mandatory to guarantee safety of the pharmaceuticals and to save resources in the pharmaceutical industry. In the case of so-called "grandfather products" like the synthetic thyroid hormone thyroxine, strict regulations enforce a detailed chemical analysis in order to characterize potentially toxic or pharmacologically relevant impurities. We report a straightforward workflow for the comprehensive impurity profiling of synthetic thyroid hormones and impurities employing ultrahigh-performance liquid chromatography (UHPLC) hyphenated to high-resolution mass spectrometry (HRMS).

Investigation of reaction mechanisms of drug degradation in the solid state: a kinetic study implementing ultrahigh-performance liquid chromatography and high-resolution mass spectrometry for thermally stressed thyroxine.

A reaction scheme was derived for the thermal degradation of thyroxine in the solid state, using data obtained from ultrahigh-performance liquid chromatography and high-resolution mass spectrometry (UHPLC-HRMS). To study the reaction mechanism and kinetics of the thermal degradation of the pharmaceutical in the solid state, a workflow was developed by generating compound-specific, time-dependent degradation or formation curves of at least 13 different degradation products. Such curves allowed one to distinguish between first- and second-generation degradation products, as well as impurities resulting from chemical synthesis.

On-line solid-phase extraction high-performance liquid chromatography-tandem mass spectrometry for the quantitative analysis of tacrolimus in whole blood hemolyzate.

Tacrolimus is an immunosuppressive drug essential for preventing organ rejection after transplantation. Since tacrolimus strongly binds to erythrocytes, therapeutic monitoring requires its quantification in whole blood lyzate, representing one of the most difficult to analyze biological fluids due to its high protein load. In this communication, we report on the successful combination of whole blood hemolysis employing ionic liquids, followed by sample preparation by means of on-line solid phase extraction (SPE) using restricted access materials (RAM), which permitted the efficient removal of hemoglobin and other large biomolecules.

Characterization of GDP-mannose dehydrogenase from the brown alga Ectocarpus siliculosus providing the precursor for the alginate polymer.

Alginate is a major cell wall polymer of brown algae. The precursor for the polymer is GDP-mannuronic acid, which is believed to be derived from a four-electron oxidation of GDP-mannose through the enzyme GDP-mannose dehydrogenase (GMD). So far no eukaryotic GMD has been biochemically characterized.