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The physicochemical properties of synthetically produced bone substitute materials (BSM) have a major impact on biocompatibility. This affects bony tissue integration, osteoconduction, as well as the degradation pattern and the correlated inflammatory tissue responses including macrophages and multinucleated giant cells (MNGCs). Thus, influencing factors such as size, special surface morphologies, porosity, and interconnectivity have been the subject of extensive research. In the present publication, the influence of the granule size of three identically manufactured bone substitute granules based on the technology of hydroxyapatite (HA)-forming calcium phosphate cements were investigated, which includes the inflammatory response in the surrounding tissue and especially the induction of MNGCs (as a parameter of the material degradation). For the in vivo study, granules of three different size ranges (small = 0.355–0.5 mm; medium = 0.5–1 mm; big = 1–2 mm) were implanted in the subcutaneous connective tissue of 45 male BALB/c mice. At 10, 30, and 60 days post implantationem, the materials were explanted and histologically processed. The defect areas were initially examined histopathologically. Furthermore, pro- and anti-inflammatory macrophages were quantified histomorphometrically after their immunohistochemical detection. The number of MNGCs was quantified as well using a histomorphometrical approach. The results showed a granule size-dependent integration behavior. The surrounding granulation tissue has passivated in the groups of the two bigger granules at 60 days post implantationem including a fibrotic encapsulation, while a granulation tissue was still present in the group of the small granules indicating an ongoing cell-based degradation process. The histomorphometrical analysis showed that the number of proinflammatory macrophages was significantly increased in the small granules at 60 days post implantationem. Similarly, a significant increase of MNGCs was detected in this group at 30 and 60 days post implantationem. Based on these data, it can be concluded that the integration and/or degradation behavior of synthetic bone substitutes can be influenced by granule size.
Different types of raw cotton were investigated by a commercial ultraviolet-visible/near infrared (UV-Vis/NIR) spectrometer (210–2200 nm) as well as on a home-built setup for NIR hyperspectral imaging (NIR-HSI) in the range 1100–2200 nm. UV-Vis/NIR reflection spectroscopy reveals the dominant role proteins, hydrocarbons and hydroxyl groups play in the structure of cotton. NIR-HSI shows a similar result. Experimentally obtained data in combination with principal component analysis (PCA) provides a general differentiation of different cotton types. For UV-Vis/NIR spectroscopy, the first two principal components (PC) represent 82 % and 78 % of the total data variance for the UV-Vis and NIR regions, respectively. Whereas, for NIR-HSI, due to the large amount of data acquired, two methodologies for data processing were applied in low and high lateral resolution. In the first method, the average of the spectra from one sample was calculated and in the second method the spectra of each pixel were used. Both methods are able to explain ≥90 % of total variance by the first two PCs. The results show that it is possible to distinguish between different cotton types based on a few selected wavelength ranges. The combination of HSI and multivariate data analysis has a strong potential in industrial applications due to its short acquisition time and low-cost development. This study opens a novel possibility for a further development of this technique towards real large-scale processes.
Hyperspectral imaging and reflectance spectroscopy in the range from 200–380 nm were used to rapidly detect and characterize copper oxidation states and their layer thicknesses on direct bonded copper in a non-destructive way. Single-point UV reflectance spectroscopy, as a well-established method, was utilized to compare the quality of the hyperspectral imaging results. For the laterally resolved measurements of the copper surfaces an UV hyperspectral imaging setup based on a pushbroom imager was used. Six different types of direct bonded copper were studied. Each type had a different oxide layer thickness and was analyzed by depth profiling using X-ray photoelectron spectroscopy. In total, 28 samples were measured to develop multivariate models to characterize and predict the oxide layer thicknesses. The principal component analysis models (PCA) enabled a general differentiation between the sample types on the first two PCs with 100.0% and 96% explained variance for UV spectroscopy and hyperspectral imaging, respectively. Partial least squares regression (PLS-R) models showed reliable performance with R2c = 0.94 and 0.94 and RMSEC = 1.64 nm and 1.76 nm, respectively. The developed in-line prototype system combined with multivariate data modeling shows high potential for further development of this technique towards real large-scale processes.
UV hyperspectral imaging (225 nm–410 nm) was used to identify and quantify the honey- dew content of real cotton samples. Honeydew contamination causes losses of millions of dollars annually. This study presents the implementation and application of UV hyperspectral imaging as a non-destructive, high-resolution, and fast imaging modality. For this novel approach, a reference sample set, which consists of sugar and protein solutions that were adapted to honeydew, was set-up. In total, 21 samples with different amounts of added sugars/proteins were measured to calculate multivariate models at each pixel of a hyperspectral image to predict and classify the amount of sugar and honeydew. The principal component analysis models (PCA) enabled a general differentiation between different concentrations of sugar and honeydew. A partial least squares regression (PLS-R) model was built based on the cotton samples soaked in different sugar and protein concentrations. The result showed a reliable performance with R2cv = 0.80 and low RMSECV = 0.01 g for the valida- tion. The PLS-R reference model was able to predict the honeydew content laterally resolved in grams on real cotton samples for each pixel with light, strong, and very strong honeydew contaminations. Therefore, inline UV hyperspectral imaging combined with chemometric models can be an effective tool in the future for the quality control of industrial processing of cotton fibers.
Due to its wide-ranging endocrine functions, adipose tissue influences the whole body’s metabolism. Engineering long-term stable and functional human adipose tissue is still challenging due to the limited availability of suitable biomaterials and adequate cell maturation. We used gellan gum (GG) to create manual and bioprinted adipose tissue models because of its similarities to the native extracellular matrix and its easily tunable properties. Gellan gum itself was neither toxic nor monocyte activating. The resulting hydrogels exhibited suitable viscoelastic properties for soft tissues and were stable for 98 days in vitro. Encapsulated human primary adipose-derived stem cells (ASCs) were adipogenically differentiated for 14 days and matured for an additional 84 days. Live-dead staining showed that encapsulated cells stayed viable until day 98, while intracellular lipid staining showed an increase over time and a differentiation rate of 76% between days 28 and 56. After 4 weeks of culture, adipocytes had a univacuolar morphology, expressed perilipin A, and secreted up to 73% more leptin. After bioprinting establishment, we demonstrated that the cells in printed hydrogels had high cell viability and exhibited an adipogenic phenotype and function. In summary, GG-based adipose tissue models show long-term stability and allow ASCs maturation into functional, univacuolar adipocytes.
Adipose tissue is related to the development and manifestation of multiple diseases, demonstrating the importance of suitable in vitro models for research purposes. In this study, adipose tissue lobuli were explanted, cultured, and used as an adipose tissue control to evaluate in vitro generated adipose tissue models. During culture, lobule exhibited a stable weight, lactate dehydrogenase, and glycerol release over 15 days. For building up in vitro adipose tissue models, we adapted the biomaterial gelatin methacryloyl (GelMA) composition and handling to homogeneously mix and bioprint human primary mature adipocytes (MA) and adipose-derived stem cells (ASCs), respectively. Accelerated cooling of the bioink turned out to be essential for the homogeneous distribution of lipid-filled MAs in the hydrogel. Last, we compared manual and bioprinted GelMA hydrogels with MA or ASCs and the explanted lobules to evaluate the impact of the printing process and rate the models concerning the physiological reference. The viability analyses demonstrated no significant difference between the groups due to additive manufacturing. The staining of intracellular lipids and perilipin A suggest that GelMA is well suited for ASCs and MA. Therefore, we successfully constructed physiological in vitro models by bioprinting MA-containing GelMA bioinks.
Influence of the respirator on volatile organic compounds : an animal study in rats over 24 hours
(2015)
Long-term animal studies are needed to accomplish measurements of volatile organic compounds (VOCs) for medical diagnostics. In order to analyze the time course of VOCs, it is necessary to ventilate these animals. Therefore, a total of 10 male Sprague–Dawley rats were anaesthetized and ventilated with synthetic air via tracheotomy for 24 h. An ion mobility spectrometry coupled to multi-capillary columns (MCC–IMS) was used to analyze the expired air. To identify background contaminations produced by the respirator itself, six comparative measurements were conducted with ventilators only. Overall, a number of 37 peaks could be detected within the positive mode. According to the ratio peak intensity rat/ peak intensity ventilator blank, 22 peaks with a ratio >1.5 were defined as expired VOCs, 12 peaks with a ratio between 0.5 and 1.5 as unaffected VOCs, and three peaks with a ratio <0.5 as resorbed VOCs. The peak intensity of 12 expired VOCs changed significantly during the 24 h measurement. These results represent the basis for future intervention studies. Notably, online VOC analysis with MCC–IMS is possible over 24 h in ventilated rats and allows different experimental approaches.
The chemical recycling of used motor oil via catalytic cracking to convert it into secondary diesel-like fuels is a sustainable and technically attractive solution for managing environmental concerns associated with traditional disposal. In this context, this study was conducted to screen basic and acidic-aluminum silicate catalysts doped with different metals, including Mg, Zn, Cu, and Ni. The catalysts were thoroughly characterized using various techniques such as N2 adsorption–desorption isotherms, FT-IR spectroscopy, and TG analysis. The liquid and gaseous products were identified using GC, and their characteristics were compared with acceptable ranges from ASTM characterization methods for diesel fuel. The results showed that metal doping improved the performance of the catalysts, resulting in higher conversion rates of up to 65%, compared to thermal (15%) and aluminum silicates (≈20%). Among all catalysts, basic aluminum silicates doped with Ni showed the best catalytic performance, with conversions and yields three times higher than aluminum silicate catalysts. These findings significantly contribute to developing efficient and eco-friendly processes for the chemical recycling of used motor oil. This study highlights the potential of basic aluminum silicates doped with Ni as a promising catalyst for catalytic cracking and encourages further research in this area.
Fast pyrolysis as a valorization mechanism for banana rachis and low-density polyethylene waste
(2021)
Banana rachis and low-density polyethylene (LDPE) were selected as secondary feedstocks for the study of fast pyrolysis in a free-fall reactor. The experiments were performed at 600 °C for banana rachis and 450 °C for LDPE, based on literature and thermogravimetric analysis. The gaseous products of both feedstocks present similar composition in the C1-C2 compounds, while C3 compounds are only found in LDPE. The liquid products from banana and LDPE correspond to functional groups and shorter hydrocarbons, respectively. Scanning electron microscopy (SEM) and Fourier transform infrared (FTIR) analyses of the char showed important morphological changes to spheres in LDPE and structural changes due to thermal decomposition in the biomass. The pyrolysis char has high potential as adsorbent, encapsulation, or catalyst.
Characterization of low density polyethylene greenhouse films during the composting of rose residues
(2022)
This study presents an evaluation of a potential alternative to plastic degradation in the form of organic composting. It stems from the urgent need of finding solutions to the plastic residues and focuses on the compost-based degradation of greenhouse film covers in an important rose exporter company in Ecuador. Thus, this study analyzes the physical, chemical, and biological changes of rose wastes composting, and also evaluates the stability of new and aged agricultural plastic under these conditions. Interestingly, results of compost characterization show a slow degradation rate of organic matter and total organic carbon, along with a significant increase in pH and rise of bacterial populations. However, the results demonstrate that despite these findings, composting conditions had no significant influence on plastic degradation, and while deterioration of aged plastic samples was reported in some tests, it may be the result of environmental conditions and a prolonged exposure to solar radiation. Importantly, these factors could facilitate the adhesion of microorganisms and promote plastic biodegradation. Hence, it is encouraged for future studies to analyze the ecotoxicity of plastics in the compost, as well as isolate, identify, and evaluate the possible biodegradative potential of these microorganisms as an alternative to plastic waste management.
The effect of Hofmeister anions on the surface properties of polyelectrolyte multilayers built from hyaluronan and chitosan by layer-by-layer deposition is studied by ellipsometry and atomic force microscopy. The thickness, roughness and morphology of the resulting coatings were found to depend on the type of the anion. Relationship between the surface properties and the biological response of the polyelectrolyte multilayers is established by assessing the degree of protein (albumin) adsorption.
The properties of polyelectrolyte multilayers are ruled by the process parameters employed during self-assembly. This is the first study in which a design of experiment approach was used to validate and control the production of ultrathin polyelectrolyte multilayer coatings by identifying the ranges of critical process parameters (polyelectrolyte concentration, ionic strength and pH) within which coatings with reproducible properties (thickness, refractive index and hydrophilicity) are created. Mathematical models describing the combined impact of key process parameters on coatings properties were developed demonstrating that only ionic strength and pH affect the coatings thickness, but not polyelectrolyte concentration. While the electrolyte concentration had a linear effect, the pH contribution was described by a quadratic polynomial. A significant contribution of this study is the development of a new approach to estimate the thickness of polyelectrolyte multilayer nanofilms by quantitative rhodamine B staining, which might be useful in all cases when ellipsometry is not feasible due to the shape complexity or small size of the coated substrate. The novel approach proposed here overcomes the limitations of known methods as it offers a low spatial sampling size and the ability to analyse a wide area without restrictions on the chemical composition and shape of the substrate.
Controlling the surface properties and structure of thin nanosized coatings is of primary importance in diverse engineering and medical applications. Here we report on how the nanostructure, growth mechanism, thickness, roughness, and hydrophilicity of nanocomposites composed of weak natural or strong synthetic polyelectrolytes (PE) can be tailored by graphene oxide (GO) doping. GO reverses the build‐up mechanism affecting the internal structure and the hydrophilicity in a way depending on the type of the PE‐matrix. The extent of GO‐adsorption and its impact on the surface morphology was found to be independent on the type of the underlying PE‐matrix. The nanostructure of the hybrid films is not significantly altered when a single surface‐exposed GO‐layer is deposited, while increasing the number of embedded GO‐layers leads to pronounced surface heterogeneity. These results are expected to have valuable impact on the construction strategies of coatings with tunable surface properties.
Herein the optimization of the physicochemical properties and surface biocompatibility of polyelectrolyte multilayers of the natural, biocompatible and biodegradable, linear polysaccharides hyaluronan and chitosan by Hofmeister anions was systematically investigated. We demonstrated that there is an interconnection between the bulk and surface properties of HA/Chi multilayers both varying in accordance with the arrangement of the anions in the Hofmeister series. Kosmotropic anions increased the hydration, thickness, micro- and macro-roughness, and hydrophilicity and improved the biocompatibility of the films by reduction (2 orders of magnitude) of the films stiffness and complete anti-thrombogenicity.
This paper is concerned with the study, optimization and control of the moisture sorption kinetics of agricultural products at temperatures typically found in processing and storage. A nonlinear autoregressive with exogenous inputs (NARX) neural network was developed to predict moisture sorption kinetics and consequently equilibrium moisture contents of shiitake mushrooms (Lentinula edodes (Berk.) Pegler) over a wide range of relative humidity and different temperatures. Sorption kinetic data of mushroom caps was separately generated using a continuous, gravimetric dynamic vapour sorption analyser at emperatures of 25-40 °C over a stepwise variation of relative humidity ranging from 0 to 85%. The predictive power of the neural network was based on physical data, namely relative humidity and temperature. The model was fed with a total of 4500 data points by dividing them into three subsets, namely, 70% of the data was used for training, 15% of the data for testing and 15% of the data for validation, randomly selected from the whole dataset. The NARX neural network was capable of precisely simulating equilibrium moisture contents of mushrooms derived from the dynamic vapour sorption kinetic data throughout the entire range of relative humidity.
We report the temperature dependence of metal-enhanced fluorescence (MEF) of individual photosystem I (PSI) complexes from Thermosynechococcus elongatus (T. elongatus) coupled to gold nanoparticles (AuNPs). A strong temperature dependence of shape and intensity of the emission spectra is observed when PSI is coupled to AuNPs. For each temperature, the enhancement factor (EF) is calculated by comparing the intensity of individual AuNP-coupled PSI to the mean intensity of ‘uncoupled’ PSI. At cryogenic temperature (1.6 K) the average EF was 4.3-fold. Upon increasing the temperature to 250 K the EF increases to 84-fold. Single complexes show even higher EFs up to 441.0-fold. At increasing temperatures the different spectral pools of PSI from T. elongatus become distinguishable. These pools are affected differently by the plasmonic interactions and show different enhancements. The remarkable increase of the EFs is explained by a rate model including the temperature dependence of the fluorescence yield of PSI and the spectral overlap between absorption and emission spectra of AuNPs and PSI, respectively.
Thermoplastic polycarbonate urethane elastomers (TPCU) are potential implant materials for treating degenerative joint diseases thanks to their adjustable rubber-like properties, their toughness, and their durability. We developed a water-containing high-molecular-weight sulfated hyaluronic acid-coating to improve the interaction of TPCU with the synovial fluid. It is suggested that trapped synovial fluid can act as a lubricant that reduces the friction forces and thus provides an enhanced abrasion resistance of TPCU implants. Aims of this work were (i) the development of a coating method for novel soft TPCU with high-molecular sulfated hyaluronic acid to increase the biocompatibility and (ii) the in vitro validation of the functionalized TPCUs in cell culture experiments.
Knee osteoarthritis is a common complication and can lead to total loss of joint function in patients. Treatment by either partial or total knee replacement with appropriate UHMWPE based implantsis highly invasive, may cause complications and may show unsatisfying results. Alternatively, treatment may be done by insertion of an elastic interpositional knee spacer with optimized material characteristics.
We report the development of high performance polyurethane-based polymers modified with bioactive molecules for fabrication of such knee spacers. In order to tailor mechanical and tribological properties and to improve resist to enzymatic degradation we propose a core-shell model for the spacer with specifically adapted properties.
Polyurethane-bases block copolymers (TPCUs) are block-copolymers with systematically varied soft and hard segments. They have been suggested to serve as material for chondral implants in joint regeneration. Such applications may require the adhesion of chondrocytes to the implant surface, facilitating cell growth while keeping their phenotype. Thus, aims of this work were (1) to modify the surface of soft biostable polyurethane-based model implants (TPCU and TSiPCU) with high-molecular weight hyaluronic acid (HA) using an optimized multistep strategy of immobilization, and (2) to evaluate bioactivity of the modified TPCUs in vitro. Our results show no cytotoxic potential of the TPCUs. HAbioactive molecules (Mw =700kDa) were immobilized onto the polyurethane surface via polyethylenimine (PEI) spacers, and modifications were confirmed by several characterization methods. Tests with porcine chondrocytes indicated the potential of the TPCU-HA for inducing enhanced cell proliferation.
Background
Alzheimer’s disease (AD) is diagnosed based upon medical history, neuropsychiatric examination, cerebrospinal fluid analysis, extensive laboratory analyses and cerebral imaging. Diagnosis is time consuming and labour intensive. Parkinson’s disease (PD) is mainly diagnosed on clinical grounds.
Objective
The primary aim of this study was to differentiate patients suffering from AD, PD and healthy controls by investigating exhaled air with the electronic nose technique. After demonstrating a difference between the three groups the secondary aim was the identification of specific substances responsible for the difference(s) using ion mobility spectroscopy. Thirdly we analysed whether amyloid beta (Aβ) in exhaled breath was causative for the observed differences between patients suffering from AD and healthy controls.
Methods
We employed novel pulmonary diagnostic tools (electronic nose device/ion-mobility spectrometry) for the identification of patients with neurodegenerative diseases. Specifically, we analysed breath pattern differences in exhaled air of patients with AD, those with PD and healthy controls using the electronic nose device (eNose). Using ion mobility spectrometry (IMS), we identified the compounds responsible for the observed differences in breath patterns. We applied ELISA technique to measure Aβ in exhaled breath condensates.
Results
The eNose was able to differentiate between AD, PD and HC correctly. Using IMS, we identified markers that could be used to differentiate healthy controls from patients with AD and PD with an accuracy of 94%. In addition, patients suffering from PD were identified with sensitivity and specificity of 100%. Altogether, 3 AD patients out of 53 participants were misclassified. Although we found Aβ in exhaled breath condensate from both AD and healthy controls, no significant differences between groups were detected.
Conclusion
These data may open a new field in the diagnosis of neurodegenerative disease such as Alzheimer’s disease and Parkinson’s disease. Further research is required to evaluate the significance of these pulmonary findings with respect to the pathophysiology of neurodegenerative disorders.
The powder coating of veneered particle boards by the sequence electrostatic powder application -powder curing via hot pressing is studied in order to create high gloss surfaces. To obtain an appealingaspect, veneer Sheets were glued by heat and pressure on top of particle boards and the resulting surfaceswere used as carrier substrates for powder coat finishing. Prior to the powder coating, the veneeredparticle board surfaces were pre-treated by sanding to obtain good uniformity and the boards werestored in a climate chamber at controlled temperature and humidity conditions to adjust an appropriate electrical surface resistance. Characterization of surface texture was done by 3D microscopy. The surfaceelectrical resistance was measured for the six veneers before and after their application on the particleboard surface. A transparent powder top-coat was applied electrostatically onto the veneered particleboard surface. Curing of the powder was done using a heated press at 130◦C for 8 min and a smooth, glossy coating was obtained on the veneered surfaces. By applying different amounts of powder thecoating thickness could be varied and the optimum amount of powder was determined for each veneer type.
In the powder coating of veneered particle boards the highly reactive hybrid epoxy/polyester powder transparent Drylac 530 Series from TIGER Coatings GmbH & Co. KG, Wels, Austria was used. Curing is accelerated by a mixture of catalysts reaching curing times of 3 min at 150 °C or 5 min at 135 °C which allows for energy and time savings making Drylac Series 530 powder suitable for the coating of temperaturesensitive substrates such as MDF and wood.
Decorative laminates based on melamine formaldehyde (MF) resin impregnated papers are used at great extent for surface finishing of engineered wood that is used for furniture, kitchen, and working surfaces, flooring and exterior cladding. In all these applications, optically flawless appearance is a major issue. The work described here is focused on enhancing the cleanability and antifingerprint properties of smooth, matt surface-finished melamine-coated particleboards for furniture fronts, without at the same time changing or deteriorating other important surface parameters such as hardness, roughness or gloss. In order to adjust the surface polarity of a low pressure melamine film, novel interface-active macromolecular compounds were prepared and tested for their suitability as an antifingerprint additive. Two hydroxy-functional surfactants (polydimethysiloxane, PDMS-OH and perfluoroether, PF-OH) were oxidized under mild conditions to the corresponding aldehydes (PDMS-CHO and PF-CHO) using a pyridinium chlorochromate catalyst. With the most promising oxidized polymeric additive, PDMS-CHO, the contact angles against water, n-hexadecane, and squalene increased from 79.8°, 26.3° and 31.4° for the pure MF surface to 108.5°, 54.8°, and 59.3°, respectively, for the modified MF surfaces. While for the laminated MF surface based on the oxidized fluoroether the gloss values were much higher than required, for the surfaces based on oxidized polydimethylsiloxane the technological values as well as the lower gloss values were in agreement with the requirements and showed much improved surface cleanability, as was also confirmed by colorimetric measurements.
Unprecedented formation of sterically stabilized phospholipid liposomes of cuboidal morphology
(2021)
Sterically stabilized phospholipid liposomes of unprecedented cuboid morphology are formed upon introduction in the bilayer membrane of original polymers, based on polyglycidol bearing a lipid-mimetic residue. Strong hydrogen bonding in the polyglycidol sublayers creates attractive forces, which, facilitated by fluidization of the membrane, bring about the flattening of the bilayers and the formation of cuboid vesicles.
The present publication reports the purification effort of two natural bone blocks, that is, an allogeneic bone block (maxgraft®, botiss biomaterials GmbH, Zossen, Germany) and a xenogeneic block (SMARTBONE®, IBI S.A., Mezzovico Vira, Switzerland) in addition to previously published results based on histology. Furthermore, specialized scanning electron microscopy (SEM) and in vitro analyses (XTT, BrdU, LDH) for testing of the cytocompatibility based on ISO 10993-5/-12 have been conducted. The microscopic analyses showed that both bone blocks possess a trabecular structure with a lamellar subarrangement. In the case of the xenogeneic bone block, only minor remnants of collagenous structures were found, while in contrast high amounts of collagen were found associated with the allogeneic bone matrix. Furthermore, only island-like remnants of the polymer coating in case of the xenogeneic bone substitute seemed to be detectable. Finally, no remaining cells or cellular remnants were found in both bone blocks. The in vitro analyses showed that both bone blocks are biocompatible. Altogether, the purification level of both bone blocks seems to be favorable for bone tissue regeneration without the risk for inflammatory responses or graft rejection. Moreover, the analysis of the maxgraft® bone block showed that the underlying purification process allows for preserving not only the calcified bone matrix but also high amounts of the intertrabecular collagen matrix.
Introduction: Bioresorbable collagenous barrier membranes are used to prevent premature soft tissue ingrowth and to allow bone regeneration. For volume stable indications, only non-absorbable synthetic materials are available. This study investigates a new bioresorbable hydrofluoric acid (HF)-treated magnesium (Mg) mesh in a native collagen membrane for volume stable situations. Materials and Methods: HF-treated and untreated Mg were compared in direct and indirect cytocompatibility assays. In vivo, 18 New Zealand White Rabbits received each four 8 mm calvarial defects and were divided into four groups: (a) HF-treated Mg mesh/collagen membrane, (b) untreated Mg mesh/collagen membrane (c) collagen membrane and (d) sham operation. After 6, 12 and 18 weeks, Mg degradation and bone regeneration was measured using radiological and histological methods. Results: In vitro, HF-treated Mg showed higher cytocompatibility. Histopathologically, HF-Mg prevented gas cavities and was degraded by mononuclear cells via phagocytosis up to 12 weeks. Untreated Mg showed partially significant more gas cavities and a fibrous tissue reaction. Bone regeneration was not significantly different between all groups. Discussion and Conclusions: HF-Mg meshes embedded in native collagen membranes represent a volume stable and biocompatible alternative to the non-absorbable synthetic materials. HF-Mg shows less corrosion and is degraded by phagocytosis. However, the application of membranes did not result in higher bone regeneration.
Different sensor types using chemical and biochemical principles are described. The former are mainly gas sensors, the latter are applied especially to liquids. Those label-free direct detection methods are compared with applications where assays take advantage of labeled receptors.
Furthermore, selected applications in the area of gas sensors are discussed, and sensors for process control, point-of-care diagnostics, environmental analytics, and food analytics are reviewed. In addition, multiplexing approaches used in microplates and microarrays are described.
On account of the huge number of sensor types and the wide range of possible applications, only the most important ones are selected here.
Salivary gland tumors (SGTs) are a relevant, highly diverse subgroup of head and neck tumors whose entity determination can be difficult. Confocal Raman imaging in combination with multivariate data analysis may possibly support their correct classification. For the analysis of the translational potential of Raman imaging in SGT determination, a multi-stage evaluation process is necessary. By measuring a sample set of Warthin tumor, pleomorphic adenoma and non-tumor salivary gland tissue, Raman data were obtained and a thorough Raman band analysis was performed. This evaluation revealed highly overlapping Raman patterns with only minor spectral differences. Consequently, a principal component analysis (PCA) was calculated and further combined with a discriminant analysis (DA) to enable the best possible distinction. The PCA-DA model was characterized by accuracy, sensitivity, selectivity and precision values above 90% and validated by predicting model-unknown Raman spectra, of which 93% were classified correctly. Thus, we state our PCA-DA to be suitable for parotid tumor and non-salivary salivary gland tissue discrimination and prediction. For evaluation of the translational potential, further validation steps are necessary.
Glioblastoma WHO IV belongs to a group of brain tumors that are still incurable. A promising treatment approach applies photodynamic therapy (PDT) with hypericin as a photosensitizer. To generate a comprehensive understanding of the photosensitizer-tumor interactions, the first part of our study is focused on investigating the distribution and penetration behavior of hypericin in glioma cell spheroids by fluorescence microscopy. In the second part, fluorescence lifetime imaging microscopy (FLIM) was used to correlate fluorescence lifetime (FLT) changes of hypericin to environmental effects inside the spheroids. In this context, 3D tumor spheroids are an excellent model system since they consider 3D cell–cell interactions and the extracellular matrix is similar to tumors in vivo. Our analytical approach considers hypericin as probe molecule for FLIM and as photosensitizer for PDT at the same time, making it possible to directly draw conclusions of the state and location of the drug in a biological system. The knowledge of both state and location of hypericin makes a fundamental understanding of the impact of hypericin PDT in brain tumors possible. Following different incubation conditions, the hypericin distribution in peripheral and central cryosections of the spheroids were analyzed. Both fluorescence microscopy and FLIM revealed a hypericin gradient towards the spheroid core for short incubation periods or small concentrations. On the other hand, a homogeneous hypericin distribution is observed for long incubation times and high concentrations. Especially, the observed FLT change is crucial for the PDT efficiency, since the triplet yield, and hence the O2 activation, is directly proportional to the FLT. Based on the FLT increase inside spheroids, an incubation time 30 min is required to achieve most suitable conditions for an effective PDT.
The early detection of head and neck cancer is a prolonged challenging task. It requires a precise and accurate identification of tissue alterations as well as a distinct discrimination of cancerous from healthy tissue areas. A novel approach for this purpose uses microspectroscopic techniques with special focus on hyperspectral imaging (HSI) methods. Our proof-of-principle study presents the implementation and application of darkfield elastic light scattering spectroscopy (DF ELSS) as a non-destructive, high-resolution, and fast imaging modality to distinguish lingual healthy from altered tissue regions in a mouse model. The main aspect of our study deals with the comparison of two varying HSI detection principles, which are a point-by-point and line scanning imaging, and whether one might be more appropriate in differentiating several tissue types. Statistical models are formed by deploying a principal component analysis (PCA) with the Bayesian discriminant analysis (DA) on the elastic light scattering (ELS) spectra. Overall accuracy, sensitivity, and precision values of 98% are achieved for both models whereas the overall specificity results in 99%. An additional classification of model-unknown ELS spectra is performed. The predictions are verified with histopathological evaluations of identical HE-stained tissue areas to prove the model’s capability of tissue distinction. In the context of our proof-of-principle study, we assess the Pushbroom PCA-DA model to be more suitable for tissue type differentiations and thus tissue classification. In addition to the HE-examination in head and neck cancer diagnosis, the usage of HSI-based statistical models might be conceivable in a daily clinical routine.
Die Ionenmobilitätsspektrometrie ist eine gasanalytische Methode, die analytisch zwischen Sensoren auf der einen Seite und Spektrometern auf der anderen angesiedelt ist. Ihre Vorteile liegen darin, auch komplexere Gasgemische als Sensoren erfolgreich vor Ort und online sowie bettseitig im Krankenhaus analysieren zu können. Beispiele als dem Bereich Bio- und Prozessanalytik sollen die jeweiligen Ansätze und das Potential von der Fragestellung über die jeweils spezifische Lösung bis hin zum Ergebnis am Prozess exemplarisch zusammenstellen. Hierbei werden sowohl die analytische Sicht als auch die Marktsicht thematisiert.
The number of publications in the field of breath analysis using different types of ion mobility spectrometers (IMS) has increased over the last few years. In this paper, the publications between 2010 and 2013 are reviewed with respect to different types of IMS such as differential mobility spectrometers, high-field asymmetric waveform ion mobility spectrometers and multi-capillary columns coupled to conventional IMS. The analytes detected by IMS and declared with significance to a specific medical question were considered further with respect to medical and analytical questions. In total, 42 different analytes were found to be detected using IMS on a high significance level and were compared to findings using other analytical methods with respect to the individual analyte.
Background: Conventional methods for lung cancer detection including computed tomography (CT) and bronchoscopy are expensive and invasive. Thus, there is still a need for an optimal lung cancer detection technique. Methods: The exhaled breath of 50 patients with lung cancer histologically proven by bronchoscopic biopsy samples (32 adenocarcinomas, 10 squamous cell carcinomas, 8 small cell carcinomas), were analyzed using ion mobility spectrometry (IMS) and compared with 39 healthy volunteers. As a secondary assessment, we compared adenocarcinoma patients with and without epidermal growth factor receptor (EGFR) mutation. Results: A decision tree algorithm could separate patients with lung cancer including adenocarcinoma, squamous cell carcinoma and small cell carcinoma. One hundred-fifteen separated volatile organic compound (VOC) peaks were analyzed. Peak-2 noted as n-Dodecane using the IMS database was able to separate values with a sensitivity of 70.0% and a specificity of 89.7%. Incorporating a decision tree algorithm starting with n-Dodecane, a sensitivity of 76% and specificity of 100% was achieved. Comparing VOC peaks between adenocarcinoma and healthy subjects, n-Dodecane was able to separate values with a sensitivity of 81.3% and a specificity of 89.7%. Fourteen patients positive for EGFR mutation displayed a significantly higher n-Dodecane than for the 14 patients negative for EGFR (p<0.01), with a sensitivity of 85.7% and a specificity of 78.6%. Conclusion: In this prospective study, VOC peak patterns using a decision tree algorithm were useful in the detection of lung cancer. Moreover, n-Dodecane analysis from adenocarcinoma patients might be useful to discriminate the EGFR mutation.
Pre-clinical evaluation of advanced nerve guide conduits using a novel 3D in vitro testing model
(2018)
Autografts are the current gold standard for large peripheral nerve defects in clinics despite the frequently occurring side effects like donor site morbidity. Hollow nerve guidance conduits (NGC) are proposed alternatives to autografts, but failed to bridge gaps exceeding 3 cm in humans. Internal NGC guidance cues like microfibres are believed to enhance hollow NGCs by giving additional physical support for directed regeneration of Schwann cells and axons. In this study, we report a new 3D in vitro model that allows the evaluation of different intraluminal fibre scaffolds inside a complete NGC. The performance of electrospun polycaprolactone (PCL) microfibres inside 5 mm long polyethylene glycol (PEG) conduits were investigated in neuronal cell and dorsal root ganglion (DRG) cultures in vitro. Z-stack confocal microscopy revealed the aligned orientation of neuronal cells along the fibres throughout the whole NGC length and depth. The number of living cells in the centre of the scaffold was not significantly different to the tissue culture plastic (TCP) control. For ex vivo analysis, DRGs were placed on top of fibre-filled NGCs to simulate the proximal nerve stump. In 21 days of culture, Schwann cells and axons infiltrated the conduits along the microfibres with 2.2 ± 0.37 mm and 2.1 ± 0.33 mm, respectively. We conclude that this in vitro model can help define internal NGC scaffolds in the future by comparing different fibre materials, composites and dimensions in one setup prior to animal testing.
In thermopervaporation the same economically favorable driving force as in membrane distillation, i.e., a temperature difference between feed and permeate for the transport, is used but with non-porous thin-film composite membranes. Membrane pores cannot be wetted and long-term operational stability can be achieved with the appropriate coating layer, but normally with a decrease of the flux compared to membrane distillation with porous hydrophobic membranes.
Porous asymmetric PVDF membranes were made to achieve low permeation resistance and pores which could be overcoated with polyelectrolyte polymers. This coating prohibits pore wetting and strongly reduces adsorption of organic substances.
Those membranes showed a high permeation rate for water due to a structure of phase-separated hydrophilic and hydrophobic three-dimensional domains. The permeation rates of these composite membranes for water is between 6 and 12 l/(h m²) at a feed temperature of 60 °C and permeate at a temperature of 40 °C of a 2% saline solution feed depending on the operational parameters. This is only a slight reduction of 10–15% in permeation rate compared to membrane distillation with porous hydrophobic membranes.
In whey dewatering experiment this membrane showed a constant performance over 4 days in intermittent operation mode and stability in cleaning with strong alkaline solution.
A vapor permeation processes for the separation of aromatic compounds from aliphatic compounds
(2014)
A number of rubbery and glassy membranes have been prepared and evaluated in vapor permeation experiments for separation of aromatic/aliphatic mixtures, using 5/95 (wt:wt) toluene/methylcyclohexane (MCH) as a model solution. Candidate membranes that met the required toluene/MCH selectivity of ≥ 10 were identified. The stability of the candidate membranes was tested by cycling the experiment between higher toluene concentrations and the original 5 wt% level. The best membrane produced has a toluene permeance of 280 gpu and a toluene/MCH selectivity of 13 when tested with a vapor feed of the model mixture at its boiling point and at atmospheric pressure. When a series of related membrane materials are compared, there is a sharp trade-off between membrane permeance and membrane selectivity. A process design study based on the experimental results was conducted. The best preliminary membrane design uses 45% of the energy of a conventional distillation process.
Long-term stability of membranes in membrane distillation operation is a problem nowadays which prevents the industrial breakthrough of this separation process. Fouling or slow pore wetting are the basic reasons for this.
Membrane distillation membranes were made by NIPS process rendering the membrane asymmetrically to achieve low permeation resistance and pores which can be over coated with polyelectrolyte polymers thus leading to thermopervaporation membranes. Those membranes prohibit pore wetting and may strongly reduce resorption of organic substances on for membrane distillation typically used hydrophobic surfaces thus leading to longterm operation stability in dewatering including stable membrane cleaning.
Asymmetric PVDF membranes have been coated with cation exchange polyelectrolyte leading to a very thin, defect-free layer which has a high permeation rate for water due to the domain structure of phase-separated hydrophilic and hydrophobic three-dimensional structures.
Chronic obstructive pulmonary disease (COPD) is a chronic airway inflammatory disease characterized by incompletely reversible airway obstruction. This clinically heterogeneous group of patients is characterized by different phenotypes. Spirometry and clinical parameters, such as severity of dyspnea and exacerbation frequency, are used to diagnose and assess the severity of COPD. The purpose of this study was to investigate whether volatile organic compounds (VOCs) could be detected in the exhaled breath of patients with COPD and whether these VOCs could distinguish COPD patients from healthy subjects. Moreover, we aimed to investigate whether VOCs could be used as biomarkers for classifying patients into different subgroups of the disease. Ion mobility spectrometry was used to detect VOCs in the exhaled breath of COPD patients. One hundred and thirty-seven peaks were found to have a statistically significant difference between the COPD group and the combined healthy smokers and nonsmoker group. Six of these VOCs were found to correctly discriminate COPD patients from healthy controls with an accuracy of 70%. Only 15 peaks were found to be statistically different between healthy smokers and healthy nonsmokers. Furthermore, by determining the cutoff levels for each VOC peak, it was possible to classify the COPD patients into breathprint subgroups. Forced expiratory volume in 1 second, body mass index, and C-reactive protein seem to play a role in the discrepancies observed in the different breathprint subgroups.
Cell-cell and cell-extracellular matrix (ECM) adhesion regulates fundamental cellular functions and is crucial for cell-material contact. Adhesion is influenced by many factors like affinity and specificity of the receptor-ligand interaction or overall ligand concentration and density. To investigate molecular details of cell ECM and cadherins (cell-cell) interaction in vascular cells functional nanostructured surfaces were used Ligand-functionalized gold nanoparticles (AuNPs) with 6-8 nm diameter, are precisely immobilized on a surface and separated by non-adhesive regions so that individual integrins or cadherins can specifically interact with the ligands on the AuNPs. Using 40 nm and 90 nm distances between the AuNPs and functionalized either with peptide motifs of the extracellular matrix (RGD or REDV) or vascular endothelial cadherins (VEC), the influence of distance and ligand specificity on spreading and adhesion of endothelial cells (ECs) and smooth muscle cells (SMCs) was investigated. We demonstrate that RGD-dependent adhesion of vascular cells is similar to other cell types and that the distance dependence for integrin binding to ECM-peptides is also valid for the REDV motif. VEC-ligands decrease adhesion significantly on the tested ligand distances. These results may be helpful for future improvements in vascular tissue engineering and for development of implant surfaces.
A full understanding of the relationship between surface properties, protein adsorption, and immune responses is lacking but is of great interest for the design of biomaterials with desired biological profiles. In this study, polyelectrolyte multilayer (PEM) coatings with gradient changes in surface wettability were developed to shed light on how this impacts protein adsorption and immune response in the context of material biocompatibility. The analysis of immune responses by peripheral blood mononuclear cells to PEM coatings revealed an increased expression of proinflammatory cytokines tumor necrosis factor (TNF)-α, macrophage inflammatory protein (MIP)-1β, monocyte chemoattractant protein (MCP)-1, and interleukin (IL)-6 and the surface marker CD86 in response to the most hydrophobic coating, whereas the most hydrophilic coating resulted in a comparatively mild immune response. These findings were subsequently confirmed in a cohort of 24 donors. Cytokines were produced predominantly by monocytes with a peak after 24 h. Experiments conducted in the absence of serum indicated a contributing role of the adsorbed protein layer in the observed immune response. Mass spectrometry analysis revealed distinct protein adsorption patterns, with more inflammation-related proteins (e.g., apolipoprotein A-II) present on the most hydrophobic PEM surface, while the most abundant protein on the hydrophilic PEM (apolipoprotein A-I) was related to anti-inflammatory roles. The pathway analysis revealed alterations in the mitogen-activated protein kinase (MAPK)-signaling pathway between the most hydrophilic and the most hydrophobic coating. The results show that the acute proinflammatory response to the more hydrophobic PEM surface is associated with the adsorption of inflammation-related proteins. Thus, this study provides insights into the interplay between material wettability, protein adsorption, and inflammatory response and may act as a basis for the rational design of biomaterials.
Derzeit finden gravierende Veränderungen im Umfeld der Informations- und Kommunikationstechnik statt, die eine große Chance für die optimierte Prozessführung und Wertschöpfung mit darauf abgestimmten vernetzt kommunizierenden Sensoren bieten. Diese Art "smarter" Sensoren stellen Dienste innerhalb eines Netzwerks bereit und nutzen Informationen daraus. Dadurch ergibt sich aktuell die Notwendigkeit, die Anforderungen an Prozesssensoren sowie an deren Kommunikationsfähigkeiten detaillierter zu beschreiben – vom einfachen Temperatursensor bis über heute in Entwicklung befindlichen Messsystemen hinaus –, da diese Technologieentwicklungen rasant voranschreiten. Vernetzte Sensoren sind die Voraussetzung für die Realisierung von Cyberphysischen Produktionssystemen (CPPS) und zukünftiger Automatisierungskonzepte für die Prozessindustrie, wie sie auch durch das Zukunftsprojekt "Industrie 4.0" adressiert werden.
Die Technologie-Roadmap liefert darüber hinaus Perspektiven für Forschungs- und Entwicklungsförderung und gibt Ansätze für die Normungsarbeit. Sie wird damit auch für Politik, Industrieverbände und Gremien von Interesse sein. Wenn sich die Exzellenz der Forschung und das ausgeprägte Know-how der Gerätehersteller und Anwender zu Forschungskonsortien auf Augenhöhe zusammentun und das Wissen gemeinsam vorangebracht wird, kommen faire und gut durchdachte Technologietransferprojekte mit Sicherheit zum Erfolg. Neben der technologischen Weiterentwicklung der Prozesssensoren ist von Herstellern und Anwendern die hohe Verfügbarkeit der komplexen Technologie sicherzustellen, damit weiterhin Vertrauen in die Technik besteht – vom Anwender bis ins Management.
The article analyzes experimentally and theoretically the influence of microscope parameters on the pinhole-assisted Raman depth profiles in uniform and composite refractive media. The main objective is the reliable mapping of deep sample regions. The easiest to interpret results are found with low magnification, low aperture, and small pinholes. Here, the intensities and shapes of the Raman signals are independent of the location of the emitter relative to the sample surface. Theoretically, the results can be well described with a simple analytical equation containing the axial depth resolution of the microscope and the position of the emitter. The lower determinable object size is limited to 2–4 μm. If sub-micrometer resolution is desired, high magnification, mostly combined with high aperture, becomes necessary. The signal intensities and shapes depend now in refractive media on the position relative to the sample surface. This aspect is investigated on a number of uniform and stacked polymer layers, 2–160 μm thick, with the best available transparency. The experimental depth profiles are numerically fitted with excellent accuracy by inserting a Gaussian excitation beam of variable waist and fill fraction through the focusing lens area, and by treating the Raman emission with geometric optics as spontaneous isotropic process through the lens and the variable pinhole, respectively. The intersectional area of these two solid angles yields the leading factor in understanding confocal (pinhole-assisted) Raman depth profiles.
A laboratory prototype for hyperspectral imaging in ultra-violet (UV) region from 225 to 400 nm was developed and used to rapidly characterize active pharmaceutical ingredients (API) in tablets. The APIs are ibuprofen (IBU), acetylsalicylic acid (ASA) and paracetamol (PAR). Two sample sets were used for a comparison purpose. Sample set one comprises tablets of 100% API and sample set two consists of commercially available painkiller tablets. Reference measurements were performed on the pure APIs in liquid solutions (transmission) and in solid phase (reflection) using a commercial UV spectrometer. The spectroscopic part of the prototype is based on a pushbroom imager that contains a spectrograph and charge-coupled device (CCD) camera. The tablets were scanned on a conveyor belt that is positioned inside a tunnel made of polytetrafluoroethylene (PTFE) in order to increase the homogeneity of illumination at the sample position. Principal component analysis (PCA) was used to differentiate the hyperspectral data of the drug samples. The first two PCs are sufficient to completely separate all samples. The rugged design of the prototype opens new possibilities for further development of this technique towards real large-scale application.
Hypericin has large potential in modern medicine and exhibits fascinating structural dynamics, such as multiple conformations and tautomerization. However, it is difficult to study individual conformers/tautomers, as they cannot be isolated due to the similarity of their chemical and physical properties. An approach to overcome this difficulty is to combine single molecule experiments with theoretical studies. Time-dependent density functional theory (TD-DFT) calculations reveal that tautomerization of hypericin occurs via a two-step proton transfer with an energy barrier of 1.63 eV, whereas a direct single-step pathway has a large activation energy barrier of 2.42 eV. Tautomerization in hypericin is accompanied by reorientation of the transition dipole moment, which can be directly observed by fluorescence intensity fluctuations. Quantitative tautomerization residence times can be obtained from the autocorrelation of the temporal emission behavior revealing that hypericin stays in the same tautomeric state for several seconds, which can be influenced by the embedding matrix. Furthermore, replacing hydrogen with deuterium further proves that the underlying process is based on tunneling of a proton. In addition, the tautomerization rate can be influenced by a λ/2 Fabry–Pérot microcavity, where the occupation of Raman active vibrations can alter the tunneling rate.
An apparatus and method for analyzing a flow of material having an inlet region, a measurement range and an outlet region, and having a first diverter and a second diverter, and a deflection area, wherein in a first state of operation, the two diverters form a continuous first material flow space from the inlet region via the first diverter through the measurement range, via the second diverter to the outlet region, and in a second state of operation, form a continuous second material flow space from the inlet region via the first diverter through the deflection area, via the second diverter to the outlet region.
Die Erfindung betrifft eine Vorrichtung und Verfahren zur Analyse eines Materialstroms S mit einem Einlassbereich E, einem Messbereich M und einen Auslassbereich A sowie mit einer ersten Weiche W1 und einer zweiten Weiche W2 und einem Umlenkbereich U, wobei die beiden Weichen W1, W2 in einem ersten Schaltzustand Z1 einen durchgängigen ersten Materialdurchströmungsraum vom Einlassbereich E über die erste Weiche W1 durch den Messbereich M über die zweite Weiche W2 bis zum Auslassbereich A ausbilden und in einem zweiten Schaltzustand einen durchgängigen zweiten Materialdurchströmungsraum vom Einlassbereich E über die erste Weiche W1 durch den Umkenkbereich U über die zweite Weiche W2 bis zum Auslassbereich A ausbilden.
Die Erfindung betrifft eine Vorrichtung und Verfahren zur Analyse eines Materialstroms (S) mit einem Einlassbereich (E), einem Messbereich (M) und einen Auslassbereich (A) sowie mit einer ersten Weiche (W1) und einer zweiten Weiche (W2) und einem Umlenkbereich (U), wobei die beiden Weichen (W1, W2) in einem ersten Schaltzustand (Z1) einen durchgängigen ersten Materialdurchströmungsraum vom Einlassbereich (E) über die erste Weiche (W1) durch den Messbereich (M) über die zweite Weiche (W2) bis zum Auslassbereich (A) ausbilden und in einem zweiten Schaltzustand einen durchgängigen zweiten Materialdurchströmungsraum vom Einlassbereich (E) über die erste Weiche (W1) durch den Umlenkbereich (U) über die zweite Weiche (W2) bis zum Auslassbereich (A) ausbilden.
Die kontinuierliche Erfassung von Qualitätsparametern ist eine zunehmende Anforderung in der Polymerextrusion. Die optische Spektroskopie kann diese Anforderung erfüllen, da sie neben der Farbe weitere Parameter wie beispielsweise chemische Eigenschaften, Trübungsgrad oder Partikelgröße erfasst. Dabei werden für Inline-Messungen im Extruder optische Sonden eingesetzt. Im laufenden Betrieb bilden sich Ablagerungen auf den Sondenfenstern. Dieser Beitrag präsentiert ein neues Cleaning in Place Konzept, mit dessen Hilfe die Fenster auch während der Produktion ohne Unterbrechung gereinigt werden können. Auch die Kalibrierung der Messtechnik ist dabei möglich. Das verhindert Rüstzeiten und sichert eine kontinuierliche Inline-Messung.