Chemische Charakterisierung und Spurenanalytik
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Eingeladener Vortrag
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Today, in scientific events often a certain separation between researchers from laboratories with highly sophisticated equipment and those from less privileged laboratories can be observed. It is not an uncommon situation that results presented at conferences are rubbished or ridiculed because the investigator only used low-end analytical methods.
The assessment of the study is then biased based on the equipment, regardless of the actual quality of the study.
The efficiency, relatively low cost and eco-friendly nature of hydrogen peroxide-assisted photocatalysis treatment procedures are significant advantages over conventional techniques for wastewater remediation. Herein, we evaluate the behaviour of g-cyclodextrin (g-CD) immobilised on either bare or chitosan (CS)–functionalised Fe3O4 nanoparticles, for photodegrading Bisphenol A (BPA) in ultrapure water and in real wastewater samples. The BPA removal efficiencies with Fe3O4/g-CD and Fe3O4/CS/g-CD were compared with those of Fe3O4/b-CD, and were monitored under UVA irradiation at near-neutral pH. The addition of H2O2 at low concentrations (15 mmol L-1) significantly increased BPA photodegradation in the presence of each nanocomposite. The highest catalytic activity was shown by both Fe3O4/g-CD and Fe3O4/CS/g-CD nanocomposites (,60 and 27%BPA removal in ultrapure water and real wastewater effluent, respectively). Our findings reveal the superior performance of g-CD-functionalised Fe3O4 relative to that of Fe3O4/b-CD. The use of CD-based nanocomposites as photocatalytic materials could be an attractive option in the pre- or post-treatment stage of wastewaters by advanced oxidation processes before or after biological treatment.
Cancer cell lipid class homeostasis is altered under nutrient-deprivation but stable under hypoxia
(2019)
Background: Cancer cells modify the balance between fatty acid (FA) synthesis and uptake under metabolic stress, induced by oxygen/nutrient deprivation. These modifications were shown to alter the levels of individual triglyceride (TG) or phospholipid sub-species. To attain a holistic overview of the lipidomic profiles of cancer cells under stress we performed a broad lipidomic assay, comprising 244 lipids from six major classes. This assay allowed us to perform robust analyses and assess the changes in averages of broader lipid-classes, stratified on the basis of saturation index of their fatty-acyl side chains.
Methods: Global lipidomic profiling using Liquid Chromatography-Mass Spectrometry was performed to assess lipidomic profiles of biologically diverse cancer cell lines cultivated under metabolically stressed conditions.
Results: Neutral lipid compositions were markedly modified under serum-deprived conditions and, strikingly, the cellular level of triglyceride subspecies decreased with increasing number of double bonds in their fatty acyl chains.
In contrast and unexpectedly, no robust changes were observed in lipidomic profiles of hypoxic (2% O2) cancer cells despite concurrent changes in proliferation rates and metabolic gene expression.
Conclusions: Serum-deprivation significantly affects lipidomic profiles of cancer cells. Although, the levels of individual lipid moieties alter under hypoxia (2% O2), the robust averages of broader lipid classes remain unchanged.
Regardless of its ban in agricultural use, the triazine derivative terbutryn is still used as a biocide against biofouling in building materials, such as façade colors and roof tiles. From there, it is washed off and may contaminate soil and surface waters, where it shows ecotoxicological behavior. For understanding of these leaching processes, analytical methods that can detect terbutryn in traces are necessary. In contrast to separation methods (Gas (GC) or liquid chromatography (LC)) coupled to mass spectrometry (MS), enzyme immunoassays (EIAs) have proven to be adequate tools for environmental monitoring. Compared to GC-or LC-MS, they are cheap, require only limited time and experimental expertise and enable high throughput. For quantification of terbutryn, EIAs have been established, with a limit of detection (LOD) of 50 ng L-1. For leaching experiments however, a lower LOD would be advantageous.
For detection of terbutryn we developed a direct competitive ELISA based on a monoclonal antibody: Terbutryn and an enzyme-terbutryn conjugate (“tracer”) compete for the binding sites of the immobilized antibody. The bound tracer converts a colourless substrate into a blue-coloured product, which can be detected via spectrophotometry. For quantification of terbutryn, a sigmoidal calibration curve is used. For establishing of the EIA, a new tracer based on a terbutryn surrogate (“hapten”) was synthesized. After optimization of the experimental conditions, the immunoassay exhibited a more than ten-fold increased sensitivity (LOD: 3 ng L-1), high stability against sample compounds (Ca2+, NaCl) and lower cross-reactivities against structurally related compounds, than reported before. Analysis of spiked samples was possible with high precision (inter-assay CV: < 10 %) and accuracy (recoveries from spiked samples: 89 % ± 10%). We therefore propose it as quick and reliable method for leaching studies of terbutryn out of building materials.
The development of an automated miniaturized analytical system that allows for the rapid monitoring of carbamazepine (CBZ) levels in serum and wastewater is proposed. Molecular recognition of CBZ was achieved through its selective interaction with microbeads carrying anti-CBZ antibodies. The proposed method combines the advantages of the micro-bead injection spectroscopy and of the flow-based platform lab-on-valve for implementation of automatic immunosorbent renewal, rendering a new recognition surface for each sample. The sequential (or simultaneous) perfusion of CBZ and the horseradish peroxidase-labelled CBZ through the microbeads is followed by real-time on-column Monitoring of substrate (3,30,5,50-tetramethylbenzidine) oxidation by colorimetry. The evaluation of the initial oxidation rate and also the absorbance value at a fixed time point provided a linear response versus the logarithm of the CBZ concentration. Under the selected assay conditions, a single analysis was completed after only 11 min, with a quantification range between 1.0 and 50 µg L⁻¹. Detection of CBZ levels in undiluted wastewater samples was feasible after a simple filtration step while good recoveries were attained for spiked certified human serum, analyzed without sample clean-up.
We present the optical sensing of phthalate Esters (PAEs), a group of endocrine-disrupting chemicals. The sensing takes place as changes in the fluorescence emission intensity of aminopyrene covalently bound to the organic ligands of the metal−organic framework compound ZIF-8. In the presence of PAEs, a quenching of the fluorescence emission is observed. We evaluated strategies to engineer colloidal size distribution of the sensing particles to optimize the sensory response to PAEs. A thorough characterization of the modified ZIF-8 nanoparticles included powder X-ray diffractometry, transmission electron microscopy, high-performance liquid chromatography, and photophysical characterization. The presented capability of the fluorophore-functionalized ZIF-8 to sense PAEs complements established methods such as chromatography-based procedures, which cannot be used on-site and paves the way for future developments such as hand-held quick sensing devices.