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Behrens MA Lopez M Kjøniksen AL Zhu K Nyström B Pedersen JS 《Langmuir : the ACS journal of surfaces and colloids》2012,28(2):1105-1114
A series of thermo-responsive cationic triblock copolymers composed of methoxy-poly(ethylene glycol) (MPEG, hydrophilic), poly(N-isopropylacrylamide) (PNIPAAM, temperature sensitive), and poly((3-acrylamidopropyl) trimethyl ammonium chloride) (PN(+), cationic) has been investigated as a function of temperature and ionic strength. In the MPEG-b-PNIPAAM-b-PN(+) copolymers, the MPEG block length is constant, and the lengths of the PNIPAAM and PN(+) blocks are varied. The solubility of the PNIPAAM block decreases with increasing temperature, and the triblock copolymer thus provides the possibilities of studying micelles with both neutral and charged blocks in the micelle corona as well as the interplay between these two blocks as the electrostatic interactions are varied by addition of salt. Investigation of the systems by densitometry and small-angle X-ray scattering (SAXS) in a temperature range from 20 to 70 °C gave detailed information on the behavior both below and above the critical micelle temperature (CMT). A clear effect of the addition of salt is observed in both the apparent partial specific volume, obtained from the densitometry measurements, and the SAXS data. Below the CMT, the single polymers can be described as Gaussian chains, for which the repulsive interchain interactions, originating from the charged PN(+) block, have to be taken into account in salt-free aqueous solution. Increasing the salt concentration of the solution to 30 mM NaCl leads to an increase in the apparent partial specific volume, and the electrostatic repulsive interchain interactions between the single polymers vanish. Raising the temperature results in micelle formation, except for the copolymer with only 20 NIPAAM units. The SAXS data show that the polymer with the medium PNIPAAM block length forms spherical micelles, whereas the polymer with the longest PNIPAAM block forms cylindrical micelles. Increasing the temperature further above the CMT results in an increase in the micellar aggregation number for both of the polymers forming spherical and cylindrical micelles. The addition of salt to the solution also influences the aggregates formed above the CMT. Overall, the micelles formed in the salt solution have a smaller cross-section radius than those in aqueous solution without added salt. 相似文献
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Mikhail M. Savitski Frank Fischer Toby Mathieson Gavain Sweetman Manja Lang Marcus Bantscheff 《Journal of the American Society for Mass Spectrometry》2010,21(10):1668-1679
Quantitative mass spectrometry-based proteomic assays often suffer from a lack of robustness and reproducibility. We here
describe a targeted mass spectrometric data acquisition strategy for affinity enriched subproteomes—in our case the kinome—that
enables a substantially improved reproducibility of detection, and improved quantification via isobaric tags. Inclusion mass
lists containing m/z, charge state, and retention time were created based on a set of 80 shotgun-type experiments performed under identical experimental
conditions. For each target protein, peptides were selected according to their frequency of observation and isobaric tag for
relative and absolute quantitation (iTRAQ) reporter ion quality. Retention times of selected peptides were aligned using similarity
driven pairwise alignment strategy yielding <1 min standard deviation for 4 h gradients. Multiple fragmentation of the same
peptides resulted in better statistics and more precise reporter ion based quantification without any loss in coverage. Overall,
24% more target proteins were quantified using the targeted data acquisition approach, and precision of quantification improved
by >1.5-fold. We also show that a combination of higher energy collisional dissociation (HCD) with collisional induced dissociation
(CID) outperformed pulsed-Q-dissociation (PQD) on the OrbitrapXL. With the CID/ HCD based targeted data acquisition approach
10% more quantifiable target proteins were identified and a 2-fold increase in quantification precision was achieved. We have
observed excellent reproducibility between different instruments, underlining the robustness of the approach. 相似文献
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Manja Kubeil Dr. Holger Stephan Dr. Hans‐Jürgen Pietzsch Dr. Gerhard Geipel Dr. Dietmar Appelhans Prof. Dr. Brigitte Voit Jan Hoffmann Prof. Dr. Bernhard Brutschy Dr. Yuri V. Mironov Dr. Konstantin A. Brylev Prof. Dr. Vladimir E. Fedorov 《化学:亚洲杂志》2010,5(12):2507-2514
The encapsulation of a nanometer‐sized octahedral anionic rhenium cluster complex with six terminal hydroxo ligands [Re6S8(OH)6]4? in maltose‐decorated poly(propylene amine) dendrimers (POPAM, generation 4 and 5) has been investigated. Ultrafiltration experiments showed that maximal loading capacity of the dendrimers with the cluster complex is achieved after about ten hours in aqueous solution. To study the inclusion phenomena, three different methods have been applied: UV/Vis, time‐resolved laser‐induced fluorescence spectroscopy (TRLFS), and laser‐induced liquid bead ion desorption mass spectrometry (LILBID‐MS). From the results obtained, it could be concluded that: a) the hydrolytic stability of the rhenium cluster complex is significantly enhanced in the presence of dendritic hosts; b) the cluster anions are preferentially bound inside the dendrimers; c) the number of cluster complexes encapsulated in the dendrimers increases with rising dendrimer generation. On average, four to five cluster anions can preferentially be captured in the interior of sugar‐coated dendritic carriers. An asymptotic progression of the release of cluster complexes from the loaded dendrimers was observed under physiologically relevant conditions (isotonic sodium chloride solution: approximately 93 % within 4 days for loaded POPAM‐G4‐maltose; approximately 86 % within 4 days for loaded POPAM‐G5‐maltose). These encapsulation and release properties of maltose‐decorated nanocarriers imply the possibility for the development of the next generation of dendritic nanocarriers with specific targeting of destined tissue for therapeutic treatments. 相似文献
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Dr. Manja Kubeil Dr. Tanmaya Joshi Prof. Bayden R. Wood Dr. Holger Stephan 《ChemistryOpen》2019,8(5):637-642
A photoactivatable ruthenium(II) carbonyl complex mer,cis-[Ru(II)Cl(BisQ)(CO)2]PF6 2 was prepared using a tridentate bisquinoline ligand (BisQ=(2,6-diquinolin-2-yl)pyridin). Compound 2 was thoroughly characterized by standard analytical methods and single crystal X-ray diffraction. The crystal structure of the complex cation reveals a distorted octahedral geometry. The decarbonylation upon exposure to 350 and 420 nm light was monitored by UV/VIS absorbance and Fourier transform infrared spectroscopies in acetonitrile and 1 % (v/v) DMSO in water, respectively. The kinetic of the photodecarbonylation has been elucidated by multivariate curve resolution alternating least-squares analysis. The stepwise decarbonylation follows a serial mechanism. The first decarbonylation occurs very quickly whereas the second decarbonylation step proceeds more slowly. Moreover, the second rate constant is lower in 1 % (v/v) DMSO in water than in acetonitrile. In comparison to 350 nm irradiation, exposure to 420 nm light in acetonitrile results in a lower second rate constant. 相似文献
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Doreen M Reich Susann Hau Tobias Stahl Markus Scholz Wilfried Naumann Frank Emmrich Johannes Boltze Manja Kamprad 《BMC neuroscience》2008,9(1):91
Background
The therapeutic capacity of human umbilical cord blood mononuclear cells (HsUCB-MNC) and stem cells derived thereof is documented in animal models of focal cerebral ischemia, while mechanisms behind the reduction of lesion size and the observed improvement of behavioral skills still remain poorly understood. 相似文献19.
Intrauterine growth restriction (IUGR) is defined as a condition in which the fetus does not reach its genetically given growth potential, resulting in low birth weight. IUGR is an important cause of perinatal morbidity and mortality, thus contributing substantially to medically indicated preterm birth in order to prevent fetal death. We subjected umbilical cord blood serum samples either belonging to the IUGR group (n = 15) or to the control group (n = 15) to fractionation by affinity chromatography using a bead system with hydrophobic interaction capabilities. So prepared protein mixtures were analyzed by MALDI-TOF mass spectrometric profiling. The six best differentiating ion signals at m/z 8205, m/z 8766, m/z 13 945, m/z 15 129, m/z 15 308, and m/z 16 001 were collectively assigned as IUGR proteome signature. Separation confidence of our IUGR proteome signature reached a sensitivity of 0.87 and a specificity of 0.93. Assignment of ion signals in the mass spectra to specific proteins was substantiated by SDS-PAGE in conjunction with peptide mass fingerprint analysis of cord blood serum proteins. One constituent of this proteome signature, apolipoprotein C-III(0) , a derivative lacking glycosylation, has been found more abundant in the IUGR cord blood serum samples, irrespective of gestational age. Hence, we suggest apolipoprotein C-III(0) as potential key-marker of the here proposed IUGR proteome signature, as it is a very low-density lipoprotein (VLDL) and high-density lipoprotein (HDL) member and as such involved in triglyceride metabolism that itself is discussed as being of importance in IUGR pathogenesis. Our results indicate that subtle alterations in protein glycosylation need to be considered for improving our understanding of the pathomechanisms in IUGR. 相似文献
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Susann Barig Manja Schiemann Vladimir M. Mirsky K. Peter Stahmann 《Analytical and bioanalytical chemistry》2013,405(26):8539-8547
A clearing assay for lipolytic enzymes has been realized in 96-well microtiter plates. A thin layer containing emulsified tributyrin as turbidity-generating substrate was placed on a thicker supporting aqueous layer. Both layers were stabilized by a gel-forming agent. Enzyme addition leads to clearing of the emulsion detected with a standard microtiter plate reader as a decrease of extinction. Dependencies of the signal kinetics on the substrate and enzyme concentrations were studied. For 0.5–1 % tributyrin content the reaction rate is not substrate-limited. An initial slope of the signal kinetics is proportional to the lipase activity. A detailed characterization of the assay was performed. Lipolysis of tributyrin was confirmed by glycerol detection. Various gel-forming agents were compared and diffusion conditions in these gels were analyzed. Agar and agarose were found to be the most suitable gel-forming agents, which do not affect enzyme diffusion whereas polyacrylamide gels block lipase diffusion and therefore are not suitable for the assay. The optimized assay prepared from 1 % tributyrin emulsion in 2 % agar gel was tested with six microbial lipases and porcine pancreatic lipase. The detection limit is 20–60 ng/well which is equivalent to 30 μU/well for T. lanuginosus lipase. Figure
A clearing assay for lipolytic enzymes has been realized in 96-well microtiter plates. A thin layer containing emulsified tributyrin as turbidity-generating substrate was placed on a thicker supporting aqueous layer. Both layers are stabilized by a gel-forming agent. Enzyme addition leads to clearing of the emulsion detected with a standard microtiter plate reader as a decrease of extinction 相似文献