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51.
Wan H Holmén AG Wang Y Lindberg W Englund M Någård MB Thompson RA 《Rapid communications in mass spectrometry : RCM》2003,17(23):2639-2648
A high-throughput pKa screening method based on pressure-assisted capillary electrophoresis (CE) and mass spectrometry (MS) is presented. Effects of buffer type and ionic strength on sensitivity and pKa values were investigated. Influence of dimethyl sulfoxide (DMSO) concentration present in the sample on effective mobility measurement was examined. A series of ten volatile buffers, covering a pH range from 2.5 to 10.5 with the same ionic strength, was employed. The application of volatile background electrolytes resulted in significant signal increase as compared with commonly used non-volatile phosphate buffers. In general, the CE/MS system provided a ten-fold higher sensitivity than conventional UV detection. The newly developed CE/MS method offers high-throughput capacity by pooling a number of compounds into a single sample. Simultaneous measurement of more than 50 compounds was readily achieved in less than 150 min. The measured pKa values are consistent with the published data obtained from the CE/UV method and are also in good agreement with data generated by other methods. Other advantages of using CE/MS for pKa screening are illustrated with typical examples, including poorly soluble compounds and non-UV-absorbing compounds. 相似文献
52.
Pretreatment of polystyrene beads with a nonpolar organic solvent is the key for the generation of mechanically robust tablets consisting of neat functionalized polystyrene beads, both alone and in combination with solid reagents or catalysts. The novel dosing methodology provides accurately preweighed tablets in virtually any shape and size and with excellent disintegration properties, speeding up parallel solution and solid phase synthesis. The use of tablets is demonstrated in parallel Mitsunobu and acylation reactions. 相似文献
53.
We consider a fifth-order partial differential equation (PDE) that is a generalization of the integrable Camassa–Holm equation. This fifth-order PDE has exact solutions in terms of an arbitrary number of superposed pulsons with a geodesic Hamiltonian dynamics that is known to be integrable in the two-body case N==2. Numerical simulations show that the pulsons are stable, dominate the initial value problem, and scatter elastically. These characteristics are reminiscent of solitons in integrable systems. But after demonstrating the nonexistence of a suitable Lagrangian or bi-Hamiltonian structure and obtaining negative results from Painlevé analysis and the Wahlquist–Estabrook method, we assert that this fifth-order PDE is not integrable. 相似文献
54.
We report a mechanism which can lead to long-range attractions between like-charged spherical macroions, stemming from the existence of metastable ionized states. We show that the ground state of a single highly charged colloid plus a few excess counterions is overcharged. For the case of two highly charged macroions in their neutralizing divalent counterion solution we demonstrate that, in the regime of strong Coulomb coupling, the counterion clouds are very likely to be unevenly distributed, leading to one overcharged and one undercharged macroion. This long-living metastable configuration in turn leads to a long-range Coulomb attraction. 相似文献
55.
The recent discovery of a new solid phase of carbon dioxide ( CO2-V) has made it apparent that the properties of this vital chemical species are drastically altered under high pressure conditions. The reported transition at around 40 GPa from the Cmca phase ( CO2-III), which is a molecular solid, into the novel phase, which was observed to be quartzlike, clearly suggests a dramatic change of the chemical, electronic, and structural properties. We here present a theoretical analysis of the implications of this metamorphosis. At even higher pressures, we predict the existence of a very hard phase of the stishovite type. 相似文献
56.
57.
Bhowmik Siddhartha Holm Arliena Ostroverkhova Oksana Atre Sundar 《Applied Physics A: Materials Science & Processing》2011,103(4):1117-1123
Metal nanostructures are of considerable interest in the field of plasmonics and metamaterials and could have a wider impact
if they are successfully embedded in a stable, inert and flexible polymer matrix. Fabrication of such structures is challenging
for a variety of reasons including thermal stability, material compatibility with processing steps and general handling of
material. In this work we have demonstrated the fabrication of metal nanostructures and embedded them in a polymer. Furthermore,
these structures were fabricated on a flexible polymer membrane and detached from a carrier substrate. Characterization of
these structures was performed with SEM, TEM and EDS. 相似文献
58.
Cellobiose dehydrogenase activity (0.25–1 U Ml?1) is monitored by oxidation of cellobiose to cellobionolactone, thus reducing 2,6-dichlorophenolindophenol to a colourless compound. To prevent any β-glucosidase from reacting, gluconolactone is added as inhibitor. The sample throughput is 120 h?1. 相似文献
59.
Targeted analysis of protein citrullination using chemical modification and tandem mass spectrometry
Maria Stensland Anders Holm Andrea Kiehne Burkhard Fleckenstein 《Rapid communications in mass spectrometry : RCM》2009,23(17):2754-2762
Protein citrullination originates from enzymatic deimination of polypeptide‐bound arginine and is involved in various biological processes during health and disease. However, tools required for a detailed and targeted proteomic analysis of citrullinated proteins in situ, including their citrullination sites, are limited. A widely used technique for detection of citrullinated proteins relies on antibody staining after specific derivatization of citrulline residues by 2,3‐butanedione and antipyrine. We have recently reported on the details of this reaction. Here, we show that this chemical modification can be utilized to specifically detect and identify citrullinated peptides and their citrullination sites by liquid chromatography/tandem mass spectrometry (LC/MS/MS) analysis. Using model compounds, we demonstrate that in collision‐induced dissociation (CID) a specific, modification‐derived fragment ion appears as the dominating signal at m/z 201.1 in the MS/MS spectra. When applying electron transfer dissociation (ETD), however, the chemical modification of citrulline remained intact and extensive sequence coverage allowed identification of peptides and their citrullination sites. Therefore, LC/MS/MS analysis with alternating CID and ETD has been performed, using CID for specific, signature ion‐based detection of derivatized citrullinated peptides and ETD for sequence determination. The usefulness of this targeted analysis was demonstrated by identifying citrullination sites in myelin basic protein deiminated in vitro. Combining antibody‐based enrichment of chemically modified citrulline‐containing peptides with specific mass spectrometric detection will increase the potential of such a targeted analysis of protein citrullination in the future. Copyright © 2009 John Wiley & Sons, Ltd. 相似文献
60.