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141.
Immobilisation and evaluation of a vancomycin chiral stationary phase for capillary electrochromatography 总被引:2,自引:0,他引:2
The macrocyclic antibiotic, vancomycin, is covalently bonded to LiChrospher diol silica packed columns and evaluated in capillary electrochromatography (CEC) both in the reversed-phase and polar organic mode. Initially, capillaries were packed with 5 microm LiChrospher 100 A diol silica and evaluated in CEC with a reversed-phase biphenyl-pyrene achiral test resulting in resolution and efficiency values of ca. 2.5 and 100000 plates meter(-1), respectively. Repeatability for this test (resolution and efficiency) was also examined and found to be acceptable for both run-to-run (n=5, 0.74% and 1.5%) and column-to-column (n=5, 3.4% and 9.0%), respectively. Similar results were obtained when the 10 microm LiChrospher 1000 A diol silica was examined with the exception of efficiency, where a reduced plate height value of four times lower was obtained compared to the 100 A material. A simple three step in-situ vancomycin immobilisation procedure was subsequently carried out on these packed diol columns. Selectivity was obtained for thalidomide enantiomers on this vancomycin chiral stationary phase in reversed-phase CEC with resolution and efficiency values of ca. 2.5 and 80000 plates meter(-1), with acceptable repeatability (n=8) 0.9% and 3.0%, respectively. Selectivity was also obtained for thalidomide enantiomers on this phase in the polar organic mode with resolution and efficiency values of ca. 2.5 and 120000 plates meter(-1), with acceptable repeatability (n=7) 0.9% and 2.0%, respectively. It was possible to deduce from a chemometric design carried out for evaluating the mobile phase component effects that organic modifier ratio, MeOH/MeCN, played a significant role in controlling both resolution and efficiency. It was also possible to separate a number of basic analytes including four beta-adrenergic blocking agents in the polar organic mode albeit with lower resolution and efficiency values, ca. 1.5 and 45000 plates meter(-1), respectively. 相似文献
142.
Investigations of electrospray sample deposition for polymer MALDI mass spectrometry 总被引:2,自引:0,他引:2
Hanton SD Hyder IZ Stets JR Owens KG Blair WR Guttman CM Giuseppetti AA 《Journal of the American Society for Mass Spectrometry》2004,15(2):168-179
In the interest of a more thorough understanding of the relationship between sample deposition technique and the quality of data obtained using matrix-assisted laser desorption/ionization (MALDI) mass spectrometry, details of the electrospray (ES) process of sample deposition are investigated using a number of techniques. Sample morphology was observed with scanning electron microscopy (SEM) and atomic force microscopy (AFM), while matrix-enhanced secondary ion mass spectrometry (MESIMS) monitored surface coverage. Electrospray deposition reduces the analyte segregation that can occur during traditional dried droplet deposition for MALDI. We attribute statistically significant improvements in the reproducibility of signal intensity and MALDI average molecular mass measurements to the ES sample deposition technique. 相似文献
143.
Scott?D.?HantonEmail author Kevin?G.?Owens 《Journal of the American Society for Mass Spectrometry》2005,16(7):1172-1180
The development of reliable sample preparation methods has been critical to the success of matrix-assisted laser desorption/ionization
(MALDI) mass spectrometry experiments. Good MALDI sample preparation for polymers involves choosing the solvent system, the
matrix, and the ionization agent correctly, and combining them in a manner that will lead to a sample that will produce the
desired ions. The vast diversity of chemistry available in industrial polymers has challenged our ability to design reliable
sample preparation methods. In the experiments reported here, we show that matrix-enhanced secondary ion mass spectrometry
(MESIMS) is an effective analytical technique to explore sample segregation in solid phase MALDI samples. Qualitative comparison
of MESIMS and MALDI results for polymer samples prepared with multiple matrices aids our investigation of the solid-phase
solubility of a variety of low molecular weight polymer materials. Including the solid-phase solubility with the liquid-phase
solubility of the polymer samples and the matrices enables the construction of a relative solubility chart, which shows the
best solubility matches between the polymer and matrix materials for MALDI experiments. 相似文献
144.
Simmons K Kinney J Owens A Kleier DA Bloch K Argentar D Walsh A Vaidyanathan G 《Journal of chemical information and modeling》2008,48(11):2196-2206
Over the years numerous papers have presented the effectiveness of various machine learning methods in analyzing drug discovery biological screening data. The predictive performance of models developed using these methods has traditionally been evaluated by assessing performance of the developed models against a portion of the data randomly selected for holdout. It has been our experience that such assessments, while widely practiced, result in an optimistic assessment. This paper describes the development of a series of ensemble-based decision tree models, shares our experience at various stages in the model development process, and presents the impact of such models when they are applied to vendor offerings and the forecasted compounds are acquired and screened in the relevant assays. We have seen that well developed models can significantly increase the hit-rates observed in HTS campaigns. 相似文献
145.
P. J. Owens 《Journal of Graph Theory》1982,6(4):473-479
It is shown that some classes of cyclically 5-edge-connected cubic planar graphs with only one type of face besides pentagons contain non-Hamiltonian members and have shortness coefficients less than unity. 相似文献
146.
X-ray photoelectron studies of solid triamino-trinitrobenzene subjected to shock pulses and UV light indicate that the NO2 group is severed from the molecule. The implications of this result with respect to the mechanism of shock induced detonation of this material is discussed. 相似文献
147.
F.J. Owens 《Solid State Communications》1979,29(11):789-791
A marked divergence of the line width of the Raman spectra of the librational modes of the NCS- ion is observed in KNCS as the temperature is raised through the transition temperature. The effect is attributed to the onset of fluctuations of the orientation of the NCS- ion between two energetically equivalent positions. 相似文献
148.
149.
We calculate cross-sections for two- and three-jet events ine ? p collisions at \(\sqrt s \) =314 GeV. We include contributions from point-like photon interactions, as well as contributions from when the photon is resolved into constituent quarks and gluons. It is shown that measurements of the angular distribution of the dijet system in two-jet events as a function of the dijet mass will assist in the separation of these two components. Aside from being a direct test of QCD photoproduction subprocesses, measurement of these events will yield information on the hadronic structure of the photon. 相似文献
150.
针对现有Web使用记录挖掘方法发现的知识和规则存在不精确或不完全的问题,提出了一种改进的基于粗糙近似的Web事务聚类算法.该算法首先对原有算法得到的每个类,用关系矩阵找出在这个类中不满足传递性的对象,然后在该对象的集合(类)上用关系矩阵找出在这个类中不满足传递性的对象,再对每个类进行分割,使其满足关系R的传递性,克服了现有算法不满足关系的传递性和在某些情况下得到的结果不准确的缺点. 相似文献