A molecular fluorophore in citric acid/ethylenediamine carbon dots identified and quantified by multinuclear solid-state nuclear magnetic resonance

The composition of fluorescent polymer nanoparticles, commonly referred to as carbon dots, synthesized by microwave-assisted reaction of citric acid and ethylenediamine was investigated by ¹³C, ¹³C{¹H}, ¹H─¹³C, ¹³C{¹⁴N}, and ¹⁵N solid-state nuclear magnetic resonance (NMR) experiments. ¹³C NMR with spectral editing provided no evidence for significant condensed aromatic or diamondoid carbon phases. ¹⁵N NMR showed that the nanoparticle matrix has been polymerized by amide and some imide formation. Five small, resolved ¹³C NMR peaks, including an unusual ═CH signal at 84 ppm (¹H chemical shift of 5.8 ppm) and ═CN₂ at 155 ppm, and two distinctive ¹⁵N NMR resonances near 80 and 160 ppm proved the presence of 5-oxo-1,2,3,5-tetrahydroimidazo[1,2-a]pyridine-7-carboxylic acid (IPCA) or its derivatives. This molecular fluorophore with conjugated double bonds, formed by a double cyclization reaction of citric acid and ethylenediamine as first shown by Y. Song, B. Yang, and coworkers in 2015, accounts for the fluorescence of the carbon dots. Cross-peaks in a ¹H─¹³C HETCOR spectrum with brief ¹H spin diffusion proved that IPCA is finely dispersed in the polyamide matrix. From quantitative ¹³C and ¹⁵N NMR spectra, a high concentration (18 ± 2 wt%) of IPCA in the carbon dots was determined. A pronounced gradient in ¹³C chemical-shift perturbations and peak widths, with the broadest lines near the COO group of IPCA, indicated at least partial transformation of the carboxylic acid of IPCA by amide or ester formation.     

Magnetic deflection of neutral metal clusters in a beam

A new apparatus for measuring the magnetic properties of metal clusters has been constructed. The technique involves the conventional Stern-Gerlach deflection scheme together with modern pulsed laser vaporization source technology and time of flight mass spectrometry. High field seeking monodirectional deflections have been measured for cobalt clusters containing between 40 and 400 atoms. The measured magnetic moments per atom are found to be lower than the known values for the bulk. Special attention has been given to velocity measurements of the metal clusters and the carrier gas atoms in the beam. The residence time of the particles in the source cavity has been measured.     

广义风险过程中渐近方差的非参数估计

本文对广义风险过程中的渐近方差作了非参数估计,得出并证明了两个定理,为广义风险过程中破产概率的区间估计作了理论准备．     

3,3,6,6-四甲基-9-邻氯苯基-1,8-二氧代-3,4,5,6,7,9-六氧化氧杂蒽的合成和晶体结构

标题化合物C23H25对O3Cl是由邻氯苯甲醛与5，5-二甲基1，3-环己二酮在N，N-二甲基甲酸腹中反应而得。结构通过单晶X-射线衍射法确定，其晶体属于单科晶系，空间群=1632。晶体结构用直接法解出，使用全矩阵最小二乘法对原子参数进行修正，最后的偏离因子为R=0．054，Rw一0．063。在晶体结构中，吡喃环与苯环之间的两面角为92．43°。     

Total Synthesis of Several 8, 8",-Biflavones

8,8"-Biflavonoidsareantw0rtantclass0fbiflavonoids.Asasystematicresearchofthe8,8"-biflav0noids,wehavepreviouslyreportedthestudyonthereactionof2'-hydroxychaloneswithl2-H2SO4-DMSOsystem.'InthispaPer,thesynthesisof5,5",7,7',-tetTameth0xy-8,8"-biflavonela2,4,4",7,7"-tetramethoxy-8,8"-biflavone1b',4',4",,5,5,',7,7"-hexamethoxy-8,8"-biflav0ne1c4and4,4"-dibenZyl0xy-5,5",7,7"-tetramothoxy-8,8"-biflavoneldisreported.ThesyntheticmethodisshownintheSchemebelow.2-Hydroxyacet0phenonescondensedwithsubsti…     

The determination of uranium in biological materials by neutron activation analysis using the fission product134I

A method for the determination of uranium based on²³⁵U thermal neutron fission, has been developed and employed on samples of ashed fish tissue and seaweed. The method involves a post-irradiation ion exchange separation of iodine isotopes. The 884 keV photopeak of¹³⁴I is used for measurement. Uranium detection limits in the samples concerned have been estimated to be 1·10⁻⁸g in terms of natural uranium. The precision achieved in analysing several series of 3–5 samples was 4–10 per cent. The accuracy of the method was tested by employing an independent neutron activation procedure based on²³⁹U measurement. The accuracy of both methods was checked by analysing NBS SRM 1571 ‘Orchard Leaves’.     

高效液相色谱氮杂冠醚键合固定相的合成及性能研究

我们曾用γ－氯丙基键合硅胶（ＣＰＳ），在氢化钠（ＮａＨ）作用下合成了３－（氮杂－１８－冠－６）丙基键合固定相（ＢＣＰ）［１］．该固定相对碱基、核苷酸、硝基苯酚等有较好的分离选择性，但由于ＮａＨ对硅胶基质腐蚀作用较大，导致ＢＣＰ柱效及渗透性较低．本文采...     

2,4,6-三硝基苯酚改性锆铝复合氧化物固定相分离富勒烯的色谱性能研究

制备了用于分离C60和C70的2，4，6－三硝基苯酚改性锆铝复合氧化物高效液相色谱固定相，考察了流动相中甲苯的含量、柱温及流速对C60和C70分离的影响，同时比较了酸腐蚀前后锆铝复合氧化物基质对分离的影响，结果表明，2，4，6－三硝基苯酚改性酸腐蚀后锆铝复合氧化物填料对富勒烯表现出较强的分离能力，具有作为富勒烯制备分离的潜力。     

Investigative proteomics: identification of an unknown plant virus from infected plants using mass spectrometry

We describe the identification of a previously uncharacterized plant virus that is capable of infecting Nicotiana spp. and Arabidopsis thaliana. Protein extracts were first prepared from leaf tissue of uninfected tobacco plants, and the proteins were visualized with two-dimensional electrophoresis (2-DE). Matching gels were then run using protein extracts of a tobacco plant infected with tobacco mosaic virus (TMV). After visual comparison, the proteins spots that were differentially expressed in infected plant tissues were cut from the gels and analyzed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Tandem mass spectrometry data of individual peptides was searched with SEQUEST. Using this approach we demonstrated a successful proof-of-concept experiment by identifying TMV proteins present in the total protein extract. The same procedure was then applied to tobacco plants infected with a laboratory viral isolate of unknown identity. Several of the differentially expressed protein spots were identified as proteins of potato virus X (PVX), thus successfully identifying the causative agent of the uncharacterized viral infection. We believe this demonstrates that HPLC-MS/MS can be used to successfully characterize unknown viruses in infected plants.     

酸性化合物在十二胺-N,N-二亚甲基膦酸改性氧化锆固定相上的分离

酸性化合物在十二胺-N; N-二亚甲基膦酸改性氧化锆固定相上的分离;氧化锆;色谱固定相;十二胺-N; N-二亚甲基膦酸