Four Triterpene Oligoglycosides from the seeds of Aesculus Chinensis

TheseedsofAesculuschinensisBge.(Hippocastanaceae)havebeenusedasfolkmedicineforthetreatmentofdistensionandpaininchestandabdomenl.Untilnow,thereisnoreportonitschemicalconstituents.Thispaperdescribesstructureelucidationoftwonewcompounds,escinsIVa3andIVb4onthebasisofspectroscopicmethodsandcomparisonwithescinsla1andfo22.Amongthem,EscinlaIwasstudiedbyX-raydistractionanalysis.Compound3,whitepowder,showediRbandsduetocarboxylanda,p-unsaturatedesterat1740,1713and1640cm-'andstrongabsorptionbandsat34…     

MALDI-TOF-MS analysis of small molecules using modified mesoporous material SBA-15 as assisted matrix

Mesoporous silica, SBA-15 was successfully functionalized with quinoline moiety, and was applied as a matrix in the MALDI-TOF-MS analysis of small molecules. The modified SBA-15 material [SBA-15-8-(3-(triethoxysilyl)propoxy) quinoline, SBA-15-8QSi] was obtained by using calcined SBA-15 and 8-hydroxy quinoline. The structure of the functionalized mesoporous material was systemically characterized by TEM, the N₂ adsorption-desorption isotherm technique and FT-IR spectra. Compared with DHB and SBA-15, SBA-15-8QSi demonstrated several advantages in the analysis of small molecules with MALDI-TOF-MS, such as less background interference ions, high homogeneity, and better reproducibility. Based on these results, the various analytical parameters were optimized. The ideal operating conditions were (1) methanol used as the dissolving solvent; (2) sample first dropping method; (3) a ratio between the analyte and the matrix of 3.5:10. Under these optimization conditions, a low detection limit (8 pmol for L-Arginine-HCl) and high reproducibility (≤29%) were obtained. This technique was successfully applied to the analysis of various types of small molecules, such as saccharides, amino acids, metabolites, and natural honey.     

Characterization of coal oil using three-dimensional excitation and emission matrix fluorescence spectroscopy

Three-dimensional （3D） excitation-emission matrix （EEM） fluorescence spectroscopy is applied to characterize the coal oil. The results show that the 3D fluorescence spectra of coal oil in aqueous solution mainly have one broad peak. This peak is identified at the excitation/emission wavelengths of 270/290 nm. The relation between the fluorescence intensity and the concentration of coal oil is also studied. When the concentration lies between 2 - 2000 ppm, the relation between the fluorescence intensity and the concentration of coal oil is well linear. The nature of solvents significantly affects the EEM fluorescence of coal oil.     

Na3AlF6-Al2O3熔盐体系中ZnFe2O4基阳极的电化学行为

研究了ＺｎＦｅ２Ｏ４基阳极在Ｎａ３ＡｌＦ６－Ａｌ２Ｏ３熔盐体系中的电化学稳定性，讨论了电极的析氧历程并得到了析氧过电位与阳极表观电流密度之间的Ｔａｆｅｌ关系式，η＝０．１２＋０．０５２ｌｏｇｉ（ｉ＝０．０１５－０．４４Ａ／ｃｍ＾２）用三角波电位扫描法测定了电极析氧过程的伏安曲线。     

石墨炉原子吸收法测定芦笋罐头中砷

采用石墨炉原于吸收法测定芦笋罐头中砷，加入硝酸铵消除氯化钠的干扰，并以镍作为基体改进剂，方法检出限为0，10μkg-1，特征量为0．80pg，回收申为94％一1。5％。     

Asymmetric synthesis of pedamide using I_2-induced heterocyclization to construct the skeleton

An alternative approach to synthesize pedamide,a key building block of pederin was described.Iodine-induced asymmetric heterocyclization was used as the key step to construct the skeleton,a tetrahydropyran ring with three chiral centers.Brown's asymmetric allylation and Lewis acid-mediated allylation were investigated to introduce chains and chiral alcohols.Sharpless dihydroxylation decorated the side chain.And high optically pure target was obtained by removing the epimers formed in these reactions on c...     

Applying Unconventional Spectroscopies to the Single-Molecule Magnets,Co(PPh3)2X2 (X=Cl,Br, I): Unveiling Magnetic Transitions and Spin-Phonon Coupling

Large separation of magnetic levels and slow relaxation in metal complexes are desirable properties of single-molecule magnets (SMMs). Spin-phonon coupling (interactions of magnetic levels with phonons) is ubiquitous, leading to magnetic relaxation and loss of memory in SMMs and quantum coherence in qubits. Direct observation of magnetic transitions and spin-phonon coupling in molecules is challenging. We have found that far-IR magnetic spectra (FIRMS) of Co(PPh₃)₂X₂ ( Co-X ; X=Cl, Br, I) reveal rarely observed spin-phonon coupling as avoided crossings between magnetic and u-symmetry phonon transitions. Inelastic neutron scattering (INS) gives phonon spectra. Calculations using VASP and phonopy programs gave phonon symmetries and movies. Magnetic transitions among zero-field split (ZFS) levels of the S=3/2 electronic ground state were probed by INS, high-frequency and -field EPR (HFEPR), FIRMS, and frequency-domain FT terahertz EPR (FD-FT THz-EPR), giving magnetic excitation spectra and determining ZFS parameters (D, E) and g values. Ligand-field theory (LFT) was used to analyze earlier electronic absorption spectra and give calculated ZFS parameters matching those from the experiments. DFT calculations also gave spin densities in Co-X , showing that the larger Co(II) spin density in a molecule, the larger its ZFS magnitude. The current work reveals dynamics of magnetic and phonon excitations in SMMs. Studies of such couplings in the future would help to understand how spin-phonon coupling may lead to magnetic relaxation and develop guidance to control such coupling.     

Synthesis of Mg–Al–carbonate layered double hydroxide by an atom-economic reaction

A clean method for preparing layered double hydroxides (LDHs) has been developed, featured by using the hydroxides of two different metals as starting materials by atom-economic reaction. The reactions were carried out under hydrothermal conditions in either a high pressure autoclave or a microwave digester. The compositions, structural parameters and thermal behavior of the resulting LDHs are very similar to those of materials produced by using the separate nucleation and aging steps (SNAS) method. The major advantage of the new method is that no by-product is produced, so that filtration and washing processes are unnecessary. The consequent reduction in water consumption is beneficial to the environment.     

Fluorescence detection in capillary arrays based on galvanometer step scanning.

A computer-controlled galvanometer scanner is adapted for scanning a focused laser beam across a 96-capillary array for laser-induced fluorescence detection. The signal at a single photomultiplier tube is temporally sorted to distinguish among the capillaries. The limit of detection for fluoresceins is 3 x 10(-11) M (S/N = 3) for 5 mW of total laser power scanned at 4 Hz. The observed cross-talk among capillaries is 0.2%. Advantages include the efficient utilization of light due to the high duty-cycle of step scan, good detection performance due to the reduction of stray light, ruggedness due to the small mass of the galvanometer mirror, low cost due to the simplicity of components, and flexibility due to the independent paths for excitation and emission.