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1.
Two new compounds have been isolated from the whole plant of Monochoria vaginalis and characterized as: (10Z)‐1‐(2,6‐dihydroxyphenyl)octadec‐10‐en‐1‐one ( 1 ) (20R, 24R)‐campest‐5‐ene‐3β, 4β‐diol ( 2 ) together with nine known ones. The structures of these compounds were elucidated on the basis of spectral data and chemical evidence. 相似文献
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To isolate epigallocatechin gallate (EGCG) of catechin compounds from Korean green tea (Bosung, Chonnam), a C18 reversed-phase preparative column (250x22 mm) packed with packings of three different sizes (15, 40-63, and 150 microm) was used. The sample extracted with water was partitioned with chloroform and ethyl acetate to remove the impurities including caffeine. The mobile phases in this experiment were composed of 0.1% acetic acid in water, acetonitrile, methanol and ethyl acetate. The injection volume was fixed at 400 microl and the flow rate was increased as the particle size becomes larger. The isolation of EGCG with particle size was compared at a preparative scale and the feasibility of separation of EGCG at larger particle sizes was confirmed. The optimum mobile phase composition for separating EGCG was experimentally obtained at the particle sizes of 15 and 40-63 microm in the isocratic mode, but EGCG was not purely separated at the particle size of 150 microm. 相似文献
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A. S. R. Anjaneyulu A. Madhusudhana Rao V. Kameswara Rao L. Ramachandra Row 《Tetrahedron letters》1975,16(52):4697-4700
A new lignan from is shown to be 1, 2a-dihydroxy-2e-piperonyl-6e-(6″-bromopiperonyl)-3, 7-dioxabicyclo-[3,3,0]-octane, the first example of a bromine containing lignan. 相似文献
7.
A series of A2Bi24Mo8X2O68 compounds, Ca2Bi24Mo8Cr2O68 (CBMC), Sr2Bi24Mo8Cr2O68 (SBMC), Pb2Bi24Mo8Cr2O68 (PBMC) and Ba2Bi24Mo8W2O68 (BBMW) have been synthesized by the solid-state method and characterized by single crystal X-ray diffraction. The compounds
index into the monoclinic P2/c system with a=11.687(4) ?, 5.784(2) ?, 24.728(9) ?, 101.911(6)°, Z=1; 11.673(6) ?, 5.775(3) ?, 24.670(2) ?, 101.757(8)°, Z=1; 11.638(3) ?, 5.790(1) ?, 24.655(6) ?, 101.716(4)°, Z=1 and 11.718(6) ?, 5.818(3) ?, 24.716(12) ?, 101.835(9)°, Z=1 for CBMC, SBMC, PBMC and BBMW, respectively. The structures were solved by direct methods and refined to R indices of 0.081,
0.065, 0.080 and 0.079 respectively. These compounds are isostructural with Bi26Mo10O69 and the structure consists of columns of [Bi12O14] along the b-axis, surrounded by Mo/Cr/WO4 tetrahedra. a.c. impedance studies indicate higher values of ionic conductivity for the tungsten-substituted compounds.
Supplementary material
The crystal data of CBMC, SBMC, PBMC and BBMW have been deposited at the Fachinformationszentrum Karlsruhe (FIZ) with the
numbers CSD 415143, CSD 415145, CSD 415144 and CSD 415142, respectively. 相似文献
8.
A simple and accurate method for the separation and determination of ofloxacin enantiomers was developed by ionic liquid-assisted ligand-exchange high performance liquid chromatography. Both achiral and chiral ionic liquids were tested for their efficiency of ofloxacin enantiomeric separation. The effects of ligands, concentration of metal ion, organic modifier, pH of the mobile phase, and temperature were also investigated and evaluated. Optimal conditions were obtained on a conventional C(18) column, where the mobile phase consisted of methanol/water (20 : 80, v/v) (containing 4.0 mmol L(-1) amino acid ionic liquid and 3.0 mmol L(-1) copper sulfate) at a flow rate of 0.5 mL min(-1). Under this condition, the ofloxacin enantiomers could be baseline separated within 14 minutes; the proposed method was used to analyze different commercial ofloxacin medicines. 相似文献
9.
Ionic liquid-modified silica, with functional groups based on imidazole as the cation, was obtained. A molecular imprinting technique was introduced to form the order of functional groups. The selectivity of the obtained ionic liquid-modified silica was successfully used as a special imprinted sorbent in the solid-phase extraction to isolate cryptotanshinone, tanshinone I and tanshinone IIA from Salvia miltiorrhiza Bunge. Several washing and elution solvents with different polarities were evaluated. The ionic liquid-modified silica as the sorbent exhibited a higher selectivity than blank ionic liquid-modified silica, traditional silica and C18 cartridges. A quantitative analysis was conducted by liquid chromatography with a C18 column and methanol/water (75:25, v/v, containing 0.5% acetic acid) as the mobile phase. A good linearity was obtained from 0.5 × 10?4 to 0.1 mg mL?1 (r 2 > 0.99) with relative standard deviations that were less than 4.6%. 相似文献
10.
A new stationary phase based on silica modified with 1-methyl-3-propylimidazolium chloride was synthesized and characterized
in this paper. A derivative of 1-methyl-3-propylimidazolium chloride was used to chemically modify the surface of silica particles
to act as the stationary phase for HPLC. The modified particles were characterized by Fourier Transform Infrared (FT-IR), 13C NMR spectroscopy and thermogravimetric analysis (TGA). The surface modification procedure rendered particles with a surface
coverage of 0.89 μmol/m2 of alkylimidazolium chloride. Columns packed with the modified silica and blank silica particles were tested under HPLC conditions.
Preliminary evaluation of the stationary phase for HPLC was performed using aromatic compounds as model compounds. The separation
mechanism appears to involve multiple interactions including ion exchange, hydrophobic and electrostatic interactions. 相似文献