Semi-industrial isolation of salicin and amygdalin from plant extracts using slow rotary counter-current chromatography

Salicin in the bark extract of Salix alba and amygdalin in the fruit extract of Semen armeniacae were each separated by slow rotary counter-current chromatography (SRCCC). The apparatus was equipped with a 40-L column made of 17 mm i.d. convoluted Teflon tubing. A 500g amount of crude extract containing salicin at 13.5% was separated yielding 63.5 g of salicin at 95.3% purity in 20h using methyl tert-butyl ether-l-butanol (1:3) saturated by methanol-water (1:5) as a stationary phase and methanol-water (1:5) saturated by methyl tert-butyl ether-1-butanol (1:3) as a mobile phase. A 400g amount of crude extract containing amygdalin at 55.3% was isolated to yield 221.2g of amygdalin at 94.1% purity in 19h using ethyl acetate-1-butanol (1:2) saturated by water as a stationary phase and water saturated by ethyl acetate-1-butanol (1:2) as a mobile phase. The flow rate of the mobile phase was 50 ml/min. The results show that industrial SRCCC separation of salicin and amygdalin is feasible using a larger column at a higher flow rate of the mobile phase.     

Capillary electrophoresis of cardiolipin with on-line dye interaction and spectrophotometric detection

Cardiolipin is an important phospholipid present in the mitochondrial inner membrane. It plays a key function in mitochondrial respiration by interacting with many enzymes or cofactors related to oxidative phosphorylation complexes. We have determined the concentration of cardiolipin using on-line 10-N-nonyl acridine orange (NAO) dye interaction capillary electrophoresis (CE) and spectrophotometric detection with a sample throughput of 3 min. In addition to the presence of 0.1 mM NAO, the background electrolyte (BGE) composition has been set at 80% methanol-10% acetonitrile-10% H(2)O (all v/v) to provide both good solubility and the maximum absorbance enhancement at 497 nm for the NAO-cardiolipin complex as compared to NAO alone. Sample consumption for each injection is about 57 nL. A calibration curve is established from 0.5 microM to 0.1 mM with R (2) = 0.9912 with a detection limit of 0.05 microM for cardiolipin. In a blind study, actual mitochondrial cell membrane samples in the microL range before or after UV light exposure were analyzed using the CE method. Cardiolipin concentration decreased in the different parts of the membrane sample upon UV photolysis of the cells. Support for the theory that UV light can induce cardiolipin translocation from the inner membrane (IM) to the outer membrane (OM) was indicated by a significant percentage increase of cardiolipin (as measured by the cardiolipin in the OM as compared to the sum total in the OM and IM) from 30.7 +/- 2.4% before UV light photolysis to 38.3 +/- 2.2% after UV irradiation.     

Synthesis and characterization of ionic organotin compounds [R2SnCl2(2-quin)](HNEt3) and crystal structures of [(2,4-Cl2-C6H3CH2)2SnCl2(2-quin)](HNEt3)

Eight ionic organotin compounds [R₂SnCl₂(2-quin)]⁻(HNEt₃)⁺ have been synthesized by reactions of 2-quinH with R₂SnCl₂ (R = PhCH₂1, 2-Cl-C₆H₄CH₂2, 4-Cl-C₆H₄CH₂3, 2-F-C₆H₄CH₂4, 4-F-C₆H₄CH₂5, 4-CN-C₆H₄CH₂6, Ph 7, 2,4-Cl₂-C₆H₃CH₂8) in the presence of organic base NEt₃, and their structures have been characterized by elemental analysis, IR and multinuclear NMR (¹H, ¹³C, ¹¹⁹Sn) spectroscopies. The structure of [(2,4-Cl₂-C₆H₃CH₂)₂SnCl₂(2-quin)]⁻(NEt₃)⁺ (8) has been determined by X-ray diffraction study. Studies show that compound 8 has a monomeric structure with the central tin atom six-coordinate in a distorted octahedral configuration and the nitrogen atoms of the 2-quin ligands are coordinating to the tin atom in all the eight compounds.     

Synthesis and crystal structure of inclusion compounds: Trans-9,10-dihydro-9,10-ethanoanthracene-11,12-dicarboxylic acid with boric acid and tetrabutylammonium salt

Two new inclusion compounds (n-C₄H₉)₄N⁺C₁₈-H₁₃O₄ ⁻·B(OH)₃ (1) and (n-C₄H₉)₄N⁺C₁₈H₁₃O₄ ⁻ (2) were prepared and characterized by X-ray crystallography. Crystal data: compound 1, monoclinic P2(1)/c, a = 1.569 9(1) nm, b = 0.995 5(6) nm, c = 2.293 3(1) nm, β = 109.962(3)°, Z = 4, and R ₁ = 0.0434, wR = 0.075 9; compound 2, monoclinic C2/c, a = 1.400 5(3) nm, b = 1,282 1(2) nm, c = 1.765 7(3) nm, β = 100.388(1)°, Z = 4, and R ₁ = 0.0584, wR = 0.096 6. In the crystal structure of 1, the tetramers formed by two trans-9,10-dihydro-9,10-ethanoanthracene-11,12-dicarboxylic acid (EADA) anions and two boric acid molecules were connected through O—H⋯O hydrogen bonds to generate a channel type host lattice. The tetra-n-butylammonium cations were stacked to give two columns within each channel with cross-sectional size of about 2.30 nm × 0.93 nm. In the crystal structure of 2, similar honeycomb host lattices with big size were also formed along the [101] direction by three-dimensional accumulation of EADA anions. The tetra-n-butylammonium cations were accommodated in a zigzag fashion within each channel. Translated from Acta Chimica Sinica, 2006, 64(18): 1904–1910 [译自: 化学学报]     

Determination of Procymidone, Pentachloroaniline and Methyl-pentachloro-phenylsulfide Residues in Wine by MSPD-GC-ECD

A rapid method based on matrix solid-phase dispersion (MSPD) was developed for the determination of procymidone, pentachloroaniline and methyl-pentachloro-phenylsulfide in wine. After the optimisation of different parameters such as the type of adsorbent, the extraction solvent, and the extraction assistance by sonication. The analysis of samples was accomplished using gas chromatography with electron-capture detector (GC-ECD). Spiked blank samples were used as standards to counteract the matrix effect observed in the chromatographic determination. The recovery of the method was in the range 82.4–93.7% and a good linear relationship (R ² ≥ 0.9992) with relative standard deviations lower than 8%. The limits of detection (LOD) ranged from 0.1 to 0.4 μg L^?1. The proposed method was applied to the analysis of these compounds in commercial wine samples.     

关于聚合物非晶态X衍射表征函数的探讨

<正> 目前许多学者已采用计算机X衍射分峰法对具有较复杂结构的结晶聚合物进行研究.这个方法的核心是数学模型,即反映晶态与非晶态的X衍射峰峰形规律的表征函数.它对研究结果的可靠性、精确度有直接的影响.Hindeleh与Johnson等人提出的三次多项式及其它形式,不能使样品的计算的衍射曲线与实验的衍射曲线相拟合,误差大.说明表征非晶态X衍射的数学模型还存在问题,分峰法还不完善.因此,我们认为有必要对非晶态表征函数进行探讨.本文提出了两个非晶态表征函数,并应用于聚丙烯结构分析,     

锂离子选择性微电极在生物体液中的响应

最近几年已报道了几种锂离子选择性电极.本文作者曾研制了以苯基膦酸二辛酯(DOPP)为溶剂,四苯硼酸盐为活性物质的PVC膜锂离子选择电极.本文在此基础上研制了锂离子选择性微电极,比较了以四苯硼酸钾(KTPB)及四苯硼酸钠(NaTPB)为活性物质的锂微电极的性能.同时考察了微电极在细胞内液、血清及生理盐液中对锂离子的响应特性.     

Pd-catalyzed synthesis of beta-biarylacryl ferrocenes via Suzuki cross-coupling

Some novel beta-biarylacryl ferrocene derivatives were synthesized via Pd-catalytic Suzuki cross-coupling reactions of beta-(2-bromophenyl)acrylferrocene and arylboronic acids. The structures were determined with elemental analyses, IR spectra, and (1)H-NMR spectra.     

Ln(η6-m-C6H4Me2)(AlCl4)3, (Ln=Pr,Er)的合成及Pr配合物的晶体结构

LnCl₃(Ln=Pr,Er)与AlCl₃在二甲苯中反应，合成了η⁶-(m-Me₂C₆H₄)Ln(AlCl₄)₃这两个新配合物并对其进行了元素分析、红外光谱和质谱的表征。测定了Pr配合物的晶体结构。该配合物具有扭曲的五角双锥几何构型。二甲苯和一个氯原子处于两个顶点，Pr配合物属单斜晶系，空间群P相似文献   

The chemical states of tellurium produced by spontaneous fission of252Cf

The distribution of the chemical states of tellurium isotopes produced by²⁵²Cf spontaneous fission, collected separately in the matrixes of NaCl, Kl, NaF, CH₃COONa·3H₂O, Na₂SO₄ and NaNO₃ crystals have been investigated. Two chemical states of tellurium isotopes maintained in these matrixes are Te(IV) and Te(VI). The relationships between the distribution of the chemical states of tellurium isotopes and the produced mode of tellurium, the chemical properties of collection matrixes, the time for collecting fission fragments are studied and the possible mechanism of the interactions of the fission products and the matrixes is discussed. The results show that the distribution of chemical states of tellurium isotopes depends on the chemical properties of the collection matrixes mainly.