高速逆流色谱法分离制备中药诃子中的没食子酸

利用高速逆流色谱法从100 mg诃子醇提物中一次性分离制备得到8.6 mg没食子酸。通过分析型高速逆流色谱对5种溶剂系统进行筛选,确定以正己烷-乙酸乙酯-甲醇-水(体积比为1:5:1:5)为两相溶剂体系并放大到制备型上,以上相为固定相,下相为流动相,在主机转速850 r/min、流动相流速2 mL/min、检测波长254 nm的条件下进行分离制备,获得4个分离峰(组分Ⅰ、Ⅱ、Ⅲ、Ⅳ)。经高效液相色谱检测,按照面积归一法计算,其中组分Ⅲ的纯度达96.40%。经电喷雾电离质谱分析,并结合与没食子酸标准品的高效液相色谱测定结果的对比,确定组分Ⅲ为没食子酸。该方法简便、快速、重复性好,适合于诃子中没食子酸的分离制备。     

HPLC法测定怀菊花中没食子酸的含量

为建立HPLC法测定怀菊花中没食子酸含量测定方法,采用Agilent C18柱(150 mm×4.6mm,5μm),以V(甲醇)+V(超纯水+0.1%磷酸)=25+75为流动相,流量:0.5 mL·min1;柱温为25℃,检测波长:258 nm;进样量:10μL,进行测定。结果表明,回归方程为y=3.054 2 x-2.207 1,r2=0.999 1(n=6),线性范围0～20μg,平均回收率97.28%,RSD为3.39%。样品中没食子酸质量分数为3.17 mg/g。方法快速、简便、准确、重现性较好,结果可靠,可为怀菊花中没食子酸的质量评价提供依据。     

Biotransformation of Aspen Lignin by the Fungus Trametes villosus

Quantitative ¹ H and ¹³ C NMR spectroscopies demonstrate that biotransformation of aspen wood by the fungusTrametes villosusresults in oxidation and destruction of lignin with cleavage of C-C alkyl-alkyl bonds in side chains and partial demethoxylation in addition to cleavage of lignocarbohydrate bonds. New C _ar -O-C bonds form while lignin is being destroyed at alkyl-alkyl bonds. Cleavage of rings and destruction of C _ar -C bonds was not observed.     

乙二胺四乙酸对锗（Ⅳ）—没食子酸体系及钒（Ⅳ）的示波极谱电流的影响

用分光光度法及电化学法详细研究了在稀硫酸介质，分别加ＥＤＴＡ到锗－没食子酸，Ｇｅ－ＧＡ－Ｖ体系以及Ｖ溶液中，所产生的影响。结果表明，ＥＤＴＡ使Ｇｅ－ＧＡ体系的两步２电子反应过程变得清Ｇｅ－ＧＡ－Ｖ体系因Ｖ２Ｈ３Ｙ＾－Ｇ形成，增强了Ｖ的化学氧化力。     

Random bond Potts model: The test of the replica symmetry breaking

The averaged spin-spin correlation function squared is calculated for the ferro-magnetic random bond Potts model in two dimensions. The technique being used is the renormalization group plus conformal field theory. The results are of the E-expansion type fixed point calculation, E being the deviation of the central charge (or the number of components) of the Potts model from the Ising model value. Calculations are done both for the replica symmetric and the replica symmetry broken fixed points. The results obtained allow for numerical simulation tests to decide between the two different criticalities of the random bond Potts model.     

Influence of the thermal modification of controlled porosity glass on the affinity chromatography of fungal proteins

Summary The properties and the coverage density of chemically bonded phases depend among others on the properties of their supports. Controlled-porosity glasses (CPG) are materials used as a support of bio-active ligands. Their network mainly consist of SiO₂ as well as of a small amount of B₂O₃ and Na₂O. The characteristic feature of porous glasses is the possibility of a change in the surface boron concentration leading to the change of the properties of their surface.This paper deals with the results of the separation of fungal proteins on packings consisting of vanillin bonded to CPG with different boron concentration on its surface. It appears from the data obtained that the changes in the affinity of the fungal proteins to the packing are related to the extend of the thermal treatment of the CPG. The protein fractions separated by chromatography were confirmed to be homogeneous by poly-acryloamide gel disc electrophoresis.     

Phase transitions in Sr 0.61 Ba 0.39 Nb 2 O 6 :Ce 3+ : II. Linear birefringence studies of spontaneous and precursor polarization

The linear birefringence (LB) of Sr _0.61-x Ba _0.39 Nb ₂ O ₆ :Ce ³⁺ x (SBN61:Ce) has been measured as a function of temperature within the range of . Large tails have been observed above the ferroelectric phase transition temperatures T _c = 350, 328, 320 and 291 K for the concentrations x = 0, 0.0066, 0.0113 and 0.0207, respectively. Within an Ornstein-Zernike analysis the critical exponents , and are determined. It suggests that pure SBN61 belongs to the 3D Ising universality class. Doping with Ce ³⁺ ions, which seem to act as random fields, enhances the relaxor properties. The critical exponents and of SBN61:Ce shift against those of the three-dimensional random-field Ising model. Received 1 October 1999     

Second-order phase transition induced by deterministic fluctuations in aperiodic eight-state Potts models

We investigate the influence of aperiodic modulations of the exchange interactions between nearest-neighbour rows on the phase transition of the two-dimensional eight-state Potts model. The systems are studied numerically through intensive Monte-Carlo simulations using the Swendsen-Wang cluster algorithm for different aperiodic sequences. The transition point is located through duality relations, and the critical behaviour is investigated using FSS techniques at criticality. While the pure system exhibits a first-order transition, we show that the deterministic fluctuations resulting from the aperiodic coupling distribution are liable to modify drastically the physical properties in the neighbourhood of the transition point. For strong enough fluctuations of the sequence under consideration, a second-order phase transition is induced. The exponents , and are obtained at the new fixed point and crossover effects are discussed. Surface properties are also studied. Received: 18 March 1998 / Revised: 29 June 1998 / Accepted: 10 September 1998     

Disorder-induced quantum-Griffiths-like features from a non-conventional renormalization group analysis near four dimensions

We investigate the role played by symmetry conserving quenched disorder on quantum criticality of a variety of d-dimensional systems with a continuous symmetry order parameter. We employ a non-standard procedure which combines a preliminary reduction to an effective classical random problem and a successive conventional renormalization group treatment. Solving the effective flow equations to first order in ε=4−d and then restoring the original coupling parameters, for d<4 we find a quantum critical point scenario exhibiting unusual features, which remind us of some predictions of the quantum Griffiths phase model.     

Electronic structure of thin film iron-tetracyanoethylene: Fe(TCNE)<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>

Thin film iron-tetracyanoethylene Fe(TCNE) _x , x∼2, as determined by photoelectron spectroscopy, was grown in situ under ultra-high vacuum conditions using a recently developed physical vapor deposition-based technique for fabrication of oxygen- and precursor-free organic-based molecular magnets. Photoelectron spectroscopy results show no spurious trace elements in the films, and the iron is of Fe²⁺ valency. The highest occupied molecular orbital of Fe(TCNE) _x is located at ∼1.7 eV vs. Fermi level and is derived mainly from the TCNE⁻ singly occupied molecular orbital according to photoelectron spectroscopy and resonant photoelectron spectroscopy results. The Fe(3d)-derived states appear at higher binding energy, ∼4.5 eV, which is in contrast to V(TCNE)₂ where the highest occupied molecular orbital is mainly derived from V(3d) states. Fitting ligand field multiplet and charge transfer multiplet calculations to the Fe L-edge near edge X-ray absorption fine structure spectrum yields a high-spin Fe²⁺ (3d⁶) configuration with a crystal field parameter 10Dq∼0.6 eV for the Fe(TCNE) _x system. We propose that the significantly weaker Fe-TCNE ligand interaction as compared to the room temperature magnet V(TCNE)₂ (10Dq∼2.3 eV) is a strongly contributing factor to the substantially lower magnetic ordering temperature (T _C ) seen for Fe(TCNE) _x -type magnets.