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111.
Simultaneous determination of triterpene saponins in ginseng drugs by high-performance liquid chromatography 总被引:3,自引:0,他引:3
A HPLC method for the simultaneous determination of 11 triterpene saponins with four-type aglycones (protopanaxadiol, protopanaxatriol, ocotillol and oleanolic acid types) in Ginseng drugs was developed and validated. Using a gradient of acetonitrile and 10 mM K-phosphate buffer (pH 5.80) as the mobile phase and UV detection at 196 nm, more than 18 ginsenosides with different aglycones were separated satisfactorily within 60 min. The detection limits (signal/noise> or =3) were 0.1 microg for ginsenosides Rb1, Rc, Rd, Re and Rg1, chikusetsusaponin III, and notoginsenoside R2, 0.2 microg for gisenoside Ro and chikusetsusaponin IVa, 0.3 microg for chikusetsusaponin IV, and 3 microg for majonoside R2. The calibration curve of each saponin had a correlation coefficient close to 1. Intra- and interday precisions were less than 2.1% (n=5) and 3.3% (n=15), respectively. The recovery rates of extraction were in the range of 96.4-102.7% for all ginsenosides. By adopting this method, the determinations of 11 ginsenosides in three Ginseng drugs derived from Panax ginseng, Panax vietnamensis var. fuscidiscus and Panax japonicus (Japan) were achieved. 相似文献
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113.
光学活性甲苄菊酯的合成及其结构与活性关系的研究 总被引:4,自引:0,他引:4
本文改进了Goffinet方法,完成了(±)-trans菊酸的拆分;改进了Campbel?方法,只用一种拆分剂(奎宁)完成了对(±)-cis菊酸的拆分。用IR、~1HNMR、旋光度测定等方法确定了各甲苄菊酯光学异构体的结构。生物试验表明结构与活性有如下关系:1,各异构体中以1R-酯的杀虫活性为高,尤其(-)-(1R,3R)-trans甲苄菊酯对全部测试昆虫均显示较高的杀虫活性;2,昆虫不同,各异构体的活性次序也略有差异。 相似文献
114.
CHENG Mingming SUN Zhenying MA Wanhong CHEN Chuncheng ZHAO Jincai WANG Zhengping 《中国科学B辑(英文版)》2006,49(5)
The organic-inorganic layered solid catalyst Fe(bpy)32+-laponite was able to photodegrade Rhodamine B (RhB) by activation of dioxygen under visible irradiation (λ>420 nm), while the homogeneous aqueous solution Fe(bpy)32+ showed no photoactivity. The catalyst could be repeatedly used and retained its reactivity. The hybrid catalyst could be separated from the suspension by centrifugation or sedimentation. The TOC removal yield of RhB was measured. Reactive oxygen species (ROS) formed during degradation was detected by EPR. A possible mechanism was proposed on the basis of the experimental results. 相似文献
115.
合成和表征了4种以四溴代邻苯二甲酸根阴离子(4Br-PHTH)桥联、以1,10-菲咯啉(phen),5-硝基-1,10-菲咯啉(NO_2-phen),2,2′-联吡啶(bpy)和4,4′-二甲基-2,2′-联吡啶(Me_2bpy)端接的双核钴(Ⅱ)配合物[Co_2(4Br-PHTH)(L)_4](ClO_4)(L=phen(l),NO_2-phen(2),bpy(3),Me_2bpy(4))。基于IR光谱、元素分析、电导测量等方法推定配合物具有四溴代邻苯二甲酸根桥联结构和Co(Ⅱ)离子具有畸变的八面体配位环境。进行了配合物变温磁化率(75~300K)的测定,其数据已用从自旋哈密顿符导出的磁方程拟合,求得交换参数J=-0.87cm~(-1)(1),-0.84cm~(-1)(2),-0.82cm~(-1)(3),-0.85cm~(-1)(4),表明金属离子间有弱的反铁磁性自旋交换相互作用。 相似文献
116.
Hamza MS Zou X Banka R Brown KL van Eldik R 《Dalton transactions (Cambridge, England : 2003)》2005,(4):782-787
Ligand substitution reactions of the vitamin B12 analog cyanoimidazolylcobamide, CN(Im)Cbl, with cyanide were studied. Cyanide substitutes imidazole (Im) in the alpha-position more slowly than it substitutes dimethylbenzimidazole in cyanocobalamin (vitamin B12). The kinetics of the displacement of Im by CN- showed saturation behaviour at high cyanide concentration; the limiting rate constant was found to be 0.0264 s(-1) at 25 degrees C and is characterized by the activation parameters: DeltaH(not =) = 111 +/- 2 kJ mol(-1), DeltaS(not =) = +97 +/- 6 J K(-1) mol(-1), and DeltaV(not =) = +9.3 +/- 0.3 cm3 mol(-1). These parameters are interpreted in terms of an I(d) mechanism. The equilibrium constant for the reaction of CN(Im)Cbl with CN- was found to be 861 +/- 75 M(-1), which is significantly less than that obtained for the reaction of cyanocobalamin with CN- (viz. 10(4) M(-1)). pKbase-off for the base-on/base-off equilibrium was determined spectrophotometrically and found to be 0.99 +/- 0.05, which is about 0.9 pH units higher than that obtained previously in the case of cyanocobalamin. In addition, the kinetics of the base-on/base-off reaction was studied using a pH-jump technique and the data obtained revealed evidence for an acid catalyzed reaction path. The results obtained in this study are discussed in reference to those reported previously for cyanocobalamin. 相似文献
117.
118.
Desorption/ionization on silicon mass spectrometry (DIOS-MS) is a matrix-free technique that allows for the direct desorption/ionization of low-molecular-weight compounds with little or no fragmentation of analytes. This technique has a relatively high tolerance for contaminants commonly found in biological samples. DIOS-MS has been applied to determine the activity of immobilized enzymes on the porous silicon surface. Enzyme activities were also monitored with the addition of a competitive inhibitor in the substrate solution. It is demonstrated that this method can be applied to the screening of enzyme inhibitors. Furthermore, a method for peptide mapping analysis by in situ digestion of proteins on the porous silicon surface modified by trypsin, combined with matrix-assisted laser desorption/ionization-time of flight-MS has been developed. 相似文献
119.
Pan A Liu R Yang Q Zhu Y Yang G Zou B Chen K 《The journal of physical chemistry. B》2005,109(51):24268-24272
Aligned CdS nanowires (NWs) were obtained through a simple thermal evaporation process with highly active CdS nanoparticles as the evaporation source. These NWs show prominent optical waveguides behavior under a continuous-wave (CW) laser excitation. Excitation intensity-dependent photoluminescence (PL) measurements show that these NWs exhibited both broad and supernarrow stimulated emission (lasing) under intense pulse optical excitation at room temperature. Raman scattering and time-resolved PL measurements were used to investigate the optical properties. The results indicated that the stimulated emission in these NWs involves the electron-hole plasma (EHP) and Farby-Perot (F-P) optical resonant processes at room temperature. 相似文献
120.
A novel method of synthesizing protein chiral stationary phase (protein-CSP) is proposed with 2,4,6-trichloro-1,3,5-triazine as the activator. The bovine serum albumin (BSA) based chiral columns (150 x 4.6 mm I.D.) were prepared successfully within 8 h. With tryptophan as the probe solute, it was observed that the BSA immobilized by this method had a better ability to distinguish enantiomers than that activated by glutaric dialdehyde. This may be due to the well-maintained BSA conformation and the larger amount of BSA immobilized on the silica gel. The BSA-CSP prepared by this method was relatively stable under experimental conditions, and the resolution of 13 chiral compounds was achieved. The coupling reaction in this method is mild, reliable and reproducible; it is also suitable for the immobilization of various biopolymers in the preparation of bioreactor, biosensor and affinity chromatography columns. 相似文献