人参与藜芦配伍化学成分变化的HPLC-ESI-MS与ESI-MS研究

采用电喷雾质谱(ESI-MS)和高效液相色谱与电喷雾质谱联用技术(HPLC-ESI-MS), 对人参与藜芦配伍过程中人参皂苷和藜芦生物碱的变化规律进行了系统研究. 在人参与藜芦配伍的共煎液中鉴定出八种人参皂苷, 其中有六种人参皂苷含量有所降低, Rf和Rb₂的含量基本不变; 此外还鉴定出八种藜芦生物碱, 其中有六种生物碱的含量随人参加入而明显增高. 人参与藜芦配伍, 煎煮液中人参皂苷的含量下降, 藜芦总碱的含量上升. 人参的加入有利于藜芦生物碱的溶出. 因藜芦总碱的毒性较强, 所以人参“反”藜芦具有一定道理.     

Optimum conditions for transformed Panax ginseng hairy roots in flask culture

Panax ginseng hairy roots were transformed by Agrobacterium rhizogenes KTCT 2744. They showed an active branching pattern and fast growth in hormone-free medium, and good growth at 23°C, pH 5.8, 1/2 MS medium, and 3% sucrose. Sucrose provided the highest growth among seven carbon sources tested. Six complex media were also tested. In the combined sugar study, hairy roots grew better on sucrose without glucose or fructose than with glucose or fructose. In the 1/2 MS basal medium, 30 mM in nitrogen and 0.62 mM phosphate salt concentration was the optimum. The growth ratio was maximal at an inoculum size of 0.4% (w/v). Crude saponin and polysaccharide levels were also measured.     

Development and Validation of Improved Reversed Phase-HPLC Method for Simultaneous Determination of Curcumin, Demethoxycurcumin and Bis-Demethoxycurcumin

Isocratic reversed phase high performance liquid chromatographic (HPLC) method using RP C18 column was developed for simultaneous determination of the curcuminoids. Mobile phase consisted of acetonitrile:0.1% trifluro-acetic acid (50:50) and flow rate was 1.5 mL min⁻¹ and elution was monitored at 420 nm. Validation in selected conditions showed that the chosen method is sensitive, selective, precise and reproducible with linear response of detector for the simultaneous determination of curcumin (C), demethoxycurcumin (DMC) and bis-demethoxycurcumin (BDMC). The limits of detection were 27.99, 31.91 and 21.81 ng mL⁻¹ for C, DMC and BDMC, respectively. Limits of quantitation for C, DMC and BDMC, were 84.84, 96.72 and 66.10 ng mL⁻¹, respectively. Linear range was form 100 to 600 ng mL⁻¹. The mean ± SD percent recoveries of curcuminoids were 99.87 ± 0.34, 100.09 ± 0.48 and 100.10 ± 0.60% of C, DMC and BDMC, respectively. Further, the method was used for quantitation of curcuminoids from turmeric rhizome.     

Determination of Phenolic Acids in Herba Epilobi by ITP–CE in the Column-Coupling Configuration

The combination of capillary isotachophoresis (ITP) and capillary zone electrophoresis (CZE) in the column-coupling configuration has been optimized in a mode in which the background electrolyte employed in the CZE step was different from the leading and terminating electrolytes of the ITP step. The optimum composition of the electrolyte system was 0.01 M HCl, 0.02 M IMI, 0.2% HEC, pH 7.2 (leading electrolyte), 0.01 M HEPES, pH 8.2 (terminating electrolyte), and 25 mM MES, 50 mM TRIS, 30 mM boric acid, 0.2% HEC, pH 8.3 (background electrolyte). All solutions contained 20% methanol. The timing of the transfer of isotachophoretically stacked analyte zones into the CZE column was also optimized. An ITP–CZE method with UV detection at 270 nm was developed for separation of nine phenolic acids (protocatechuic, syringic, vanillic, cinnamic, ferulic, caffeic, ρ-coumaric, chlorogenic, and gentisic acids) in a model mixture and used for assay of some of these acids in a methanolic extract of herba epilobi. Application of ITP–CZE resulted in 100-fold better sensitivity than conventional CZE; limits of detection ranged between 10 and 60 ng mL⁻¹. When MES–TRIS–borate-based buffer, pH 8.3, was used in the CZE separation step the linearity of the ITP–CZE response was satisfactory (correlation coefficients were from 0.9937 to 0.9777). Repeatability was also satisfactory (RSD values ranged between 0.77% and 1.28% for migration times and between 1.65% and 13.69% for peak area). Revised: 23 March and 27 April 2006     

人参茎叶挥发油中含氧化合物的分离与结构鉴定

组成鉴定;人参茎叶挥发油中含氧化合物的分离与结构鉴定     

Evaluation of the results from an inter-laboratory comparison study of the determination of acrylamide in crispbread and butter cookies

Analytical methods currently employed for determination of acrylamide (AA) in two carbohydrate-rich food samples, crispbread and butter cookies, obtained commercially, and native and spiked bread extract samples have been evaluated in a collaborative study. The objective of the study was to obtain information about the performance of the participating laboratories when analysing samples with an AA content close to the limit of quantification (LOQ) and at a higher AA level, and to investigate the influence of sample-preparation procedures on the results of the analysis. For this purpose an aqueous native extract of white bread crumb, a fortified extract, and AA standard solutions, the analyte content of which were not disclosed to the participants, were included in the study. A total of 62 laboratories, applying seven different measurement techniques and a broad spectrum of analyte extraction and sample-preparation procedures reported their analytical results. Because the measurement data were not normally distributed, they were evaluated by application of robust statistics. The relative performance of the laboratories was highlighted by calculation of z-scores. For the crispbread sample, especially, a large percentage of the calculated z-scores were outside the satisfactory range. From their distribution it became obvious that one of the analytical techniques might be biased, if not applied correctly. Consequently, the impact of the applied methods was examined in more detail. Information about the analytical technique, extraction solvent, quantity weighed, calibration method, clean-up, and the experience of the participating laboratories were extracted from the analytical protocols and transcribed into a data matrix which was evaluated by multifactor analysis of variance. The applied measurement technique seems to have a statistically significant influence on the analytical results.     

A novel method for extraction and separation of total flavones and total astragalosides from <Emphasis Type="Italic">Radix astragali</Emphasis>

In this paper a novel method for extraction and separation of total flavones and total astragalosides from Radix astragali using a resin method is suggested. Ethanol is used as the extractant, the macroporous absorption resin modeled H-107 is used to enrich the astragalus extract, and the macroporous strong base anion resin D-280 is used to separate the total flavones and the total astragalosides. This method allows a good yield of total flavones of 600 mg/100 g Radix astragali, a purity of 94.2%, and a yield of total astragalosides of 28 mg/100 g Radix astragali. Published in Khimiya Prirodnykh Soedinenii, No. 1, pp. 26–29, January–February, 2007.     

Chemical characterization and anti-breast cancer effects of silver nanoparticles using Phoenix dactylifera seed ethanolic extract on 7,12-Dimethylbenz[a] anthracene-induced mammary gland carcinogenesis in Sprague Dawley male rats

The aim of the recent research was to investigate the anti-breast cancer effects of silver nanoparticles using Phoenix dactylifera seed ethanolic extract (AgNPs). After preparation of Phoenix dactylifera seed extract, GC/MS was performed to detect the compounds. The findings indicated that 9-Octadecenoic acid (Z)- methyl ester (40.95%) and Dodecanoic acid methyl ester (20%) were the most frequent constituents found in P. dactylifera. These nanoparticles were spherical with a size range of 17-19 nm and characterized using various analytical techniques including UV–Vis absorption spectroscopy to determine the presence of AgNPs in the solution. We studied functional groups of P. dactylifera extract in the reduction and capping process of AgNPs by FT-IR, crystallinity and FCC planes by X-ray diffraction (XRD) pattern and surface morphology, shapes, and size of AgNPs by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). DPPH free radical scavenging test was used to test the antioxidant properties of P. dactylifera and AgNPs, which revealed high antioxidant potential similar to butylated hydroxy toluene (BHT) as the positive control. The results of cytotoxicity analysis indicated that P. dactylifera and AgNPs were toxic for MCF-7 cells. In vivo design, induction of breast cancer was done by 7,12-Dimethylbenz[a] anthracene (DMBA) in 50 animals. After 10 days, the animals were randomly divided into six subgroups, including healthy control, untreated control, two groups receiving the P. dactylifera at 2 and 6 mg/kg and two groups receiving the AgNPs at 2 and 6 mg/kg concentrations. Both doses of P. dactylifera and AgNPs (especially AgNPs6) significantly (p ≤ 0.05) reduced the weight and volume of liver, mammary gland, kidney, spleen, ALP, AST, ALT, GGT, cholesterol, LDL, triglyceride, total and conjugated bilirubin, urea, creatinine, glucose, ferrous, ferritin, erythropoietin, GR, IL1, IL6, IL12, IL18, IFNY, and TNFα and increased HDL, total protein, albumin, WBC, lymphocyte, neutrophils, platelet, RBC, Hb, PCV, MCV, MCH, MCHC, SOD, CAT, GPx, IL4, IL5, IL10, IL13, and IFNα compared to the untreated group. Moreover, P. dactylifera and AgNPs (especially AgNPs6) significantly (p ≤ 0.05) treated breast cancer with reduction of organs free of metastasis compared to the untreated group. Seemingly, the AgNPs can be used for the treatment of breast cancer.     

Effect of plant extracts on book deteriorated fungal species

Abstract

The aim of the study was to evaluate the effect of leaf extracts of four plants against some isolated fungal species from deteriorated books. Aqueous, methanol and chloroform extracts of selected plant species were screened in vitro for their antifungal activity against some book deteriorating fungal species. Fifteen species belonging to 09 genera were isolated and identified from infested books in library. Aqueous and solvent extracts of leaves of Azadiracta indica, Callistemon citrinus, Eucalyptus lanceolatus and Pongamia pinnata were tested against some dominant fungal species viz. Chaetomium spiralis, Alternaria alternata, Aspergillus flavus, Aspergillus niger, Aspergillus fumigatus and Rhizopus stolonifer. Solvent extracts exhibited potent inhibitory activity than aqueous extracts. However, these plant extracts exhibited moderate activity against A. flavus, C. spiralis, R. stolonifer and A. alternata.     

Green synthesis of Pd truncated octahedrons using of firmiana simplex leaf extract and their catalytic study for electro‐oxidation of methanol and reduction of p‐nitrophenol

A facile and eco‐friendly biosynthetic route for preparing Pd truncated octahedrons (PdTOs) using firmiana simplex leaf extract was reported without any chemical reducing agents. The information of reducing components, reduction process and time were obtained by ATR‐FTIR imaging, FTIR and UV–Vis spectroscopy, respectively. TEM image revealed that more than 75% of PdNPs were composed of PdTOs with an average diameter of 9.2 nm. HR‐TEM analysis demonstrated that a single PdTO consisted of the mix of {100} and {111} crystal planes. SAED and XRD pattern confirmed the well crystalline nature of fcc structured PdTOs. The model reactions of electro‐oxidation of methanol and reduction of p‐nitrophenol (p‐NP) were adopted to explore the effects of structure and size of PdNPs on the catalytic properties. In the electro‐oxidation of methanol, the forward‐scan peak current density (If) of PdTOs was 10.05 mA cm‐2, 6.3 times and 1.9 times of PdNPs‐0 and PdNPs‐4:1, illustrating its superior electro‐catalytic property to that of spherical PdNPs. In the p‐NP reduction reaction, the apparent rate constant (Ka) over PdTOs was 0.358 min‐1, higher than spherical PdNPs‐0 (0.08 min‐1) with the similar particle size and lower than the same spherical PdNPs‐4:1 (0.562 min‐1) and commercial Pd/C (0.415 min‐1), which all about half the size of PdTOs. It has been demonstrated that electro‐chemical oxidation of methanol was a structure‐sensitive reaction, while the reduction of p‐NP was mainly dependent on the particle size of PdNPs.