Determination and identification of isoflavonoids in Radix astragali by matrix solid-phase dispersion extraction and high-performance liquid chromatography with photodiode array and mass spectrometric detection

The isoflavonoids in Radix astragali were determined and identified by HPLC-photodiode array detection-MS after extraction employing matrix solid-phase dispersion (MSPD). As a new sample preparation method for R. astragali, the MSPD procedure was optimized, validated and compared with conventional methods including ultrasonic and Soxhlet extraction. The amounts of two major components in this herb, formononetin (6) and ononin (2), were determined based on their authentic standards. Four major isoflavonoids, formononetin (6), ononin (2), calycosin (5) and its glycoside (1), and three minor isoflavonoids, (6aR,11aR)-3-hydroxy-9, 10-dimethoxypterocarpan (7), its glycoside (3), and (3R)-7,2'-dihydroxy-3',4'-dimethoxyisoflavone-7-O-beta-D-glycoside (4), were identified based on their characteristic two-band UV spectra and [M + H](+), [aglycone + H](+) and [A1 + H](+) ions, etc. The combined MSPD and HPLC-DAD-MS method was suitable for quantitative and qualitative determination of the isoflavonoids in R. astragali. (C) 2003 Elsevier B.V. All rights reserved.

Applications of homemade kit in mutation detection of genes

Several methods of mutation detection, such as single-strand conformation polymorphism (SSCP), tandem SSCP/heteroduplex analysis and SNaPshot analysis were developed using homemade kit on ABI 310 genetic analyzer, and were successfully applied to mutation detection of 31 colorectal tumor samples. The sieving capability of homemade kit and commercial kit were compared, results demonstrate that homemade kit has higher resolution and shorter analysis time. In clinical tumor samples, 26% K-ras (exon 1) and 24% p53 (exons 7-8) were found to have mutations, and all mutations were single point variations. A majority of mutations occurred in one gene, only 1 tumor contained alterations in the two genes, which indicates that development of colorectal cancer lies on alternate pathways, and may correlate with different gene mutations.

Study on conical columns with different conical angles for semi-preparative liquid chromatography

The dynamic flow profiles and separation performances in conically shaped preparative liquid chromatographic columns (inlet i.d. larger than outlet i.d.) with three different angles (7, 10 and 15degrees) were studied and compared with cylindrical column of the same length and internal volume. The shapes of dynamic flow profiles were studied by on-column visualization method. The transparent chromatographic columns made of polymethyl methacrylate (PMMA), packed with C-18 bonded silica, were immerged into a cubic pool filled with glycerol to eliminate the cylindrical and conical lens effect. The flow profiles of colored iodine solution in the columns were observed clearly using cyclohexane as mobile phase since the refractive indices of C-18, column wall and the mobile phase are very close. In the conical column of 15degrees (20-7 mm i.d.) the mobile phase in the central region migrated slower than in wall region as it moved toward the column outlet, while in the conical column of 7degrees (17-11 mm i.d.) the mobile phase in the central region migrated faster than in wall region just like in cylindrical column. We found that a plug-like flow profile was generated in the conical column of 10degrees (18-9 mm i.d.) during the whole migration process. A carmine and brilliant blue mixture was used as a probe to test the separation ability of the columns. The resolutions of the two compounds on the conical column of 7, 10, 15degrees and on the cylindrical column were 0.6, 1.57, 1.29 and 0.8, respectively. (C) 2003 Elsevier B.V. All rights reserved.

Chemisorption and reaction characteristics of methyl radicals on Cu(110)

Methyl radicals are generated by pyrolysis of azomethane, and the condition for achieving neat adsorption on Cu(110) is described for studying their chemisorption and reaction characteristics. The radical-surface system is examined by X-ray photoemission spectroscopy, ultraviolet photoemission spectroscopy, temperature-programmed desorption, low-energy electron diffraction (LEED), and high-resolution electron energy loss spectroscopy under ultrahigh vacuum conditions. It is observed that a small fraction of impinging CH3 radicals decompose into methylene possibly on surface defect sites. This type of CH2 radical has no apparent effect on CH3(ads) surface chemistry initiated by dehydrogenation to form active CH2(ads) followed by chain reactions to yield high-mass alkyl products. All thermal desorption products, such as H-2, CH4, C2H4, C2H6, and C3H6, are detected with a single desorption peak near 475 K. The product yields increase with surface coverage until saturation corresponding to 0.50 monolayer of CH3(ads). The mass distribution is, however, invariant with initial CH3(ads) coverage, and all desorbed species exhibit first-order reaction kinetics. LEED measurement reveals a c(2 x 2) adsorbate structure independent of the amount of gaseous exposure. This strongly suggests that the radicals aggregate into close-packed two-dimensional islands at any exposure. The islanding behavior can be correlated with the reaction kinetics and is deemed to be essential for the chain propagation reactions. Some relevant aspects of the CH3/Cu(111) system are also presented. The new results are compared with those of prior studies employing methyl halides as radical sources. Major differences are found in the product distribution and desorption kinetics, and these are attributed to the influence of surface halogen atoms present in those earlier investigations.

Heat capacity and enthalpy of fusion of penconazole (C13H15C12N3)

Low-temperature heat capacities of penconazole (C13H15Cl2N3) were precisely measured with an automated adiabatic calorimeter over the temperature rang from 78 to 364 K. The sample was observed to melt at 332.38 +/- 0.06 K. The molar enthalpy and entropy of fusion of the compound were determined to be 33580 +/- 11 J mol(-1), 101.03 +/- 0.02 J mol(-1) K-1, respectively. Further research of the melting process for this compound was carried out by means of differential scanning calorimetry (DSC) technique. The result was in agreement with that obtained from the measurements of heat capacities. (C) 2003 Elsevier B.V. All rights reserved.

Synthesis of chiral stationary phases with radical polymerization reaction of cellulose phenylcarbamate derivatives and vinylized silica gel

Cellulose phenylcarbamate derivatives having methacrylate groups were synthesized with regioselective and non-regioselective procedures. These derivatives were chemically immobilized onto a vinylized silica gel, respectively, via a radical co-polymerization reaction. The immobilization was efficiently attained using a small amount of AIBN. The chiral recognition abilities of the prepared chiral stationary phases (CSPs) were evaluated by HPLC resolution of test enantiomers. It was observed that most of the enantiomers were completely resolved with markedly high column efficiency of 30,000-40,000 plates per metre for the eluted peaks. The effect of the amount of methacrylolyl chloride used for preparation on resolution was investigated. A direct comparison of the chiral recognition ability was made on the regioselectively and non-regioselectively prepared CSPs. In addition, the chemically bonded-type of CSPs were found to be relatively stable with addition of solvents such as tetrahydrofuran (THF) and chloroform into the mobile phase, which can lead to the dissolution of cellulose derivatives on the coated CSPs. Thus the choice of solvents used as the mobile phase is greatly extended and better resolution of several test enantiomers was observed on the prepared CSPs with THF and chloroform as a composition in the mobile phase. The batch-to-batch and run-to-run reproducibility was also discussed on the newly prepared CSPs. (C) 2004 Elsevier B.V. All rights reserved.

The role of acid strength of zeolites in liquid-phase alkylation of benzene with ethylene

The role of acid strength of zeolites in liquid-phase alkylation of benzene with ethylene was studied over beta, MCM-22, and USY zeolites by means of adsorbing NH3 at different temperatures. The strong acid sites are active centers, while the weak acid sites are inactive. The selectivity behavior of the strong acid sites varies with the relative acid strength as well as the types of the zeolites.

尺度变换的正确率分析

采用优势规则和随机规则为基础的尺度分析方法 ,对分类的 TM数据 (景观类型图 ,包含 8类型 )进行了尺度变换分析。随着尺度的增加 ,优势规则分析方法使景观中优势景观类型的面积增加 ,相反 ,面积较小的非优势景观类型的面积减少。随机规则使各景观类型的面积基本上保持不变。随着尺度的增加 ,随机 K appa指数、位置 Kappa指数和标准 Kappa指数减少。在优势规则分析法中数量 Kappa指数减少 ,但在随机规则为基础的处理中它保持 10 0 %。优势规则处理中的正确率大于随机规则处理的。由景观类型的面积百分比引起的数量正确率在优势规则处理中增加 ,但在随机规则处理中保持 9.6 4 %不变 ;相反数量错误在优势规则处理中明显增加 ,但在随机规则处理中少量增加。偶然正确率保持 12 .5 0 %不变。位置正确率减少 ,相反位置错误明显增加。层和亚层水平上的位置正确率和错误的变化不明显 ,而网格水平上的位置正确率和错误大幅度减少。网格水平上的位置正确率和错误率决定了整个位置正确率和错误率 ,同时位置正确率和错误率基本上决定了整个正确率和错误率。标准Kappa指数大于等于 70 %作为选择依据 ,认为 2 10 m是优势规则处理法的尺度阈值 ,15 0 m是随机规则处理法的尺度阈值 ,欲提高尺度阈值 ,必须改变研究范围或

大兴安岭北部林区景观格局变化及其影响分析

人为干扰影响着景观格局变化的速率和方向 ,这在景观格局变化过程中的作用越来越大 ,同时景观格局的变化也对人类活动产生了重大影响。通过对大兴安岭北部林区的景观多样性指数、优势度指数等一系列景观指数来研究该地区森林景观格局的变化 ,简要分析了格局变化产生的影响。结果表明 ,大兴安岭森林景观中 ,人为干扰使森林景观短时期内多样性增加、森林的优势度降低 ;景观向破碎化趋势发展 ;景观格局的变化对环境和人类活动产生了重大影响 ,森林向不可持续方向发展 ,因此应该进行合理的人类活动使森林可持续发展。

Correlation between the characteristics and catalytic performance of Ni-V-O catalysts in oxidative dehydrogenation of propane

Ni - V - O series catalysts for the oxidative dehydrogenation (ODH) of propane were prepared and characterized by BET, XRD, H-2- TPR, O-2-TPD-MS and electrical conductivity. At 425 degreesC a C3H6 selectivity of 49.9% was observed on Ni0.9V0.1OY at a C3H8 conversion of 19.4%, and the obtained selectivity is almost two times higher than that over NiO at the roughly same conversion of C3H8. The mobile oxygen species created by the interaction of NiO and V2O5 has been found in the composite catalysts by O-2-TPD-MS and electrical conductivity studies, which seems to be responsible for the enhanced selectivity of the propane oxidative dehydrogenation.

光合细菌N9281生物学特性及其应用

从黑龙江省同江水稻根际土壤中分离得到光合细菌N92 81菌株 ,经系统细菌学鉴定定名为球形红假单孢菌 (Rhodop seudomonassphaeroides)。该菌菌体呈卵球形或球形 ,革兰氏染色呈阴性 ,无芽孢 ,能较好利用H2 S ,对碳、氮源利用广泛 ,在厌氧光照条件下培养 72h ,菌数达到 30亿个活菌 mL。在农业生产中 ,以 2L/亩剂量接种 ,田间试验结果表明 :可使波菜增产 2 0 .8%;果实类蔬菜增产 12 .5 - 13.6 %;水稻增产 10 .4 %;人参增产 2 2 .0 3%;出红参率增加 6 .5 %,并减轻人参锈病发病率 ,防治效果达到 6 1.3%。

空间和平衡理论在景观生态学中的发展和应用

传统生态学承认生态系统中平衡、稳定状态的存在 ,“自然平衡理论”是其集中体现。而近 30年来 ,非平衡理论的出现 ,使得人们对生态系统的认识发生了彻底的改变。非平衡理论认为 ,偶然事件 (如干扰等 )在生态过程中起着重要作用。随着认识的转变 ,对生态过程中的“空间”和空间异质性的理解也发生了变化 ,传统生态学总是试图回避空间动态和空间异质性问题 ,而着重强调时间格局的重要性。但在近 2 0年来 ,空间格局则得到了广泛重视。空间理论及空间格局的研究表明 ,空间异质性既可能增加生态系统和生态过程的稳定性 ,也可能降低其稳定性。分析两种变化趋势 ,指出了它们的相互关系 ,同时讨论了空间理论的发展及其在景观生态学中的应用 ,并阐述了生态平衡的含义。

利用柞蚕幼虫繁殖rApNPV的研究初报

利用重组柞蚕核型多角体病毒(RecombinantAntheraeapernyiNuclearPolyhedrosisVirus,rApNPV) ,研究了无包涵体重组病毒(含β-半乳糖苷酶基因)在柞蚕幼虫体内的繁殖情况。结果表明 :无包涵体的重组病毒能够在柞蚕幼虫体内正常繁殖并引起继发感染 ,经柞蚕幼虫繁殖的重组病毒粒子能够完成对柞蚕幼虫的再次创伤感染。重组病毒所携带的β-半乳糖苷酶基因经柞蚕幼虫繁殖后仍能在柞蚕幼虫体内获得高效表达 ,表达量达到经培养细胞繁殖的重组病毒在柞蚕幼虫体内的表达水平 ,说明在利用杆状病毒批量表达外源蛋白时 ,可采用昆虫幼虫体内繁殖方法繁殖重组病毒

辽宁医巫闾山种子植物区系研究

医巫闾山约有野生种子植物 71 8种 ,隶属于 94科 362属之中。依据它们的现代分布 ,这些种被归纳成 2 3个分布区类型和 2 0个亚型。研究表明 ,医巫闾山植物区系属于温带性质 ,但在其发生发展过程中曾经历过与热带相联系的历史渊源。本区系地理联系广泛 ,尤以与东亚地区特别是与日本的联系较为密切 ,其次则是与北温带的联系 ,并且这些成分构成本区系种类组成的主体