New diterpenoid glucosides from Siegesbeckia pubescens

Plants of the genus Siegesbeckia are annual herbs widely distributed in tropical and temperate zones and they are used as a traditional medicine to treat rheumatic arthritis, hypertension, malaria, neurasthenia and snake-bite in China. In previous papers, we reported on five new ent-kaurane and ent-pimarane diterpenoids, siegesbeckioside, siegesbeckiol and siegesbeckic acid1, orientalin A and B, and eight know compounds2,3. The present paper describes the isolation and structural elucidation …     

One-Pot Synthesis of N-Boc-2, 5-bis(trimethylsilyl)pyrrolidine

Since Daly reported the structure of epibatidine and its potent analgesic activity in 19921, study on the synthesis of epibatidine and its derivatives and relationships between the structure and activity of epibatidine has received much attention2. During the course of our research for the synthesis of epibatidine derivatives, N-boc-2, 5-bis(trimethylsilyl)pyrrolidine 4 was used as the key intermediate to construct the skeleton of epibatidine via the 1, 3-dipolar cycloaddition (Scheme 1). Ac…     

Molecular Arrangement of a Bolaamphiphilic Anthrancene Derivative in Langmuir-Blodgett Film

Langmuir monolayer at the air/water interface is the basis to understand the molecular arrangement and to fabricate the organized molecular films1. Bolaamphiphiles describes the molecules in which two head functional groups are linked by one or two hydrophobic chains2,3. In comparison with the one-headed amphiphile, abundant configurations of Langmuir monolayer are expected in bolaamphiphiles. Generally, three kinds of configurations of the Langmuir monolayers of bolaamphiphile at the air/w…     

Cobalt Determination by Means of Flow Injection On-line Sorbent Preconcentration-Flame Atomic Absorption Spectrometry with 1-Nitroso-2-naphthol as a Complexing Reagent

The suitability of 1-nitroso-2-naphthol(NN) as a complexing agent for on-line preconcentration of cobalt eluted on the C_(18) microcolumn by means of the FI-FAAS system was tested. Various parameters affecting the complex formation and its elution were optimized. A 2.3×10~(-3) mol/L reagent solution and the aqueous sample solution acidified with 0.1％ (volume fraction) nitric acid were on-line mixed (6.4 mL/min) on a reaction coil set at (65±1)℃ and flowed through the microcolumn for 30 s. The pH of the mixed solution was adjusted to 3—4 with HNO_3(1 mol/L) or NaOH(1 mol/L). The adsorbed complexes in the microcolumn were eluted into the nebulizer of FAAS in 10 s with ethanol acidified with 1％ HNO_3(3.0 mL/min). A good precision(1.6％ for 100μg/L Co(Ⅱ), n=10), a high enrichment factor 17.2, with detection limit (3σ) 3.2μg/L, and sample throughput (90 h~(-1)) were obtained. The method was applied to the certified reference materials(CRMs), NBS-362 and NBS-364, for the determination of cobalt and the results were in good agreement with the certified values.     

Studies on the Electrochemical Behavior of Bleomycin at a Co/GC Ion Implantation Modified Electrode and Its Application

In a 0. 10 mol/L HAc-NaAc buffer solution (pH = 4. 59), a sensitive reduction peak of bleomycin was observed by linear sweep voltammetry at a Co/GC ion implantation modified electrode. The peak potential was-0. 73 V(iw. SCE). The peak current was proportional to the concentration of bleomycin over the range of 5.0 × 10-8-1.0× 10-6 and 1.0× 10-6-1. 0 × 10-5 mol/L with a detection limit of 2.0 × 10-8 mol/L. The electrochemical behavior of the reduction peak of bleomycin at the Co/GC modified electrode was studied by linear sweep and cyclic voltammetry and applied to the determination of bleomycin in urine. This method is simple, rapid and reliable. The reduction process is quasi-reversible. The experiments of AES and XPS showed that Co was surely implanted into the surface of GCE and the depth distribution of Co was in good agreement with Gooses normal distribution; the implanted Co at GCE improved the electrocatalytic activity.     

Time-resolved ESI-MS Investigation on Reduction and Alkylation in Unfolding Process of Lysozyme

The kinetic procedure of the unfolding of lysozyme induced by the reduction of disulfide was monitored by the time-resolved ESI-MS with a sheath liquid assistant electrospray interface. It was found that the reduction process for the eight disulfides had a less difference in the reaction time after denatured treatment. In addition, the alkylation of the reduced free thiols was much slower than the reduction procedure. An artifact peak produced by the CID fragmentation in the mass spectra was identified and the possible mechanism of the Hofmann elimination reaction was proposed.     

New Soluble Fluorinated Polyimides

Aromatic polyimides have been widely used in aerospace, electrical and electronic applications due to their outstanding thermal stability, mechanical strength at elevated temperature and electrical properties1-3. However, polyimide materials are usually difficulty to fabricate owing to their insolubility in most organic solvents and infusibility. Besides solubility, low moisture uptake of polyimide is also a major concern for microelectronics and optical applications. The present article descr…     

Crystal and Molecular Structure of 1-Phenoxy(α-methyl)acetyl-2-diethylamino-3-phenyl-1,3,2-diazaphospholidin-4-one-2-sulfide

1　INTRODUCTIONAsherbicides,thearyloxycarboxylicacidssuchas2,4-D(2,4-Dichlorophenoxyaceticacid)etc.havenotbeenusedwidelysince1970sbecauseoftheircausingenvi-ronmentalpollutionandinjuriestothecrops.Studiesonthenewtypeofherbicideshavebeendevelopinginrecentyears.Itwasreportedrecentlythatthederivativesofdiazaphospholidinoneorthecorrespondingthionespossessinterestingherbicidalactiv-ity[1～3].Itwasalsoknownthat1,4,2-diazaphospholidine-5-thione-2-oxideshasgoodselectiveherbicidalactivity[4,5],but…     

CdS纳米粒子的表面修饰及其对光学性质的影响

用反胶束法合成了用表面活性剂分子磺基焉珀酸双－２－乙基已酯钠盐（ＡＯＴ）进行表面修饰的ＣｄＳ纳米粒子（记为ＣｄＳ／ＡＯＴ－ＳＯ３＾－）,研究了这种纳米粒子在正庚烷（ｈｅｐｔａｅ）和吡啶（Ｐｙ）溶剂中的荧肖及光解行为,发现其在正庚烷中荧光很强,而Ｐｙ却强烈地猝灭ＣｄＳ纳一子的荧光,用电荷转移猝灭机制进行了解释,这种解释为ＣｄＳ纳米粒子在Ｐｙ中光解实验进一步证实。     

K3C60单晶膜的同步辐射光电子谱研究

在C₆₀单晶(111)解理面上制备出厚度约30 nm的K₃C₆₀单晶膜.利用同步辐射光源,在低温下(约150K)测量了样品法向发射的角分辨光电子谱.观察到K₃C₆₀导带和价带明显的色散.导带的光电子谱峰可清晰分辨出4个子峰,这些子峰的最大色散超过0.5eV,并且色散曲线与K₃C₆₀的一维无序晶体结构模型下的能带理论基本吻合,只是子带间隔差异较大.