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Table of Content
24 August 2003, Volume 19 Issue 3
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Articles
Alkali Metal-incorporated Mesoporous Smectites:Crystallinity and Textural Properties
HE Yan-feng, Shinichiro Fujita, Nobuhiro Iwasa, Bhalchandra M. Bhanage, Masahiko Arai
2003, 19(3): 253-256.
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A series of mesoporous smectite-like materials incorporated with alkali metals such as Li, Na, K and Cs has been synthesized with the hydrothermal method. The crystalline and the pore structures of the materials synthesized significantly change with the introduction of alkali metals. The addition of Li gives highly ordered layer phases, while the incorporation of Cs yields much less crystalline structures. Although Na or K has little effect on the crystalline structure, they modify the pore structure.
Synthesis and Structures of Two New Molybdophosphates
LIN Zheng-zhong, ZHANG Han-hui, HUANG Chang-cang, SUN Rui-qing, YANG Qi-yu
2003, 19(3): 257-262.
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A one-dimension solid and a two-dimension solid consisting of polyoxoanions bridged by {CoO
3
N
2
} and {CoO
4
} groups respectively have been synthesized by the hydrothermal method and structurally characterized by X-Ray crystallography. Each structure has the [(PO
4
)
4
Mo
6
O
15
]
12-
cluster that is commonly observed in many molybdophosphates. In compound 1, [(PO
4
)
4
Mo
6
O
15
]
12-
clusters are linked by {CoO
3
N
2
} groups to form a chain-like structure, and the chains are hydrogen-bonded into a network. Compound 2 is a layer structure with channnels constructed from [(PO
4
)
4
Mo
6
O
15
]
12-
clusters and {CoO
4
} groups, the organic molecules and the lattice water molecules are distributed disorderly in the interlamellar region and form strong hydrogen bonds with inorganic framework. The IR and the fluorescent spectra were investigated and discussed.
Synthesis and Crystal Structure of One-dimensional Chain Complexes [K(18-C-6)]
2
[M(mnt)
2
](M=Zn, Hg)
WANG Da-qi, HE Guo-fang, QIU Lin-lin, DOU Jian-min
2003, 19(3): 263-268.
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The reactions of 18-crown-6 with each of K
2
[M(mnt)
2
](M=Zn, Hg; mnt=1,2-dicyanoethene-1,2-dithiolate, C
2
S
2
(CN)
2
2-
) were studied and novel complexes [K(18-C-6)]
2
[Zn(mnt)
2
](1) and [K(18-C-6)]
2
[Hg(mnt)
2
](2) were characterized by elemental analysis, IR spectrum and X-ray diffraction analysis. Complex 1 displays a one-dimensional chain of [K(18-C-6)]
2
[Zn(mnt)
2
] bridged by K-O interactions between adjacent [K(18-C-6)]
+
units. Complex 2 is also a one-dimensional chain of [K(18-C-6)]
2
[Hg(mnt)
2
] bridged by K...S weak interactions between adjacent [K(18-C-6)]
+
and [Hg(mnt)
2
]
2-
.
Synthesis and Characterization of CdSe Nanocrystals Capped by CdS
SU Xing-guang, LIN Zhang-bi, HU Hai, ZHANG Jia-hua, JIN Qin-han
2003, 19(3): 269-274.
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CdSe semiconductor nanocrystals capped by CdS were synthesized in the aqueous solution with 2-mercaptoethanol as the stabilizer. The CdS capping with a higher band-gap than that of the core crystallite has successfully eliminated the surface traps. Optical absorption and fluorescence emission spectra were used to probe the effect of CdS passivation on the electronic structure of the nanocrystals. The composite CdSe/CdS nanocrystals exhibit strong, narrow(FWHM≤40 nm) and stable band-edge photoluminescence. X-ray powder diffraction, transmission electron microscopy and X-ray photoelectron spectroscopy were used to analyze the composite nanocrystals and determine their average size, size distribution, shape, internal structure and elemental composition.
Fluorescence Microscopic Image Analysis of Nucleic Acids Based on The Capillary Flow Directed Assembly Ring of Neutral Red-nucleic Acid Supramolecular Complexes
LI Yuan-fang, HUANG Cheng-zhi
2003, 19(3): 275-279.
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It is critical to establish a direct and precise method with a high sensitivity and selectivity in analytical chemistry. In this research, making use of a well known phenomenon of capillary flow, we have proposed an image analysis method of nucleic acids at the price of a small amount of sample. When a droplet of the supramolecular complex solution, formed by neutral red and nucleic acids(NA) under an approximate neutral condition, was placed on the hydrophobic surface of dimethyl dichlorosilane pretreated glass slides, and it was evaporated, the supramolecular complex exhibited the periphery of the droplet due to the capillary effect, and accumulated there to form a red capillary-flow-directed assembly ring(CFDAR). A typical CFDAR has an outer diameter of (2
r
) about 1.18 mm and a ring width(2δ) of about 41 μm. Depending on the experimental conditions, a variety of CFDAR can be assembled. The experimental results are in agreement with our former theoretical discussion. It was found that when a droplet volume is 0.1 μL, the fluorescence intensity of the CFDAR formed by the NR-NA is in proportion to the content of calf thymus DNA in the range of 0-0.28 ng, fish sperm DNA of 0-0.24 ng and yeast RNA of 0-0.16 ng with the limit of detection(3σ) of 1.7, 1.4 and 0.9 pg, respectively for the three nucleic acids.
Studies on Non-potentiometric Piezoelectric Sensor System for Determination of Vitamin B
1
YUAN Jin-bin, NIE Li-hua, YAO Shou-zhuo
2003, 19(3): 280-285.
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A piezoelectric sensor responsive to vitamin B
1
was fabricated based on the vitamin B
1
-tetraphenylborate ion pair. The general performance characteristics of the sensor are presented here. The proposed sensor showed a wide working pH range, a good sensitivity and selectivity. The response range is between 1.0×10
-7
-4.9×10
-5
mol/L with a detection limit of 8×10
-8
mol/L at pH 4.0. The selectivity should be attributed to the preferential adsorption of the component ion on the membrane/solution interface. The adsorption behavior of vitamin B
1
on the crystal surface was investigated with a quartz crystal impedance(QCI) system.
Chemical Characteristic of Bioactive Polysaccharides Isolated from
Ornithogalum caudatum Ait.
SHI Lei, LI Juan, LIU Wen-Xiang, WANG Yong, LIU Zhi-qiang, LIU Shu-ying
2003, 19(3): 286-289.
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A water-soluble crude extract prepared from Ornithogalum caudatum Ait.(OCA) showing a high immunomodulating activitiy was isolated and characterized by virtue of gel filtration and column chromatography. The presence of the monosaccharides has been established by the chemical analysis. The quantitative analysis of the alditol acetate derivatives of them showed the ratios of the monosaccharides analyzed by means of GC respectively. The concentrations of protein(280 nm) and carbohydrate(496 nm) were detected respectively. The information of the molecular weight from the pure polysaccharide was obtained by several standard Dextrans from the Sephadex chromatography.
Voltammetric Studies on Heteropoly Phosphotungstovanadate Anions Across the Liquid/Liquid Interface
LU Xiao-quan
2003, 19(3): 290-293.
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Electrochemical transfer behavior of V
Ⅴ
W
11
-V
3
Ⅴ
W
9
heteropoly anions on the water/nitrobenzene interface was investigated by means of cyclic voltammetry. The effect of the solution acidity on the transfer behavior and the stable pH range for the heteropoly anions were studied. The stability of mixed tungstovanadate decreases with increasing the number of vanadium atoms. The main transfer species within the potential window have the negative charges of 4 and the transfer process is diffusion-controlled. The apparent transfer potential Δ
w
o
Ψ
0
and the free energy ΔG
0
tr
w→o
for the heteropoly anions can be obtained from the experimental data. For the different anions, the Δ
w
o
Ψ
1/2
-pH relationship can be expressed as: Δ
w
o
Ψ
1/2
=constant-53pH.
Synthesis of 6
E
-Geranylgeraniol-19-oic Acid
LI Shu-hua, PENG Li-Zeng, LI Wei-dong, LI Yu-lin
2003, 19(3): 294-296.
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The present paper deals with the facile synthesis of 6E-geranylgeraniol-19-oic acid(1), a naturally occuring alicyclic diterpene acid, by a Horner-Wadsworth-Emmons olefination of two readily available fragments 7 and 3.
Synthesis and Biological Activity of New Pyrethroid Acid Oxime-esters Containing Pyrazole Ring
MA Jun-an, HUANG Run-qiu, FENG Lei, SONG Jian, QIU De-wen
2003, 19(3): 297-301.
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A series of compounds containing oxime-ester linkage and pyrazole ring(in place of the ester linkage and the alcohol moiety in pyrethroid ester) was designed and synthesized. The structures of all the compounds prepared were confirmed by
1
H NMR and MS spectroscopy as well as elemental analyses. The bioassay data of those compounds against tobacco mosaic virus(TMV), cucumber mosaic virus(CMV), potato virus X(PVX) and potato virus Y(PVY) were presented. Among them compound 6i was found to possess significant plant antiviral activities. But all the compounds showed low insecticidal and acaricidal activities.
Efficient Synthesis of 2-(8-Quinolinoxy)-4
H
-imidazolin-4-ones
DING Ming-wu, SHU Ya-li, LIU Zhao-jie
2003, 19(3): 302-305.
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The title compounds 2-(8-quinolinoxy)-4H-imidazolin-4-ones(4) were synthesized by means of base catalytic reactions of 8-hydroxyquinoline with each of carbodiimides 2, which were obtained via aza-Wittig reactions of iminophosphoranes 1 with the corresponding aromatic isocyanates.
Studies on Syntheses and Biological Activities of Novel Triazole Compounds Containing Phosphorodithioate Groups
XU Liang-zhong, ZHANG Shu-sheng, CHEN Xiao, JIAO Kui
2003, 19(3): 306-309.
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Sixteen new triazole organic phosphorus compounds were synthesized. Their structures were confirmed with IR,
1
H NMR, elemental analysis and MS. The primary biological tests show that the titled compounds have the fungicidal activities, which are influenced by R groups and the substituents attached to the P atom.
Studies on Synthesis and Biological Activities of Novel Triazole compounds Containing Thiophene Groups
XU Liang-zhong, ZHANG Shu-sheng, HU Zhi-qiang, JIAO Kui
2003, 19(3): 310-313.
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Fifteen new triazole compounds containing thiophene groups were synthesized and their structures were confirmed by means of
1
H NMR, IR, MS spectroscopies and elemental analyses. The preliminary biological tests show that the titled compounds exhibit some activities of fungicides and plant growth regulators.
A Study of Bioactivity of Corn Peptides with Low Molecular Weight Ⅱ: Effect on Plasma Free Amino Acid Concentrations in Rats
XU Li, ZHANG Li-qiang, WU Xiao-xia, WANG Na, ZHANG Xue-zhong
2003, 19(3): 314-316.
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The effects of the ingestion of corn peptides with a low molecular weight(LMCP) prepared from zein on some plasma free amino acid concentrations in rats that had taken ethanol were investigated. LMCP(1.0 g/kg body weight) in 15% ethanol(10 mL/kg body weight) was given to Wister rats by intragastrical administration. The amino acid analysis showed that the concentrations of alanine, leucine, and proline in the plasma reached their maximum levels at 30 min for the LMCP-intake group. They are 582.39, 99.60 and 272.51 μg/L, respectively. But in the control group, the plasma free amino acid levels were not changed obviously. Therefore, LMCP could cause an increase in concentration of some free amino acids such as alanine, leucine and proline etc. in plasma of the rats that have taken ethanol.
Chemical Modification of Amino Acid Residues in Human Plasminogen
LIANG Fang, SUN Hong, ZHAO Cheng-guang, CUI Ting, HONG Shui-sheng, CHEN Jia, LIU Lan-ying
2003, 19(3): 317-319.
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The chemical modification of human plasminogen(HPg) was studied with 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide(EDC), N-acetylimidazole(NAI), 1,2-cyclohexanedione(CHD), chloramine T(Ch-T) and N-bromosuccinimide(NBS) as modifying reagents at its carboxyl group, tyrosine, arginine, methionine and tryptophan residues, respectively. The results indicate that tyrosine and arginine residues are not essential for HPg activity, while carboxyl groups, methionine and tryptophan residues are important for the activity of HPg. The Keech and Farrant′s kinetic analysis reveals that one tryptophan residue, one methionine residue and two carboxyl groups are essential for HPg activity.
Formation Mechanism and Emission Spectrum of AlO Radicals in Reaction of Laser-ablated Al Atom and Oxygen
ZHANG Shu-dong, LI Hai-Yang
2003, 19(3): 320-323.
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The emission spectrum of AlO radicals was analyzed in 440-540 nm in the reaction of laser ablated Al beam and O
2
. The carrier of spectrum was assigned to Δν=0, ±1, ±2 vibrational sequences of B
2
Σ
+
-X
2
Σ
+
transition of AlO radicals, the observed maximum vibrational quantum number was ν′=6. The rotational and vibrational temperatures of B state were estimated at 3000 and 7500 K by spectrally simulating the rovibronic population distribution. There is a strong evidence that the production of excited Al(
2
S) atoms is essential to the formation of excited AlO radicals.
Immobilization of Penicillin G Acylase on Calcined Layered Double Hydroxides
REN Ling-ling, HE Jing, Evans D. G., DUAN Xue
2003, 19(3): 324-329.
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A hydrotalcite-like Mg
2+
/Al
3+
layered double hydroxide(LDH) material was prepared by means of a modified coprecipitation method involving a rapid mixing step followed by a separate aging process. LDH calcined at 500 ℃, denoted as CLDH, was characterized by XRD, IR and BET surface area measurements. CLDH has a poor crystalline MgO-like structure with a high surface area and porosity. CLDH was used as a support for the immobilization of penicillin G acylase(PGA). The effect of varying the immobilization conditions, such as pH, contact time and the ratio of enzyme to support, on the activity of the immobilized enzyme in the hydrolysis of penicillin G has been studied. It was found that the activity of the immobilized enzyme decreased slightly with decreasing pH and reached a maximum after a contact time of 24 h. The activity of the immobilized enzyme increased with increasing the ratio of enzyme to support. It was found that the adsorption of PGA inhibited the expected reaction of CLDH with an aqueous medium to regenerate a LDH phase. Its original activity(36%) after 15 cycles of reuse of the immobilized enzyme was retained, but no further loss in the activity was observed.
Characterization and Catalytic Activity of Titanium-containing Aluminum Phosphate Prepared by Sol-gel and Nonuniform Precipitation for O-Alkylation of Catechol with Ethanol
PAN Chun-liu, ZHANG Wen-xiang, LI Xue-mei, JIANG Da-zhen, WU Tong-hao
2003, 19(3): 330-334.
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Three titanium-containing aluminum phosphate catalysts with a general formula Al
0.77
Ti
0.23
PO
4
were prepared by the sol-gel method at room temperature(APTS), and a nonuniform precipitation procedure at room temperature(APTR) and under reflux(APTF), respectively. The structural features and the surface properties of the three catalysts were determined by means of the physical adsorption of nitrogen at liquid N
2
temperature, XRD, UV-Vis, NH
3
-TPD and IR of adsorbed pyridine. The vapor phase O-alkylation of catechol with ethanol over the prepared catalysts was studied. It was found that the activity and the selectivity of these catalysts are greatly dependent on the preparation method, and catalyst APTF shows the highest activity and selectivity. The characterization evidence indicates that the weak Brönsted acid sites were more effective for the reaction.
Catalytical Activities of Reconstructed Hemoglobin with Different Central Ions in Prosthetic Group
LIU Jian-yu, SUN Bao-wei, LI Yuan-zong, CHANG Wen-bao
2003, 19(3): 335-339.
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Hemoglobin(Hb) was de-prosthetized, which was then reconstructed with the prosthetic groups with different central metal ions including Fe(Ⅲ), Co(Ⅱ) and Mn(Ⅱ). The spectral properties along with the catalase and peroxidase activities of the reconstructed hemoglobin were compared with those of Hb and prosthetic groups with different ions. When the central ion is iron, the reconstituted Hb(rHb) has the highest catalase and peroxidase activities. Maybe it is the reason that iron is chosen as the central ion in the prosthetic groups of natural hemoproteins. Different from peroxidase activity, the catalase activity of hemin cannot be enhanced by the microenvironment of apoHb. This result shows that the structure of apoHb is more similar to that of apoHRP than that of apocatalase.
The Relationship Between Relative Hydration Free Energies of
99m
TcON
2
S
2
Complexes and Their Brain Uptakes
SONG Wei, XUE Ying, CHEN Wei-zu, WANG Cun-xin, JIA Hong-mei, LIU Bo-li
2003, 19(3): 340-343.
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A thermodynamic integration dual-transform method was firstly applied to calculating the relative hydration free energies of
99m
TcO-N
2
S
2
complexes. The relationship between the brain uptakes(B.U.) of
99m
TcO-N
2
S
2
complexes with different substituted functional groups and their relative hydration free energies was investigated. The simulation results show that the experiment brain uptake(B.U.) data are strongly influenced by the relative hydration free energies of
99m
TcO-N
2
S
2
complexes, thus the simulations can provide the useful information for the medicine design of
99m
Tc brain imaging agents.
A Raman Study of Spinel LiMn
2
O
4
WANG Chun-zhong, GONG Jie, LIU Wei, WEI Ying-jin, WU Feng, CHEN Gang
2003, 19(3): 344-346.
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A Raman study was carried out for LiMn
2
O
4
, which was synthesized via the mixture of Mn
3
O
4
and LiNO
3
sintered at different temperatures. It is shown that there are two kinds of Raman spectra for LiMn
2
O
4
at different sintering temperatures, while the X-ray diffraction patterns of LiMn
2
O
4
sintered at different temperatures are the same. Five Raman bands observed for the materials sintered below 500 ℃ are consistent with the theoretical prediction for spinel structure based on the group theory. Only two Raman bands were observed for the materials sintered at temperatures higher than 500 ℃. The best preparation condition for obtaining a good spinel LiMn
2
O
4
is suggested based on the Raman study.
Dielectric Properties of Nanocrystalline TiO
2
Prepared by the Stearic Acid Gel Method
DONG Wei, RUAN Sheng-ping, ZHANG Xin-dong, GUO Wen-bin, LIU Cai-xia, ZHANG Shuang, JIA Cui-ping, PAN Jian-xuan, CHEN Wei-you
2003, 19(3): 347-349.
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Nanocrystalline TiO
2
was prepared by means of a stearic acid gel method. The product was investigated by differential thermal analysis, thermogravimetric analysis, X-ray powder diffraction and transmission electronic microscopy(TEM). The results of the dielectric properties tested indicate that the dielectric constant of anatase-form nanocrystalline TiO
2
is much higher than that of the coarse crystal. The dielectric constant of the nanocrystalline material is not related with the amplitude of an external AC field in a certain range.
Synthesis of 3-(1-Cyclohexenyl)-2-butanone via Environmentally Friendly Catalysts
ZHAO Zhen-hua
2003, 19(3): 350-354.
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We substituted several environmentally friendly catalysts which included HY and H-β zeolites, various cation-exchanged β zeolites, and solid-supported ferric chloride for conventional catalysts for the synthesis of 3-(1-cyclohexenyl)-2-butanone from the reaction of ethylidenecyclohexane with acetic anhydride at room temperature. HY zeolite was found to be the most effective for this reaction, and gave the acylated product in a 72% yield under the conditions of n(ethylidenecyclohexane)/n(acetic anhydride)/m(HY zeolite)=1 mmol/10 mmol/0.100 g, reaction temperature 25 ℃ and reaction time 2 h. The used HY zeolite can be recovered, regenerated and gave almost the same yield as the fresh one. The lifetime of the HY zeolite is over 80 h. The effect of different factors on the reaction has also been investigated.
Theoretical Studies on Thermal Decomposition of Benzoyl Peroxide in Ground State
SUN Cheng-ke, YANG Si-ya, LIN Xue-fei, MA Si-yu, LI Zong-he
2003, 19(3): 355-361.
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Systematic studies of the thermal decomposition mechanism of benzoyl peroxide(BPO) in ground state, leading to various intermediates, products and the potential energy surface(PES) of possible dissociation reactions were made computationally. The structures of the transition states and the activation energies for all the paths causing the formation of the reaction products mentioned above were calculated by the AM1 semi-empirical method. This method is shown to to be one predict correctly the preferred pathway for the title reaction. It has been found that in ground state, the thermal decomposition of benzoyl peroxide has two kinds of paths. The first pathway PhC(O)O-OC(O)Ph→PhC(O)O
·
→Ph
·
+CO
2
produces finally phenyl radicals and carbon dioxide. And the second pathway PhC(O)OO-C(O)Ph→PhC(O)OO
·
+PhC(O)
·
→PhC(O)
·
+O
2
→Ph
·
+CO+O
2
, via which the reaction takes place only in two steps, produces oxygen and PhC(O)
·
radicals, and the further thermal dissociation of PhC(O)
·
is quite difficult because of the high activation energy in ground state. The calculated activation energies and reaction enthalpies are in good agreement with the experimental values. The research results also show that also the thermal dissociation process of the two bonds or the three bonds for the benzoyl peroxide doesn′t take place in ground state.
Density Function Theory Studies on Reaction of HCS with OH
PEI Ke-Mei, LI Yi-Min, LI Hai-Yang
2003, 19(3): 362-365.
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The exothermic reaction of HCS with OH on the single-state potential energy surface was explored by means of Density Function Theory(DFT). The equilibrium structural parameters, the harmonic vibrational frequencies, the total energies and the zero point energies(ZPE) of all the species in the reaction were computed. Six intermediates and seven transition states were located, three exothermic channels were found. The frequency analysis and the Intrinsic Reaction Coordinate(IRC) calculation confirm that the transitions are truthful. The results indicate that there are three exothermic channels and their corresponding products are: P1(H
2
O+CS), P2(H
2
S+CO), P3(OCS+H
2
), and P1 has a larger branch ratio.
Studies on Adsorption Behavior and Mechanism of Copper(Ⅱ) onto Amino Methylene Phosphonic Acid Resin
XIONG Chun-hua, WANG Yong-jiang, SHI Lin-mei
2003, 19(3): 366-369.
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The adsorption behavior and the mechanism of a novel chelate resin, amino methylene phosphonic acid resin(APAR) for Cu(Ⅱ) were investigated. Cu(Ⅱ) was quantitatively adsorbed by APAR in the medium of pH=4.09. The statically saturated adsorption capacity is 181 mg/(g resin). Cu(Ⅱ) adsorbed on APAR can be eluted by 1.0-3.0 mol/L HCl. The rate constant is k
298
=5.58×10
-5
s
-1
. The adsorption of Cu(Ⅱ) on APAR follows the Freundlich isotherm. The ΔH of the adsorption is 3.91 kJ/mol. The apparent activation energy is E
a
=21.4 kJ/mol. The coordination molar ratio of APAR to Cu(Ⅱ) is 1/1. It is shown that the nitrogen and the oxygen atoms in the functional group of APAR coordinate to Cu(Ⅱ).
Probability Properties of Multi-contact in Protein Molecules
WANG Xiang-hong, KE Jian-hong, HU Min-xiao, ZHANG Lin-xi
2003, 19(3): 370-375.
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The compact conformations of polymers are important because the native conformations of all bio-polymers with certain function are highly compact. The properties of mutil-contact bio-polymer chains were studied by Gaussian statistics of the random-flight chain. The theoretical expressions(were given, also), the calculations of probability distributions and correlation functions for different topologic cases were derived and made respectively. Comparison between single, double and triple contacts was also made. By means of setting the parameters, the results of the current calculations of the multiple contacts are just the same as those calculated by single, double or tripe contacts separately. It is a useful method to investigate native conformations of biopolymers. The probabilities of multi contacts and correlation functions between chains contacts were calculated for the Gaussian chains. Because the bond probability distributions are Gaussians distributions, the probability distributions of the separations of various points along the chains are always consecutive. All the contacts may break up into several groups, and each group consists of many contacts. Here we investigated the probability distribution from one group to three groups of contacts.
In situ Coordination and Surface Morphology of Langmuir Films of Non-amphiphilic Dithizone with Metal Ions on Air/Water Interface
WU Yi-tian, LIU Ming-hua
2003, 19(3): 376-378.
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Jihong YU
ISSN 1005-9040
CN 22-1183/O6
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