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Table of Content
24 July 2005, Volume 21 Issue 4
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Articles
Synthesis, Structure Characterization and Biological Activity of a Novel Polyoxovanadate Cluster: [NH
3
(CH
2
)
2
NH
2
(CH
2
)
2
NH
3
]
4
·[V
6
Ⅴ
V
12
Ⅳ
O
42
(PO
4
)](PO
4
)·2H
2
O
FU Ping-ping, WANG Xin-long, WANG En-bo, QIN Chao, XU Lin
2005, 21(4): 381-385.
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A new polyoxovanadate cluster,[NH
3
(CH
2
)
2
NH
2
(CH
2
)
2
NH
3
]
4
[V
6
Ⅴ
V
12
Ⅳ
O
42
(PO
4
)](PO
4
)·2H
2
O, has been synthesized and characterized by means of elemental analysis, IR spectrometry, EPR spectrometry, TG analysis and single crystal X-ray diffraction. This compound crystallizes in a monoclinic space group C2/c with a=2.3912(5) nm, b=1.3002(3) nm, c=2.0172(4) nm, β=105.75(3)°, V=6.036(2) nm
3
, Z=2, R
1
=0.0572, wR
2
=0.1476. It has a superKeggin structure with a Keggin unit capped by six [VO
5
] moieties on the pits on every side of the Keggin unit. The anti-tumor activity of the compound was estimated in three human tumor cell lines
in vitro.
Heterogeneous Photocatalytic Mineralization of Chlorobenzene by Paratungstate-loaded Titania Catalysts in an Aqueous Medium
YUE Bin, JIANG Lei, HU Chang-wen, CHEN Jian-min, HE He-yong
2005, 21(4): 386-390.
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Paratungstate-loaded titania catalysts were prepared via the addition of a series of aqueous solutions of paratungstate(denoted as W
7
) into an isopropanol solution of Ti[OCH(CH
3
)
2
]
4
by means of the sol-gel method. The catalysts were characterized by EDX, BET, FTIR, UV-Vis DRS, XRD and the results indicate that such paratungstate-loaded catalysts maintained their heptatungstate structure in the anatase titania matrix up to 400 ℃. The catalysts were tested for the heterogeneous photodegradation of chlorobenzene in aqueous media and showed a better catalytic activity than P-25 TiO
2
because paratungstate can prevent the recombination of the holes and electrons produced during irradiation. Moreover, the paratungstate-loaded titania catalysts can resist the disaggregation during the photoirradiation and can be easily recycled from the aqueous suspensions after reactions.
Synthesis and Structural Characterization of Mono- and Di-nuclear Zinc(Ⅱ) Coordination Compounds of Triphenylphosphoniopropionate
LI Song-lin, HOU Jian-feng, JIANG Ning-yi, Mak Thomas C. W.
2005, 21(4): 391-395.
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Two novel coordination compounds of Zn(Ⅱ) with PH
3
P
+
(CH
2
)
2
CO
2
-
(L), namely, [ZnL
4
(H
2
O)
2
]·(ClO
4
)
2
·2H
2
O(compound 1) and [Zn
2
Cl
4
(μ-L-O,O′)
2
](compound 2), have been prepared. The single crystal X-ray structure analysis of these compounds indicates that in compound 1 the Zn(Ⅱ) atom is coordinated by four monodentate carboxylato groups on the equatorial plane and two aqua ligands occupy the axial coordination positions. The pendant oxygen atoms form strong hydrogen bonds with the aqua molecules which results in the stability of this structure. In compound 2, two Zn(Ⅱ) atoms are bridged by a pair of carboxylato groups, showing a skew-bridge mode, and thus enabling a long Zn(Ⅱ)…Zn(Ⅱ) separation. As we know, it is a dinuclear coordination compound with the longest Zn…Zn separation.
Syntheses, Structural Characterization of Fe and Ni Complexes with Polypyrazolyl Borate Ligand:Fe[HB(pz)
3
]
2
and Ni[HB(pz)
3
]
2
XING Yong-heng, Katsuyuki Aoki, BAI Feng-ying
2005, 21(4): 396-400.
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Fe(Ⅱ) complex Fe[HB(pz)
3
]
2
(compound 1, pz=pyrazole) and Ni(Ⅱ) complex Ni[HB(pz)
3
]
2
(compound 2) have been obtained by the reaction of MCI
2
(M=Fe and Ni) with NaHB(pz)
3
in MeOH. The two complexes(compounds 1 and 2) were characterized by IR, NMR, elemental analysis and X-ray diffraction. Compound 1 crystallizes in space group P2
1
/c with a=1.224(3) nm, b=1.161(2) nm, c=1.648(3) nm, β=107.62(15)°, V=2.233(8) nm
3
, Z=2. Compound 2 crystallizes in space group P2
1
/c with a=0.97926(18) nm, b=1.7423(3) nm, c=1.3156(2) nm, β=97.055(16)°, V=2.2277(7) nm
3
, Z=4. The results of X-ray structural analyses show that both compounds 1 and 2 are monomeric neutral, possessing a similar coordination mode and a similar structure around the metal centers. The related spectral characterizations, steric effects and binding properties are discussed.
Assembly and Electrochemical Study of Transition Metal Substituted Polyoxometalates SiW
11
NiO
39
6-
and SiW
11
MnO
39
6-
on 4-Aminothiophenol Modified Glassy Carbon Electrode
LÜ Gui-qin, DU Jin-yan, HU Chang-wen
2005, 21(4): 401-405.
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Via
layer-by-layer assembly, the polyoxometalates of Keggin type, SiW
11
O
39
Ni(H
2
O)
6-
(SiNiW
11
) and SiW
11
O
39
Mn(H
2
O)
6-
(SiMnW
11
) were first immobilized on a 4-aminothiophenol(4-ATP) modified glassy carbon electrode surface. The electrochemical behavior of these polyoxometalates was investigated. They exhibited some special properties in the films, which are different from those in a homogeneous aqueous solution. Their reaction mechanism in a multilayer film is proposed. The electrocatalytic behavior of these multilayer film electrodes for the reduction of BrO
3
-
and NO
2
-
were comparatively studied.
Synthesis, Structure and Characterization of Manganese(Ⅱ) Coordination Polymer with Camphoric Acid and 1,10-Phenanthroline
HOU Ying, SHI Zhan, YANG Ming, LI Guang-hua, FENG Shou-hua
2005, 21(4): 406-410.
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A novel coordination polymer, Mn(H
2
O)(CA)(Phen)·H
2
O(CA=camphoric acid, Phen=1,10-phenanthroline), was synthesized and its crystal structure was determined by single crystal X-ray diffraction. Six-coordinated Mn(Ⅱ) atoms are linked with carboxyl groups from camphoric acid ligands to form infinite one-dimensional chains. These chains are packed by means of hydrogen bonding and π-π stacking, forming a three-dimensional structure. IR, thermogravimetric analysis and magnetic susceptibility data for Mn(H
2
O)(CA)(Phen)·H
2
O are given.
Transformation of 1-D Chiral-chained Titanium Phosphate to 2-D Layer Structure Through a 1-D Zigzag Chain
CHEN Chao, YANG Yu-lin, LI Wei-sheng, LIU Yun-ling, YI Zhuo, GUO Yang-hong, PANG Wen-qin
2005, 21(4): 411-414.
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The transformation of titanium phosphate from 1-D chiral- chain(JTP-A) to 2-D layer(TP-J1) has been carefully investigated. Through a hydrolysis-condensation self-assembly pathway, the crystals of TP-J1 can be obtained from the JTP-A phase under hydrothermal conditions. An intermediate material with zigzag chain during the transformation was observed by XRD characterization. A hypothesis of the transformation mechanism is also described in this article. It is noteworthy that ethylenediamine plays an important role in the transformation.
Synthesis and Crystal Structures of the α and β Forms of Bis(salicylaldoxime)copper(Ⅱ) Complexes
WAN Jun, WANG Shi-ying, WEN Yong-hong, YE Su-juan, OUYANG Ping-kan, ZHANG Shu-sheng
2005, 21(4): 415-418.
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Modified α and β bis(salicylaldoxime)copper(Ⅱ) have been obtained by recrystallization from ethyl acetate(CCDC Nos. 212157 & 212158). The X-ray analysis reveals that the two modificated forms have the same structure with different geometric parameters. The α form crystallizes in the P2(1)/c space group and the β form in the P1 space group. Both the crystal structures consist of centrosymmetric monomeric molecules of Cu(OC
6
H
4
CNOH)
2
. The IR spectra are in agreement with the structural data.
Synthesis, Crystal Structure and Characterization of α-(1-Benzimidazolyl)-hypnone Cobalt(Ⅱ) Complex:[CoCl(C
7
H
5
N
2
CH
2
COPh)
4
]Br
JIAN Fang-fang, SUN Ping-ping, XIAO Hai-lian, ZHAO Pu-su
2005, 21(4): 419-422.
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The crystal structure of [CoCl(C
7
H
5
N
2
CH
2
COPh)
4
]Br has been determined by means of X-ray crystallography. The molecular structure consists of a discrete [CoCl(C
7
H
5
N
2
CH
2
COPh)
4
]
+
cation and one Br
-
anion. In the [CoCl(C
7
H
5
N
2
CH
2
COPh)
4
]
+
cation, the coordination geometry of the central Co atom is square-pyramidal with four tertiary N atoms of benzimidazole from four α-(benzimidazol-1-yl)-hypnone ligands in the basal position and one chloride anion in the apical position. In the solid state, [CoCl(C
7
H
5
N
2
CH
2
COPh)
4
]
+
and Br
-
anion possess intermolecular and intramolecular interactions, which stabilize the crystal structure. The characterization of the title compound were also carried out by using elemeutal analysis, FTIR, UV spectrometries and TG-DSC.
Studies on Manganese Peroxidase Immobilized in Gelatin-containing Microemulsion-based Gels
SONG Shao-fang, LUAN Yu-xia, SU Xiu-rong
2005, 21(4): 423-425.
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The immobilized technique of manganese peroxidase(MnP) in gelatin-containing microemulsion-based gels and the effects of storage time and reuse times on its catalytic activity were studied. The results show that the MnP immobilized together with Mn
2+
and H
2
O
2
could effectively oxidize syringaldazine in n-heptane. The immobilized MnP still had a high catalytic activity after one-month storage under a freezing condition. The reuse times have a relation to the amount of the immobilized H
2
O
2
. When the amount of the immobilized H
2
O
2
is sufficient, the microemulsion-based gels containing MnP could be used many times.
Determination of Proteins by Measuring Total Internal-reflected Resonance Light Scattering Signals on Water/Tetrachloromethane Interface with Evans Blue and Cetyltrimethylammonium Bromide
HUANG Cheng-zhi, FENG Ping, LI Yuan-fang, ZHAO Hua-wen
2005, 21(4): 426-430.
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A sensitive and selective assay of proteins is proposed based on measuring the total internal-reflected resonance light scattering(TIR-RLS) signals produced on the water/tetrachloromethane(H
2
O/CCl
4
) interface. In an aqueous medium with pH value in the range of 3.29-3.78, electrostatic attraction occurs between the negatively charged Evans Blue(EB) and positively charged proteins, forming hydrophobic ion associates and resulting in EB-protein adsorption on H
2
O/CCl
4
interface. The presence of cetyltrimethylammonium bromide prompts this adsorption, resulting in strongly enhanced TIR-RLS signals. The intensity of the enhanced TIR-RLS at 360-370 nm was found to be proportional to the concentration of proteins. For bovine serum albumin and human serum albumin, the linear range of detection is 0.07-1.2 μg/mL and the limits of detection are 6.68 and 6.30 ng/mL(3σ), respectively, while for lysozyme, the linear range of detection is 0.06-1.0 μg/mL and the limit of detection is 6.0 ng/mL(3σ). The content of the total albumin in a human urine sample could be directly determined by using the standard addition method with a percent recovery of 97.6%-104.1%, and the RSD ranging from 1.9% to 4.2%.
Electrochemical Behavior of Methanol Influenced by Polyaniline Incorporated with Ferrocenesulfonic-carboxylic Acid
NDAMANISHA Jean Chrysostome, WANG Hui, GUO Li-ping
2005, 21(4): 431-435.
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After the synthesis of polyaniline in the presence of ferrocenesulfoniccarboxylic acid, its influence on the electrochemical reaction of methanol was studied. The result indicates that the ferrocenyl in ferrocenesulfoniccarboxylic acid plays an important role in the electrocatalytic oxidation of methanol. CH
3
OH is adsorbed on PANI-Fc before its electrocatalytic oxidation. When the concentration of methanol is 2 mol/L, it begins to be oxidized. The effect of scan rate on the electrochemical reaction of methanol was also studied and 5 mV/s was favourable. It is another method to insert a metal catalyst in polyaniline without its electrodeposition.
Direct MALDI-MS Analysis of Proteins Isolated by Liquidphase Isoelectric Focusing Electrophoresis
LIU Ning, LÜ Lei, ZHANG Xuan, WANG Zhi, SUN Ya-dong, LIU Zhi-qiang, LIU Shu-ying
2005, 21(4): 436-438.
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A liquid-phase isoelectric focusing electrophoresis system(Rotofor) was used as the prefractionation tool for the sample preparation in the MALDI-MS analysis of a protein mixture. Each fraction collected was then directly subjected to MALDI-TOF-MS analysis. By this approach, we are able to resolve two types of hemoglobins, A and C, which cannot be successfully separated by means of the traditional SDS-PAGE method.
Synthesis and Characterization of Novel Sulfonylurea Derivatives
ZHANG Guang-liang, LI Yao-xian, ZHANG Suo-qin, GAO Fei-fei
2005, 21(4): 439-443.
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On the basis of study on the mechanism of action of sulfonylurea herbicides, nine sulfonylurea derivatives of iso-xazolidinone were designed and synthesized. The structures of these compounds were confirmed by means of IR, MS, NMR and elemental analysis. The results of preliminary active tests indicate that the compounds have some herbicidal activity. The structure-activity relationship was also studied.
Synthesis, Crystal Structure and Biological Activities of
N′
-(4-Methoxybenzylidene)-2-(1
H
-1,2,4-triazol-1-yl)acetohydrazide
XU Liang-zhong, LI Wei-hua, SI Guo-dong, ZHU Chong-yi, LI Kai, HOU Bao-rong
2005, 21(4): 444-446.
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The title compound, N′-(4-methoxybenzylidene)-2-(1 H -1,2,4-triazol-1-yl)acetohydrazide, was synthesized and its structure was confirmed by means of IR, MS, 1H NMR and elemental analysis. The single crystal structure of the title compound was determined by X-ray diffraction. The preliminary biological test shows that the synthesized compound has a low antifungal activity.
Syntheses of Nucleoside Derivatives Containing Fmoc- or Trityl-protected Amino Acids
GUO Hui, ZOU Wu-xin, JI Qi, MA Yu-xin, MENG Ji-ben
2005, 21(4): 447-451.
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Facile direct esterification reactions between 2′,3′-O-isopropylidene-nucleosides and Fmoc- or trityl-protected amino acids via N,N-dicyclohexyl-carbodiimide(DCC) mediated condensation are described. These reactions offer a mild and convenient method to synthesize aminoacylated nucleoside derivatives.
Mass Spectrometry of 2a,4-Disubstituted 5-Benzoyl-2a,3,4,5-tetrahydro-2-phenoxy-azeto[1,2-a][1,5]benzodiazepin-1(2
H
)-ones Under Electron Impact Ionization Conditions
XU Jia-xi, HUANG Xu
2005, 21(4): 452-456.
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The mass spectrometric fragmentation of 2a,4-disubstituted 5-benzoyl-2a,3,4,5-tetrahydro-2-phenoxy-azeto[1,2-a][1,5]benzodiazepin-1(2H)-ones has been investigated by means of mass-analyzed ion kinetic energy spectrometry under electron impact ionization conditions. All compounds tend to lose different moieties, such as phenoxy, phenoxy and H, and phenoxyketene. Both [M
+
-PhO] and [M
+
-PhOH] ions could further lose CO, and the [M
+
-PhOCH＝C＝O] ions could lose propene or styrene, PhCON, PhCOHN, and other fragments.
Syntheses of Novel Highly Symmetric Carbohydrates Bearing Diacylhydrazine Framework
YANG Bo, ZHANG Shu-sheng, LI Hui-xiang, LI Ji-zhi, JIAO Kui
2005, 21(4): 457-459.
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Several novel highly symmetric carbohydrates bearing a diacylhydrazine framework have been synthesized via a five-step procedure by utilizing D-glucose, D-galactose and D-xylose as the starting materials, respectively. The target compounds have been characterized with IR,
1
H NMR and elemental analysis.
Syntheses of Tetrahydropyrrolizino[2,1-c]quinoline Derivatives
SONG Hong-rui, WANG Fei, LI Jian, ZHANG Shou-fang
2005, 21(4): 460-462.
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The three title compounds were prepared from 2-phenylaminomethyl-3H-1,2-dihydro-1-pyrrolizinols via an intramolecular Friedel-Crafts reaction. 2-Phenylaminomethyl-3H-1,2-dihydro-1-pyrrolizinols were prepared from 2-phenylaminomethyl-3H-1,2-dihydro-1-pyrrolizinones via reduction. The heterocyclic ring system of pyrrolizino[2,1-c]quinoline has not been found in literature.
Trihydroxybenzoic Acid Dimer-induced Apoptosis Effects
in vitro
NIU Feng-lan, WANG Xue-dong, WANG Ying-li, SONG Lian-sheng
2005, 21(4): 463-467.
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The in vitro inhibitory effect of trihydroxybenzoic acid dimer(TAD) extracted from Trapabispinosd roxb on HeLa cell growth was investigated via the MTT[3-(4,5-dimethylthiazol-2-yl)-2,5-diophenyl-tetrazolium bromide] reduction method. The morphological changes of HeLa cells were observed by means of an optical microscope and a transmission electron microscope(TEM); the cell circles and apoptosis were detected by a flow cytometer. It was found that TAD can significantly inhibit the growth of Hela cells and can induce the apoptosis of HeLa cells. It was also found that the inhibition to the growth of Hela cells and the induction to the apoptosis of HeLa cells have a dosage-dependent feature. The inhibiting rates of TAD with mass concentrations of 25.000, 12.500 and 6.250 mg/L to the HeLa cell growth were 52.04%, 34.44% and 23.72% after 30 h, respectively, while those with TAD mass concentrations of 100.000, 50.000, 25.000, 12.500, 6.250 and 3.125 mg/L showed positive correlation with a correlation coefficient value of r=0.9859(P＜0.01) and a IC
50
value of 10.90 mg/L. Observed by means of TEM, the HeLa cells exposed to 25.000, 12.500 and 6.250 mg/L TAD showed apoptosis to various extents, shrinkage of the cell nuclei, condensation and margination of chromatin, and cavitation of mitochondrion. An apoptosis peak was detected via a flow cytometer. It can be drawn from the results that TAD extracted from Trapabispinosd roxb has an evident inhibitory effect on the proliferation of and an inductive effect on the apoptosis of HeLa cells, but has no obvious arrest action towards the cell circles of HeLa cells.
Purification of
Pseudomonas sp.
Lipase by Continuous Elution Electrophoresis Based on Pb
2+
Precipitation Method
ZHANG Hua-li, WANG Zhi, LIU Bin, WANG Xue-li, CAO Shu-gui, LI Zheng-qiang
2005, 21(4): 468-470.
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A Pb
2+
precipitation method was designed to get rid of the impure proteins in a lipase. The results show that it was a simple way in the primary treatment of the crude samples and about 20% impure proteins were removed in the precipitation step. Further, continuous elution electrophoresis was also applied as a preparative technique for attaining the highly pure lipase. During the continuous elution electrophoresis, the enzyme was eluted as a single peak and 5.7-fold purification was achieved in a yield of 54.3%. The two steps finally yielded an electrophoretically homogeneous enzyme.
Synthesis of Ni/Mg/Al Layered Double Hydroxides and Their Use as Catalyst Precursors in the Preparation of Carbon Nanotubes
ZHAO Yun, JIAO Qing-ze, LIANG Ji, LI Chun-hua
2005, 21(4): 471-475.
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Ni/Mg/Al layered double hydroxides(LDHs) with different n(Ni):n(Mg):n(Al) ratio values were prepared via a coprecipitation reaction. Then Ni/Mg/Al mixed oxides were obtained by calcination of these LDHs precursors. Carbon nanotubes were produced in the catalytic decomposition of propane over the Ni/Mg/Al mixed oxide catalysts. The quality of as-made nanotubes was investigated by SEM and TEM. The nanotubes were multiwall with a high length-diameter ratio and appeared to be flexible. The catalytic activities of these mixed oxides increased with increasing the Ni content. The Ni/Mg/Al mixed oxide with the highest Ni content [n(Ni)/n(Mg)/n(Al)=1/1/1] showed the highest activity and the carbon nanotubes grown on its surface had the best quality.
Optically Active Chiral Auxiliary Benzyloxyphenylglycinol for Preparation of Oxazolidine and Its Derivatives
FU Ying-huan, CHEN Jin, WU Tong-hao, BAI Xu
2005, 21(4): 476-479.
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To investigate the recovery of amino alcohols as chiral auxiliaries, optically active p-benzyloxyphenylglycinol and its corresponding oxazolidine of 1-naphthylcarboxaldehyde were prepared. Grignard additions to the oxazolidine followed by electrophilic quench and acidic hydrolysis afforded an aldehyde(compound 8)(later it was reduced to an alcohol, compound 9) in an excellent enantiomeric excess and a good recovery of the chiral amino alcohol. This research provides a model study of chiral amino alcohols in solid phase asymmetric synthesis.
A Novel Photocleaver with Long Wavelength Absorption-Highly Efficient Antitumor Agent:4-(2-Diethylamino-ethylamino)-8-oxo-8
H
-acenaphtho-[1,2-b]pyrrole-9-carbonitrile
ZHANG Zhi-chao, LÜ Zhe, QIAN Xu-hong, LIU Feng-yu, SHENG Hui
2005, 21(4): 480-483.
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The photocleavage abilities of a novel family of compounds, 8-oxo-8 H -acenaphtho[1,2-b] pyrrole-9-carbonitrile and its derivatives(compounds 1-5) were evaluated with M13 mp18 single strand circular DNA. Only compound 1 with a diethylamine group could bind to DNA via electrostatic attraction and intercalation. At a concentration of 50 μmol/L, it could generate singlet oxygen to cleave circular DNA into linear DNA under the irradiation of long wavelength light(λ>400 nm). The antitumor ability of compound 1 was also evaluated in vitro, and its IC
50
on HeLa cells was as low as 6.8 μmol/L.
Studies on the Self-condensing Vinyl Polymerization of a Novel Maleimide Inimer
REN Qiang, JIANG Bi-biao, ZHANG Dong-liang, YU Qiang, FANG Jian-bo, YANG Yang, CHEN Jian-hai
2005, 21(4): 484-488.
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The self-condensing vinyl polymerization(SCVP) of a novel maleimide inimer(initiator-monomer) 1, N-(4-α-bromobutyryloxy phenyl) maleimide with the complex of CuBr/Bipy(2, 2′-bipyridine) as the catalyst was studied. GPC was used to determine the molecular weight and the results show that the molecular weight increases exponentially with polymerization time during the first hour, and then the rate of increase molecular weight slows down. The molecular weight also increases with increasing dosage of the catalyst. The coincidence of the molecular weights determined by
1
H NMR and GPC proves that the polymer obtained from the SCVP of inimer 1 has a linear structure, which is further verified by
13
C NMR spectrum. A hyperbranched polymer was obtained by the copolymerization of inimer 1 and styrene.
Raman Scattering of Nanocrystalline δ-TiN
x
Synthesized by Mechanical Milling
DING Zhan-hui, YAO Bin, MA Hong-an, JIA Xiao-peng, QIU Li-xia, SU Wen-hui
2005, 21(4): 489-491.
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Intercalation of PM-19 into and in vitro Release of Anti-tumor Drug from Layered Double Hydroxide
WANG Zhong-liang, WANG En-bo, TIAN Shang-yi, XIAO Dong-rong, GAO Lei, WANG Li, XU Lin
2005, 21(4): 492-495.
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Syntheses, Characterization and Crystal Structures of New Nickel Complexes with 2,6-Bis(imino)pyridyl Ligands
FAN Rui-qing, ZHU Dong-sheng, MU Ying, LI Guang-hua, SU Qing, NI Jian-guo, FENG Shou-hua
2005, 21(4): 496-500.
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Non-isothermal Kinetics of the First-stage Decomposition Reaction of Cobalt Oxalate Dihydrate
ZHANG Jian-jun, REN Ning, BAI Ji-hai
2005, 21(4): 501-504.
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A Facile Route to Rapid Synthesis of Soluble Monodisperse Oligo(1,4-phenyleneethynylene)s
LI Guo-rong, WANG Xian-hong, LI Ji, ZHAO Xiao-jiang, WANG Fo-song
2005, 21(4): 505-507.
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