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Table of Content
25 May 2012, Volume 28 Issue 3
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Content
Cover and Content of Chemical Research in Chinese Universities Vol.28 No.3(2012)
2012, 28(3): 0-0.
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Letters
Synthesis of Silica Hollow Spheres with Diameter Around 50 nm by Anionic Surfactant
RAN Hua, HAN Lu, CHE Shun-ai
2012, 28(3): 361-363.
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Silica hollow spheres(SHSs) have attracted great attention because of their low toxicity, low density, large surface area, high chemical and thermal stability, and surface permeability. They can be widely applied in storage
[1]
, catalysis
[2]
, drug delivery
[3,4]
, low-dielectric-constant materials
[5]
, low-refractive materials
[6-8]
, and so on. Up to now, there have been various methods to produce SHSs. Inorganic
[9]
or organic particles
[10]
, such as polystyrene or calcium carbonate, were used as hard templates to create hollow cavities. However, the multistep synthetic process and the lack of structural robustness of the shells upon template removal process weaken their application. Soft templates, including oil-in-water emulsions
[11,12]
, vesicles
[13]
, micelle
[14,15]
and gas bubbles
[16]
, are applied widely.
Microwave Accelerated Synthesis of 2,2′,3,3′-Biphenyltetracarboxylic Dianhydride
HUANG Yuan-yuan, SHAO Tao, MEN Jian, GAO Guo-wei
2012, 28(3): 364-365.
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Polyimides have been widely used in aerospace and microelectronics due to their excellent mechanical properties and thermo oxidative stability
[1]
. However, most of aromatic polyimides are severe difficult to process because of their bad solubility in common solvents and intractable in their fully imidized forms, which restrict their applications and developments
[2,3]
. Therefore, many investigations were focused on improving the dissolvability of polyimides and it was found that the excellent solubilizing units could be obtained from substituted biphenyls
[4-7]
. Biphenyltetracarboxylic dianhydrides(BPDAs) are the most important monomers for the synthesis of these compounds. Among them, the synthesis of 2,3,3′,4′-/3,3′,4,4′- biphenyltetracarboxylic dianhydride has been widely investigated, but only a few literatures reported the synthesis of 2,2′,3,3′-biphenyltetracarboxylic dianhydride(
em
-BPDA)
[8-10]
.
Articles
Hydrothermal Synthesis of H
3
PW
12
O
40
/TiO
2
Nanometer Photocatalyst and Its Catalytic Performance for Methyl Orange
FENG Chang-gen, SHANG Hai-ru
2012, 28(3): 366-370.
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H
3
PW
12
O
40
/TiO
2
nanometer photocatalyst was prepared by one step hydrothermal synthesis from H
3
PW
12
O
40
·
n
H
2
O and Ti(OBu)
4
, simultaneously realizing the load and modification of H
3
PW
12
O
40
. The catalyst was characterized by Fourier transform infrared spectroscopy(FTIR), powder X-ray diffraction(XRD), nitrogen adsorption-desorption analysis and scanning electron microscopy(SEM). The results show that the catalyst is Keggin structure and crystallized in anatase structure, the diameter and specific area of the prepared catalyst are 3.8 nm and 177.9 m
2
/g, respectively, and its dispersity is better. The photocatalytic properties were compared for TiO
2
, H
3
PW
12
O
40
/TiO
2
prepared by impregnation and H
3
PW
12
O
40
/TiO
2
prepared by hydrothermal method with methyl orange as a probe. The effects of H
3
PW
12
O
40
loadings, crystallization method, initial pH and concentration of dye solution on the degradation of methyl orange were investigated.
Hydrothermal Synthesis, Structure Characterization and Magnetic Studies of Perovskite-type Fluorides K
2
NaVF
6
and (NH
4
)
3
VF
6
HE Li-jie, ZHANG Dong, FENG Shou-hua, CHEN Gang, ZOU Bo
2012, 28(3): 371-374.
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Two perovskite-type fluorides K
2
NaVF
6
and (NH
4
)
3
VF
6
were synthesized under mild hydrothermal conditions. The structures of the compounds were determined by means of powder X-ray diffraction analysis. The Rietveld refinement indicates that K
2
NaVF
6
has a cubic elpasolite-type structure and crystallizes in space group Fm3m with lattice constant a=8.3180(2) nm. (NH
4
)
3
VF
6
has a cubic cryolite-type structure and crystallizes in space group Fm3m with lattice parameter a=9.090(1) nm. The compounds were further characterized by scanning electron microscopy( SEM), thermogravimetric(TG) and differential thermal analysis(DTA). The variable temperature magnetic susceptibility of these two compounds was characterized for the first time and the result shows that the magnetic ordering is related to the crystallographic features and isolated magnetic unit with the temperature decreasing.
Novel Chiral Polyoxometalate: First Arginine Based Anderson-type Complex
LIN Shi-wei, WU Qiong, WANG En-bo
2012, 28(3): 375-378.
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A novel chiral polyoxometalate(POM), {[Na(Arg)
2
]NaH}[AlMo
6
(OH)
6
O
18
]·6H
2
O(1, Arg=
L
-arginine) has been synthesized by the reaction between Na
3
[AlMo
6
(OH)
6
O
18
]·8H
2
O and Arg in aqueous solution and was structurally characterized by single-crystal X-ray diffraction, elemental analyses and UV-Vis spectrometry. Compound 1 was an example of Arg based Anderson-type complex. Photocatalytic analysis indicates that compound 1 presents catalytic activity for photodegradation of rhodamine-B(RhB) under UV irradiation.
Thin Film of Perovskite Oxide with Atomic Scale p-n Junctions
HU Bin, HUANG Ke-ke, HOU Chang-min, YUAN Hong-ming, PANG Guang-sheng, FENG Shou-hua
2012, 28(3): 379-381.
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Thin films of perovskite manganese oxide La
0.66
Ca
0.29
K
0.05
MnO
3
(LCKMO) on Au/ITO(ITO=indium tin oxide) substrates were prepared by off-axis radio frequency magnetron sputtering and characterized by X-ray diffraction( XRD), high-resolution transmission electron microscopy(HRTEM), and conductive atomic force microscopy (C-AFM) at room temperature. The thin films with thickness ranged from 100 nm to 300 nm basically show cubic structures with a=0.3886 nm, the same as that of the raw material used, but the structures are highly modulated. C-AFM results revealed that the atomic scale p-n junction feature of the thin films was the same as that of the single crystals. The preparation of the thin films thus further confirms the possibility of their application extending from micrometer-sized single crystals to macroscopic thin film.
New Supramolecular Networks Based on Paratungstate with N-Donor Bridging Ligands
YAO Wei, WANG Xin, XIE Hong-wei, MA Rui-ying, YU Yang, LI Yang-guang
2012, 28(3): 382-386.
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Three new supramolecular networks based on paratungstate and N-donor bridging ligands, [H
2
bpmp]
2.5
H[H
2
W
12
O
40
]2H
2
O(1), [H
2
(bpp)]
2
[H(py―CH
3
)]
0.25
[H(py―C
2
H
5
)]
0.25
H
1.5
[H
2
W
12
O
40
]·4H
2
O(2) and [H
2
pip]
3
[H
2
W
12
O
40
](3)[bpmp=
N
,
N
'-bis(4-pyridylmethyl)piperazine; bpp=1,3-bis(4-pyridyl)propane; py=pyridine; pip=piperazine] were prepared by the hydrothermal synthesis and characterized by elemental analysis, infrared(IR), thermogravimetric(TG) analysis and single-crystal X-ray diffraction(XRD). All the compounds show high-dimen- sional supramolecular networks based on [H
2
W
12
O
40
]
6-
and the protonated N-donor ligands
via
the N―H···O―W hydrogen bonds and/or
π
···
π
stacking interactions. Their luminescent properties were investigated.
Multi-step Reaction Route Developed for Improving Crystallinity of Boron Nitride Nanoparticles
TAN Miao, LIAN Gang, ZHANG Xiao, ZHANG Shun-jie, CUI De-liang, WANG Qi-long
2012, 28(3): 387-390.
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A multi-step reaction route was developed to synthesize boron nitride(BN) nanoparticles via the reaction between NaN
3
and BCl
3
in a benzene-thermal solution. By means of this route, the crystallinity of BN nanoparticles was improved
via
increasing the reaction steps. Meanwhile, a phase transformation from hexagonal BN(hBN) or turbostratic BN(tBN) to cubic BN(cBN) occurred, resulting in the increase of cBN content. Moreover, the content of cBN also slightly increased when the temperature was elevated from 265 ℃ to 280 ℃.
Synthesis and Ferrimagnetic Behaviour of Mn Doped Rare Earth Iron Garnets
GUO Li, YUAN Lin, PENG Wen, YUAN Hong-ming, FENG Shou-hua
2012, 28(3): 391-394.
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Rare earth iron garnets R
3
Fe
5–
x
Mn
x
O
12
(R=Pr, Nd, Sm, Eu) were prepared through mild hydrothermal method. The initial alkalinity of solutions was thought to play an important role in governing the content of Mn. The effect of substitution Fe
3+
ions by Mn
3+
ions on magnetic properties was investigated. The saturation magnetizations of Mn-doped samples are larger than that of corresponding parent compounds due to the moment of Mn
3+
ion being smaller than that of Fe
3+
. It is clearly shown that incorporation of Mn
3+
gives rise to significant variations in the Curie temperature. With increasing of Mn content
x
, Curie temperatures reduced sharply for the garnets, which could be explained by the exchange interaction between a-d Fe
3+
being reduced in these compounds.
L-Cysteine-assisted Synthesis of Copper Gallium Sulfide Microspheres
LIANG Xiao-juan, ZHONG Jia-song, CAI Qian, HUANG Hai-yu, LIU Hai-tao, XIANG Wei-dong, SUN Jun-cai
2012, 28(3): 395-398.
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An effective
L
-cysteine-assisted synthetic route has been successfully developed to prepare copper gallium sulfide(CuGaS
2
) microspheres under solvothermal conditions with CuCl
2
·2H
2
O, GaCl
3
and
L
-cysteine as source materials, in which
L
-cysteine was used as the sulfide source and complexing molecule. The experiments revealed that the synthesized sample was of a typical CuGaS
2
tetragonal structure. Moreover, the prepared CuGaS
2
crystals consisting of microspheres made up of nanoflakes, and the diameter of the nanoflakes was about 20 nm. Raman spectrum of the obtained CuGaS2 exhibits a high-intensity peak of the
A
1
mode at 306 cm
-1
. Meanwhile, a possible growth mechanism was proposed based on the investigations.
Liquid Chromatography-electrospray Ionization Tandem Mass Spectrometry for Simultaneous Determination of Metformin and Glimepiride in Beagle Dog Plasma and Bioequivalence Study
BAI Jing, SHI Xiao-wei, DU Ying-feng, XIANG Bai, WANG Shuai, CAO De-ying
2012, 28(3): 399-405.
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A sensitive and selective liquid chromatography-electrospray ionization tandem mass spectrometry(LCESI- MS/MS) was used for the simultaneous determination of metformin and glimepiride in beagle dog plasma with glipizide as internal standard(IS). After simplified protein precipitation with methanol, both the analytes and IS were chromatographed on a Zorbax CN column via gradient elution with methanol(containing 5 mmol/L ammonium acetate) and 5 mmol/L aqueous ammonium acetate as the mobile phase. Detection was performed by multiple reaction monitoring(MRM) scanning via ESI source operated in positive ionization mode. Specificity, linearity, accuracy, precision, recovery, matrix effect and stability were validated for metformin and glimepiride in beagle dog plasma. The calibration curves were linear in a concentration range of 10―10000 ng/mL for metformin and 4―4000 ng/mL for glimepiride with both correlation coefficients higher than 0.99. The recoveries obtained for the analytes and IS were all between 82.7% and 101.2%. The method exhibited excellent performance in terms of selectivity, robustness, short analytical time and simplicity of sample preparation. Finally, the proposed method was applied to a bioequivalence study of self-made bilayer tablet and commercial formulation containing 500 mg of metformin and 1 mg of glimepiride in beagle dogs.
Purification of Astaxanthin from
Laminaria japonica
by Ionic Liquid-based Monolithic Cartridge
YOON Chang-hwan, ZHU Tao, ROW Kyung-ho
2012, 28(3): 406-409.
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An effective and accurate method was developed for the extraction of astaxanthin from
Laminaria japonica
with subsequent separation by ionic liquid-based monolithic cartridge. The optimized extraction conditions including extraction solvent(ethanol), extraction time(90 min) and ultrasonic power(75 W) were obtained by systematical investigation. Chromatographic analysis was performed on a C
18
column with ultraviolet(UV) detection at 476 nm, and a solution consisting of methanol/acetonitrile/H
2
O/dichloromethane(83:6:6:5, volume ratio) was used as the mobile phase at a flow rate of 0.7 mL/min. After ionic liquid-based monolithic solid phase extraction, 17.82 μg/g astaxanthin was obtained from
Laminaria japonica
. This ionic liquid-based monolithic cartridge exhibits high affinity and selectivity for astaxanthin, and it can be potentially used as the stationary phase of high performance liquid chromatography(HPLC).
Development and Characterization of an Electrochemical Sensor for Cinchonidine Detection Based on Molecularly Imprinted Polymer with Modified Rosin as Cross-linker
LIU Li, TAN Xue-cai, ZHAO Dan-dan, WANG Lin, LEI Fu-hou, HUANG Zai-yin
2012, 28(3): 410-414.
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Molecularly imprinted polymers(MIPs) were applied as molecular recognition elements to an electrochemical sensor for cinchonidine(CD). A kind of MIP was synthesized with cinchonidine as template, modified rosin( ethylene glycol maleic rosinate acrylate) containing the skeleton of phenanthrene rings as cross-linker and methylacrylic acid as functional monomer. MIP membrane was prepared on a glassy carbon electrode for the determination of CD
via
free radical polymerization method. Electrochemical impedance spectroscopy(EIS) and cyclic voltammetry( CV) were used to characterize the membrane electrochemical behavior in electrode fabrication process. The experimental conditions were discussed. Under optimum conditions, it was found that the response of peak currents was linear to the concentration of CD in a range of 0.013―2.26 mmol/L. The detection limit for CD is 1 μmol/L, the relative standard deviation for 100 μmol/L CD is 1.34% and the incubation time is 2 min. The sensor was applied to the determination of CD in urine samples with satisfactory results.
Determination of Nicotine in Tobacco by Capillary Electrophoresis with Electrochemical Detection
SUN Jin-ying, XU Xiao-yu, YU Huan, YOU Tian-yan
2012, 28(3): 415-418.
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A sensitive, simple and low-cost method based on capillary electrophoresis(CE) with electrochemical(EC) detection at a carbon fiber microdisk electrode(CFE) was developed for the determination of nicotine. Effects of detection potential, concentration and pH value of the phosphate buffer, and injection time as well as separation voltage were investigated. Under the optimized conditions: a detection potential of 1.20 V, 40 mmol/L phosphate buffer(pH 2.0), a sample injection time of 10 s at 10 kV and a separation voltage of 16 kV, the linear range obtained was from 5.0×10
-7
mol/L to 1.0×10
-4
mol/L with a correlation coefficient of 0.9989 and the limit of detection(LOD, S/N=3) obtained was 5.0×10
-8
mol/L. The method was also used to determine the nicotine in cigarettes. Nicotine amount ranged from 0.211 mg/g to 0.583 mg/g in the pipe tobacco of seven brands of cigarette and the amount in one cigarette varied from 0.136 mg/cigarette to 0.428 mg/cigarette.
Elution of 17α 25-Norhopanes and Triaromatic Steroids from Weathered Soils by Mixed Triton X-100/Na
2
SiO
3
Surfactant Solution
JI Guo-dong, ZHOU Guo-hui
2012, 28(3): 419-423.
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Sodium silicate(Na
2
SiO
3
) was used to improve the elution of super heavy oil from weathered soil on an ultrasound-enhanced elution system by the solution containing 0―6000 mg/L surfactant Triton X-100. The removal extent of three markers[C
26―34
17
α
25-norhopanes, C
26―28
triaromatic steroids(TAS), and C
27―29
methyl triaromatic steroids(MTAS)] was monitored. The average elution percentages of C
26―34
norhopanes, C
26―28
TAS, and C
27―29
MTAS by Triton X-100/Na
2
SiO
3
solutions were increased by 11%―13%, 9%―11% and 8%―13% with increasing Triton X-100 concentrations from 150 mg/L to 6000 mg/L. All the concentrations of Triton X-100 improved the elution of TAS homologs containing fewer carbon atoms, whereas high concentrations improved the elution of larger 17
α
25-norhopane and MTAS species. Addition of Na
2
SiO
3
produced a noticeable increase in elution, particularly for lower-weight species. Scanning electron microscope(SEM) images and energy spectroscopy data reveal that surfactant solution of 6000 mg/L Triton X-100 and 4000 mg/L
Na
2
SiO
3
produced the greatest improvement in the elution of super heavy oil aggregates encapsulating the soil surface and the emulsification of particle dispersions. That is to say mixed solutions of Triton X-100 and Na
2
SiO
3
in combination with ultrasound are a potential means of removing super heavy oil from weathered soils.
Synthesis and Antibacterial Activities of 1,4-Disubstituted Phenyl-5-(halo-2-hydroxyphenyl)imino-1,2,3-triazole
ZHAO Xu, LU Jun-rui, XIN Chun-wei, LU Bo-wei, BAO Xiu-rong, LI Jian-fa, LIU Ya, YANG Xu-yun, YUAN Yi
2012, 28(3): 424-429.
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According to the superposition principle of reinforcement of biological activities, 24 novel 1,4- disubstituted phenyl-5-(halo-2-hydroxyphenyl)imino-1,2,3-triazoles was synthesized and characterized by 1H NMR,
13
C NMR, elemental analysis and IR. All the target compounds were screened for their antibacterial potential
in vitro
against
Monilia albican, Escherichia coli
and
Staphylococcus aureus
. It was shown that all the compounds possessed efficient antibacterial activities at a concentration of 0.1 mg/mL, even at a concentration of 0.01 mg/mL, some of the compounds still exhibited antibacterial activities against
Escherichia coli
and
Monilia albican
. At last, the structure- activity relationship was discussed based on the antibacterial results.
Design, Synthesis and Insecticidal Activities of Novel Phenyl Substituted Isoxazolecarboxamides
LIU Peng-fei, ZHANG Ji-feng, YAN Tao, XIONG Li-xia, LI Zheng-ming
2012, 28(3): 430-433.
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Thirteen novel phenyl substituted isoxazolecarboxamides were synthesized, and their structures were characterized by
1
H NMR, elementary analysis and high-resolution mass spectrometry(HRMS) techniques. Their evaluated insecticidal activities against oriental armyworm(
Mythimna separata
) indicate that the phenyl substituted isoxazolecarboxamides exhibited moderate insecticidal activities, among which compounds 9c and 9k showed comparatively higher activities.
Promising Ultraviolet Absorbers—Novel Guanine Analogs Having Significantly Improved Ultraviolet Absorption Capacity and Dissipating the Energy of Absorbed Photons by Nonradiative Decay Mechanism
HAN Song-zhe, WU Yu-ting, ZHANG Meng, JIAO Jia-jun
2012, 28(3): 434-437.
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Structural properties of nucleobase underlie their ultrafast excited-state dynamics and low fluorescence quantum yields, which cause effectively nonradiative decay process and render them like sunscreens. Thus, eight guanine analogs[
N
-2-(2'-nitrobenzoyl)-guanine,
N
-2-(3'-nitrobenzoyl)-guanine,
N
-2-(4'-nitrobenzoyl)-guanine,
N
-2-(2'-hydroxybenzoyl)-guanine,
N
-2-(4'-methoxylbenzoyl)-guanine,
N
-2-(4'-chloricbenzoyl)-guanine,
N
-2-(4'- methylicbenzoyl)- guanine and
N
-2-(3',5'-dinitrobenzoyl)-guanine] with different substituted benzoyls, except
N
-2-(4'-chloricbenzoyl)-guanine, were newly synthesized. In contrast with guanine, they exhibit wider ultraviolet absorbent range, higher molar extinction coefficient and lower fluorescence intensity.
Synthesis and Anti-VSMC Vegetation Activities of New Aurone Derivatives
FAN Rui, BAN Shu-rong, FENG Xiu-e, ZHAO Chen-xiao, LI Qing-shan
2012, 28(3): 438-442.
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A series of new aurone derivatives was prepared by means of a practical route and their anti-vascular smooth muscle cells(VSMC) vegetation activities were evaluated by the 3-(4,5-dimethylthlazol-2-yl)-2,5- diphenyltetrazolium bromide(MTT) method with tetrandrine as a positive contrast drug. The structures of the compounds were confirmed by
1
H NMR,
13
C NMR and electrospray ionization mass spectrometry(ESI-MS). Several new compounds exhibited promising activity against VSMC proliferation and the preliminary structure-activity relationships( SAR) were discussed in order to investigate the essential structures required for their bioactivities.
Enrichment of Fetal Nucleated Red Blood Cells by Multi-core Magnetic Composite Particles for Non-invasive Prenatal Diagnosis
PAN Ying, WANG Qing, HUANG Wen-jun, QIAO Feng-li, LIU Yu-ping, ZHANG Yu-cheng, HAI De-yang, DU Ying-ting, WANG Wen-yue, ZHANG Ai-chen
2012, 28(3): 443-448.
Abstract
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)
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A novel kind of multi-core magnetic composite particles, the surfaces of which were respectively modified with goat-anti-mouse IgG and antitransferrin receptor(anti-CD71), was prepared. The fetal nucleated red blood cells(FNRBCs) in the peripheral blood of a gravida were rapidly and effectively enriched and separated by the modified multi-core magnetic composite particles in an external magnetic field. The obtained FNRBCs were used for the identification of the fetal sex by means of fluorescence
in situ
hybridization(FISH) technique. The results demonstrate that the multi-core magnetic composite particles meet the requirements for the enrichment and speration of FNRBCs with a low concentration and the accuracy of detetion for the diagnosis of fetal sex reached to 95%. Moreover, the obtained FNRBCs were applied to the non-invasive diagnosis of Down syndrome and chromosome 3p21 was detected. The above facts indicate that the novel multi-core magnetic composite particles-based method is simple, reliable and cost-effective and has opened up vast vistas for the potential application in clinic non-invasive prenatal diagnosis.
Antitumor Active Protein-containing Glycans from the Body of
Ganoderma tsugae
LIU Ying, LI Yue-fei, ZHENG Ke-yan, FEI Xiao-fang
2012, 28(3): 449-453.
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)
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To explore the effects of traditional herbal medicine
Ganoderma tsugae
(
G. tsugae
) on immunomodulatory and antitumor activities, the crude polysaccharides of
G. tsugae
were purified by filtration, diethylaminoethyl(DEAE) sepharose-fast flow chromatography and sephadex G-100 size-exclusion chromatography. Two main fractions, protein- containing glycans CSSLP-1 and CSSLP-2, were obtained via the gradient elution. The protein content, molecular weight, and monosaccharide composition of the two fractions were analyzed. Furthermore, the influence of the protein-containing glycans from
G. tsugae
on the activation of human acute monocytic leukemia cell line(THP-1) and their antitumor activities to the human hepatocellular liver carcinoma cell(HepG-2)
in vitro
were evaluated. The results indicate that CSSLP-1 and CSSLP-2 could increase the pinocytic activity of THP-1 cells and induce THP-1 cells to produce the cytokines of TNFα and IL-2, significantly. CSSLP-1 and CSSLP-2 also played an inhibiting effect on the cancer cell(HepG-2). Moreover, the anti-proliferation activity of CSSLP-1 and CSSLP-2 increased with the participation of TNFα and IL-2 or other antitumor factors induced from THP-1 cells by
G. tsugae
protein-containing glycan fractions.
Antioxidant Effect of Selenium-containing Glutathione S-Transferase in Rat Cardiomyocytes
YIN Li, HAN Xiao, YU Yang, GUO Xiao, REN Li-qun, FANG Jing-qi, LIU Zhi-yi, YAN Gang-lin, WEI Jing-yan
2012, 28(3): 454-458.
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As one of the most important antioxidant enzymes, glutathione peroxidase(GPX) protects cells and tissues from oxidative damage, and plays an important role in cardiovascular and cerebrovascular injuries induced by oxidative stress. The antioxidant effect of selenium-containing glutathione S-transferase(Se-GST), a mimic of GPX was investigated on rat cardiomyocytes. To explore the protection function of Se-GST in hydrogen peroxide(H
2
O
2
) challenged rat cardiomyocytes, we examined malondialdehyde(MDA), lactate dehydrogenase(LDH), superoxide dismutase( SOD) and cell apoptosis. The results demonstrate exposure of rat cardiomyocytes to H
2
O
2
for 6 and 12 h induced the significant increases of MDA, LDH and apoptosis rate of cardiomyocytes, but pretreatment of rat cardiomyocytes with Se-GST at 0.0005 or 0.001 unit/mL prevents oxidative stress induced by H
2
O
2
with the decreases of cell apoptosis. All the results hint Se-GST has antioxidant activity for oxidative stress challenged rat cardiomyocytes.
Purification and Properties of an Extracellular Polyhydroxybutyrate Depolymerase from
Pseudomonas mendocina
DSWY0601
WANG Yan, LI Fan, WANG Zhan-yong, LIU Dong-bo, XIA Hong-mei, LIU Ling-fei, CHEN Shan
2012, 28(3): 459-464.
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An extracellular polyhydroxybutyrate(PHB) depolymerase was purified to homogeneity from the culture supernatant of a PHB-degrading bacterium,
Pseudomonas mendocina
DSWY0601, which was isolated from brewery sewage for the ability to form clear zones on the PHB mineral agar plates. The molecular weight of the purified PHB depolymerase as determined by sodium dodecyl sulfate-polyacrylamide gel electrophoresis(SDS-PAGE) was approximately 59800 at the optimal temperature and pH value being 50 ℃ and 8.5, respectively. PHB depolymerase was stable in a temperature range of 20―50 ℃ and sensitive to pH value within a pH range of 8.0―9.5. PHB depolymerase degraded poly-3-hydroxybutyrate-co-4-hydroxybutyrate(P3/4HB) and poly-3-hydroxybutyrate-co-3- hydroxyvalerate(PHBV) but did not degrade poly(lactic acid)(PLA), poly(butylene succinate)(PBS) or poly- (caprolactone)(PCL). PHB depolymerase was sensitive to phenylmethylsulfonyl fluoride(PMSF), H
2
O
2
and SDS. The main product after enzymatic degradation of PHB was indentified as 3-hydroxbutyrate monomer(3HB) by mass spectrometric analysis, suggesting that PHB depolymerase acted as an exo-type hydrolase. Analysis of
phaZ
pm
gene reveals that PHB depolymerase is a typical denatured short-chain-length PHA(dPHA
SCL
, PHA=polyhydroxyalkanoate) depolymerase containing catalytic domain, linker and substrate-binding domain.
Inhibition of Dual Specific Oncolytic Adenovirus on Esophageal Cancer
via
Activation of Caspases by a Mitochondrial-dependent Pathway
SU Jia-qiang, CHI Bao-rong, LI Xiao, LIU Lei, LIU Li-ming, QI Yan-xin, WANG Zhuo-yue, JIN Ning-yi
2012, 28(3): 465-471.
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We investigated the anti-tumor effects of dual cancer specific-oncolytic adenovirus Ad-VP on esophageal cancer(EC). The anti-tumor activity of Ad-VP was compared with that of the control recombinant adenoviruses (Ad-GP, Ad-Apoptin, Ad-EGFP) in human esophageal cancer cell EC-109 and human normal liver cell L02
in vitro
. In 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide(MTT) assays, the growth of EC-109 cells was slightly inhibited by Ad-GP, Ad-Apoptin and Ad-EGFP. However, Ad-VP induced a significant cytotoxic effect. Infection of EC-109 cells with Ad-VP resulted in a significant induction of apoptosis of them
in vitro
, detected by 4′,6-diamidino-2-phenylindole(DAPI) or acridine orange and ethidium bromide staining. The results of Western blot and flow cytometric assay indicate the loss of mitochondrial membrane potential(ΔΨ
m
), the release of cytochrome c and the activation of caspase-3, 6 and 7 in Ad-VP infected EC-109 cells. In contrast, all these assays show almost no effects of the recombinant adenoviruses on L02 cells. These results demonstrate that the treatment of tumors with Ad-VP selectively inhibits tumor growth and induces apoptosis of esophageal cancer cells. Ad-VP may provide a novel and powerful strategy for cancer gene therapy.
Wound Healing Assay Using Microfluidic Channels
XI Yan-li, WANG Shu-tao, SU Bin, HA Qing, NIU Feng-lan, NIE Fu-qiang
2012, 28(3): 472-476.
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An approach was described to produce a wound area
in vitro
using laminar flow technique to selectively remove cells in microfluidic channels. Cell migration which plays an important role in the process of wound healing can be observed dynamically by this method. In order to prove our system, we have studied its properties by injecting NIH-3T3 cells into main channel and added several reagents to observe the mediatory influence. The results reveal that fibroblast growth factor-2(FGF-2), insulin-like growth factor 1(IGF-I), platelet-derived growth factor BB(PDGF-BB) and ascorbic acid(Vc) groups can promote cell migration compared with the control group. But the average migration distance was diminished in dexamethasone group. It can be concluded that this system can be used to analyze the process of wound healing.
Biochemical Characterization of Uracil-DNA Glycosylase from
Pyrococcus furiosus
LIN Li-bo, LIU Yu-fen, LIU Xi-peng, LIU Jian-hua
2012, 28(3): 477-482.
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We report the characterization of a uracil-DNA glycosylase(UDG) from the hyperthermophilic archaea
Pyrococcus furiosus
(
P. furiosus
).
P. furiosus
UDG(PfUDG) has high sequence similarity to the families IV and V UDGs(thermostable UDG family and PaUDG-b family). PfUDG excises uracil from various DNA substrates with the following order: U/T≈U/C>U/G≈U/AP≈U/->U/U≈U/I≈U/A. The optimal temperature and pH value for uracil excision by PfUDG are 70 ℃ and 9.0, respectively. The removal of U is inhibited by the divalent ions of Fe, Ca, Zn, Cu, Co, Ni and Mn, as well as a high concentration of NaCl. The phosphorothioates near uracil strongly inhibit the excision of uracil by PfUDG. Interestingly, pfuDNA(
Pyrococcus furiosus
DNA) polymerase, which tightly binds the uracil- carrying oligonucleotide, does not inhibit the excision by PfUDG, suggesting PfUDG in vivo functions as the repair enzyme to excise uracil damage in genome.
UV-Enhanced Room Temperature Ozone Sensor Based on Hierarchical SnO
2
-In
2
O
3
SUN Jian-bo, XU Jing, WANG Biao, SUN Peng, LIU Feng-min, LU Ge-yu
2012, 28(3): 483-487.
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SnO
2
-In
2
O
3
hierarchical microspheres were prepared by the hydrothermal and solvothermal method. The morphology, phase crystallinity of the obtained SnO
2
-In
2
O
3
were measured by X-ray diffraction(XRD), scan electron microscopy(SEM), respectively. A room temperature ozone sensor based on SnO
2
-In
2
O
3
hierarchical microspheres was fabricated and investigated. The gas sensing properties of the sensor using SnO
2
-In
2
O
3
strongly depended on the proportion of SnO
2
and In
2
O
3
. The sensitivity and response/recovery speed were greatly enhanced by UV illumination. A gas sensing mechanism related to oxygen defect was suggested.
Comparison of Surface-enhanced Raman Scattering Spectra of Two Kinds of Silver Nanoplate Films
TAO Jin-long, TANG Bin, XU Shu-ping, PAN Ling-yun, XU Wei-qing
2012, 28(3): 488-492.
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Surface-enhanced Raman scattering(SERS) spectra of different silver nanoplate self-assembled films at different excitation wavelengths were fairly compared. Shape conversion from silver nanoprisms to nanodisks on slides was
in situ
carried out. The SERS spectra of 4-mercaptopyridine(4-MPY) on these anisotropic silver nanoparticle self-assembled films present that strong enhancement appeared when the excitation line and the surface plasmon resonance(SPR) band of silver substrate overlapped. In this model, the influence of the crystal planes of silver nanoplates on SERS enhancement could be ignored because the basal planes were nearly unchanged in two kinds of silver nanoplate self-assembled films.
Activation of
β
2
-Adrenergic Receptor Induced by Three Catecholamine Agonists: a Docking and Molecular Dynamics Study
ZHANG Rui, DONG Li-hua, LING Bao-ping, WANG Zhi-guo, LIU Yong-jun
2012, 28(3): 493-499.
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We studied the activation of
β
2
-adrenergic receptor(
β
2
AR) by norepinephrine, epinephrine and isoproterenol using docking and molecular dynamics(MD) simulation. The simulation was done on the assumption that
β
2
AR was surrounded with explicit water and infinite lipid bilayer membrane at body temperature. So the result should be close to that under the physiological conditions. We calculated the structure of binding sites in
β
2
AR for the three activators. We also simulated the change of the conformation of
β
2
AR in the transmembrane regions(TMs), in the molecular switches, and in the conserved DRY(Aspartic acid, Arginine and Tyrosine) motif. This study provides detailed information concerning the structure of
β
2
AR during activation process.
Theoretical Study on GSH Activation Mechanism of a New Type of Glutathione Transferase Gtt2
LI Xue, WU Yun-jian, LI Zhuo, CHU Wen-ting, ZHANG Hong-xing, ZHENG Qing-chuan
2012, 28(3): 500-502.
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)
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Glutathione transferases(GSTs) play an important role in the detoxification of xenobiotic/endobiotic toxic compounds. The
α
-,
π
-, and μ-classes of cytosolic GSTs have been studied extensively, while Gtt2 from
Saccharomyces cerevisiae
, a novel atypical GST, is still poorly understood. In the present study, we investigated the glutathione( GSH) activation mechanism of Gtt2 using the density functional theory(DFT) with the hybrid functional B3LYP. The computational results show that a water molecule could assist a proton transfer between the GSH thiol and the N atom of His133. The energy barrier of proton transfer is 46.0 kJ/mol. The GSH activation mechanism and the characteristics of active site are different from those of classic cytosolic GSTs.
Highly Efficient Organic Ultraviolet Photodetectors Based on Re(I) Complexes
LIU Chun-bo, WANG Long, LIU Min, LI Chuan-bi, LI Chun-mei, CHE Guang-bo, SU Bin
2012, 28(3): 503-506.
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High response organic ultraviolet photodetectors(UV-PDs) were demonstrated with 4,4',4''- tris[3-methyl-pheny(phenyl)amino]triphenylamine(m-MTDATA) and two Re(I) complexes, (bathocuproine)- Re(CO)
3
Cl(Re-BCP) and (bathophenanthroline)Re(CO)
3
Cl(Re-Bphen) to act as the electron donor and acceptor, respectively. UV-PDs have the configuration of indium tin oxide(ITO)/m-MTDATA(25 nm)/m-MTDATA:Re-complex (25―35 nm)/Re-complex(20 nm)/LiF(1 nm)/Al(200 nm) with different blend layer thicknesses of 25, 30 and 35 nm. The optimized PD based on Re-Bphen offers a corrected-dark photocurrent up to 760 μA/cm
2
at ?10 V, corresponding to a response of 310 mA/W which is among the best values reported for organic UV-PDs. Excellent electron transport ability makes for such high photo-to-electron conversion.
Synthesis and Temperature-dependent Electrochemical Properties of Boron-doped Diamond Electrodes on Titanium
DU Li-li, SUN Jian-rui, CUI Hang, LI Hong-dong, CUI Tian, LIN Hai-bo
2012, 28(3): 507-510.
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On the sand-blasting-treated titanium(Ti) substrate, the boron-doped diamond(BDD) electrodes with a wide potential window were prepared by microwave plasma chemical vapor deposition(MPCVD). The electrochemical oxidation ratios of phenol at BDD/Ti electrodes at elevated temperatures(from 20 ℃ to 80 ℃) were examined by the chemical oxygen demand(COD) of phenol electrolyte during electrolysis. The results show that the COD removal was increased at high temperatures and the optimized temperature for enhancing the electrochemical oxidation ratio of phenol is 60 ℃. The mechanism for the temperature-dependent electrochemical oxidation ratios of phenol at the electrodes was investigated. The study would be favorable for further improving the performance of BDD/Ti electrodes, especially working at high temperatures.
In situ
XRD Studies on Heat-treated PtRu/C Nanocatalysts
LIU Juan-ying, LI Zhi-lin, VOGEL Walter, YANG Hui
2012, 28(3): 511-515.
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Extremely small PtRu/C nanocatalysts were prepared via a carbonyl route. A thorough
in situ
reduction X-ray structural characterization of these catalysts was performed. After synthesis and storage under ambient conditions, the diffraction patterns of PtRu/C catalysts were seriously modified, indicating the surface oxide formation. In the reduced state, the particle size is around 2 nm. The observed relative fluctuations of lattice constants are 3%, which is far too large to be explained by a compositional fluctuation. Their origin is attributed to strong but isotropic strains and is related to the alloy formation. The annealing experiments show all the catalysts present an exceptional thermal stability when annealed in inert ambient, especially that of the Pt
1
Ru
1
/C catalyst. Besides, it is interesting to note that there is no thermal expansion evidence from the patterns.
Thermal Behavior and Thermal Safety of Nitrate Glycerol Ether Cellulose
XU Si-yu, ZHAO Feng-qi, YI Jian-hua, GAO Hong-xu, SHAO Zi-qiang, HAO Hai-xia, HU Rong-zu, PEI Qing
2012, 28(3): 516-519.
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The thermal behavior, nonisothermal decomposition reaction kinetics and specific heat capacity of nitrate glycerol ether cellulose(NGEC) were determined by thermogravimetric analysis(TGA), differential scanning calorimetry(DSC) and microcalorimetry. The apparent activity energy(
E
a
), reaction mechanism function, quadratic equation of specific heat capacity(
C
p
) with temperature were obtained. The kinetic parameters of the decomposition reaction are
E
a
=170.2 kJ/mol and lg(
A
/s
–1
)=16.3. The kinetic equation is
f
(
α
)＝(4/3)(1–α)[–ln(1–α)]
1/4
. The specific heat capacity equation is
C
p
=1.285–6.276×10
–3
T
+1.581×10
–5
T
2
(283 K<
T
<353 K). With these parameters, the thermal safety properties of NGEC were studied, such as the self-accelerating decomposition temperature(
T
SADT
), critical temperature of thermal explosion(
T
b
) and adiabatic time-to-explosion(
t
Tlad
). The results of the thermal safety evaluation of NGEC are:
T
SADT
=459.6 K,
T
b
=492.8 K,
t
Tlad
=0.8 s.
Electron Interaction Among the Noncovalently Engineered Graphene-methylene Blue Nanocomposites
LI Zhi, SHI Xiao-jun, GE Xue-ping, WEI Jian-jun, YANG Cun-zhong, FANG Bin, XIE Hai-fen, AN Xing-cai
2012, 28(3): 520-523.
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The electron interaction among the noncovalently engineered graphene-methylene blue(MB) nanocomposite with a dipolar pull-push hybrid model was studied. The
π-π
interaction between reduced graphene oxide(rGO) and MB molecule was studied by
1
HNMR spectroscopy. The electrochemical investigation indicates MB has a stronger electron transfer interaction with rGO than with GO. The ability of graphene-MB nanocomposites to undergo photoinduced electron transfer was confirmed from the capability of the nanocomposites coated electrode to generate photocurrent in a photoelectrochemical cell. The role of graphene as electron acceptor in the opto-electronic assembly was discussed.
Molecular Structure and Properties of a Novel Acylhydrazone (C
14
H
14
O
6
N
4
)·HCON(CH
3
)
2
·2H
2
O
CHEN Feng-ying, WU Wang-ting, LI Heng-xin, HE Shui-yang, WEN Zhen-yi, LI Jia-xing
2012, 28(3): 524-528.
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[N-(Propionic acid)] terephthalal acyl dihydrazone(H
4
L) was synthesized and characterized by element analysis, IR,
1
H NMR and MS. The theoretical studies on H
4
L were carried out at HF/6-31+G(
d
) and B3LYP/ 6-31+G(
d
) levels. The main decomposition stage of it was studied with IR track. The kinetic parameters[the apparent activation energy(
E
a
) and pre-exponential constant(
A
) of the first and second stages of decomposition reaction] were obtained by Kissinger and Ozawa’s methods. Furthermore, the antimicrobial activity of H
4
L against wheat rust was investigated by spore sprout method.
Preparation of Superhydrophobic ZnO Films on Zinc Substrate by Chemical Solution Method
XU Wen-guo, LI Ji-hong, LU Shi-xiang, DUAN Ya-qiong, MA Cheng-xiang, SHI Xiao-feng, CHEN Yi-ling, YANG Yan-bo
2012, 28(3): 529-533.
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Superhydrophobic surface was prepared on the zinc substrate by chemical solution method via immersing clean pure zinc substrate into a water solution of zinc nitrate hexahydrate[Zn(NO
3
)
2
·6H
2
O] and hexamethylenetetraamine( C
6
H
12
N
4
) at 95 ℃ in water bath for 1.5 h, then modified with 18 alkanethiol. The best resulting surface shows superhydrophobic properties with a water contact angle of about 158° and a low water roll-off angle of around 3°. The prepared samples were characterized by powder X-ray diffraction(XRD), X-ray photoelectron spectroscopy (XPS), energy-dispersive X-ray spectroscopy(EDX), transmission electron microscopy(TEM), and scanning electron microscopy(SEM). SEM images of the films show that the resulting surface exhibits flower-shaped micro- and nano-structure. The surfaces of the prepared films were composed of ZnO nanorods which were wurtzite structure. The special flower-like micro- and nano-structure along with the low surface energy leads to the surface superhydrophobicity.
Facile Method to Prepare Metal Sulfide(Ag
2
S, CuS, PbS) Nanoparticles Grown on Surface of Polyacrylonitrile Nanofibre and Their Optical Properties
ZHANG Chao-qun, SUN Jiao, WANG Wei, YANG Qing-biao, LI Yao-xian, DU Jian-shi
2012, 28(3): 534-538.
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Polyacrylonitrile-metal sulfide nanocomposites with metal sulfide(Ag
2
S, CuS, PbS) nanoparticles homogeneously dispersed on the polyacrylonitrile(PAN) nanofibre were synthesized by means of electrospinning technology combined with gas-solid reaction. A series of experiments was performed to characterize the morphology variation and distribution of the nanocrystalline. The result shows that the concentration of metal salt aqueous solution affects the size and morphology of metal sulfide nanoparticles during the chelating process. Further more, these metal ions nanoparticles were attached to the surface of the nanofibre homogeneously through chelating effect which will be propitious to prevent nanoparticles from aggregation. These results suggest that the method reported here is extremely effective for synthesizing PAN-metal sulfide nanocomposites which have good visible light photocatalytic activity. Further more, this method could be extended to prepare other PAN-metal halides nanocomposites, too.
Supercooling Suppression of Microencapsulated
n
-Alkanes by Introducing an Organic Gelator
ZHU Kong-ying, WANG Shuang, QI Heng-zhi, LI Hui, ZHAO Yun-hui, YUAN Xiao-yan
2012, 28(3): 539-541.
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)
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Supercooling of the microencapsulated phase change materials(PCMs) during cooling usually happens. This phenomenon can interfere with heat transfer and is necessary to further overcome. In this study, melamine- formaldehyde microcapsules containing two
n
-alkane PCMs, namely,
n
-dodecane(C
12
) or
n
-tetradecane(C
14
) were prepared by in situ polymerization. A small amount of
n
-hexatriacontane(C
36
) was introduced as an organic gelator into the core of microcapsules to cope with the supercooling problem. Analyses demonstrate that supercooling of the microencapsulated C
12
or C
14
was significantly suppressed by adding 3%(mass fraction) C
36
, without changing the spherical morphology and dispersibility. It could be also found that the enthalpy of microencapsulated C
12
or C
14
containing C
36
was similar to that of microencapsulated
n
-alkanes without C
36
, whereas the difference between onsets of crystallization and melting(degree of supercooling) is similar to that of those of pure
n
-alkanes, suggesting the remarkable suppression ability of the organic gelator on supercooling.
Surface Heparinization of Poly(ether ether ketone)
SUN Hui, CHEN Rui-chao, LIU Shu, XU Guo-zhi
2012, 28(3): 542-545.
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)
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Photo-grafting of hydrophilic monomer and space arms was used to enhance the hydrophilicity of poly(ether ether ketone)(PEEK) with the aim of extending its application to biological fields. PEEK films were surface modified by UV grafting of acrylic acid(AA) to introduce ―COOH on PEEK surface. Adipic amine was used as a space arm to introduce heparin on PEEK surface based on the condensation reaction between ―NH
2
and ―COOH. The modified PEEK(PEEK-COOH, PEEK-NH
2
and PEEK-Hep) was characterized by energy-disperse spectroscopy (EDS), X-ray photoelectron spectroscopy(XPS) and water contact angle measurements, which show that heparin was grafted on PEEK surface. The contact angles of modified PEEK films were lower than those of original films, demonstrating a significant improvement of surface hydrophilicity.
Fabrication of Porous Silica Microspheres Under the Assistance of Solid Template
MAO Zheng-wei, HU Ling, ZHAO Qing-he, GAO Chang-you
2012, 28(3): 546-549.
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)
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Spherical porous silica microparticles were synthesized by a sol-gel process in the presence of porous CaCO
3
particles, followed by removal of the carbonate templates. The resulting silica particles had very high porosity and wide pore size distribution, whose surface area and pore volume reached up to 367.3 m
2
/g and 0.72 mL/g, respectively. With a larger amount of the tetraethyl orthosilicate used, hollow silica microspheres were further obtained. Characterization was made to confirm the chemical and physical structures and purity of the silica microspheres. Spontaneous deposition of tetramethyl rhodamine isothiocyanate labeled dextran into the microspheres was also observed due to the charge attraction.
Synthesis of Perfluorinated Oxetane and Surface Properties of Its Cationic UV Cured Coating as a Reactive Additive
ZHAN Fu, ZHANG Yong, SHI Wen-fang
2012, 28(3): 550-554.
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Perfluorinated oxetane(F-OXE) was synthesized
via
the ring-opening reaction of epoxy-functionalized oxetane with 2-(perfluorooctyl)ethanol under base-catalysis, and characterized by FTIR and
1
H NMR spectroscopy. The synthesized F-OXE was mixed with a commercial cationic UV curable resin, UVR6110, as a reactive additive at different mass fractions, and UV-irradiation cured in the presence of triphenylsulphonium hexafluoroantimonate as a cationic photoinitiator. The surface property study of cured films indicated that both hydrophobicity and oleophobicity were effectively enhanced by the addition of a small amount of F-OXE. The contact angles of water and 1-bromonaphthalene on the surface of the cured film with 1.0%(mass fraction) F-OXE loading increased from 72° to 106° and from 0° to 76°, respectively, compared with those on the surface of the film without F-OXE addition. The surface tension of UVR6110-F-OXE cured film decreased greatly from 55.6 mN/m of referenced film to 22.9 mN/m. The results from X-ray photoelectron spectroscopy analysis confirm the migration and aggregation effect of perfluoroalkyl group to the surface of cured film. For 1%(mass fraction) addition of F-OXE, the relative content of fluorine greatly increased from 0.70%(mass fraction) in the interior of the cured film to 36.73%(mass fraction) at the surface of the cured film, whereas those of carbon and oxygen decreased from 73.29% to 40.96% and from 26.00% to 22.30%, respectively.
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