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2006 Volume 17 Issue 8
2006, 17(8): 995-998
Abstract:
Phakellistatin 13 is a good antitumor lead compound isolated from halobios. It was synthesized first time by solution method in combination of stepwise coupling and segment condensation. Final deprotection and cyclization were achieved according to our designed method, which was different from the reported process. The spectral data of synthetic product is consisted with literatureal data of natural product. Total synthesis of phakellistatin 13 is a significant achievement to further study of its derivatives and developing novel antitumor drugs.
Phakellistatin 13 is a good antitumor lead compound isolated from halobios. It was synthesized first time by solution method in combination of stepwise coupling and segment condensation. Final deprotection and cyclization were achieved according to our designed method, which was different from the reported process. The spectral data of synthetic product is consisted with literatureal data of natural product. Total synthesis of phakellistatin 13 is a significant achievement to further study of its derivatives and developing novel antitumor drugs.
2006, 17(8): 999-1001
Abstract:
A convenient synthetic method of metal dendritic porphyrins through the convergent synthetic strategy is described. The porphyrin core were linked with the synthetic fragments by forming ether or ester bonds to give five target compounds were prepared.
A convenient synthetic method of metal dendritic porphyrins through the convergent synthetic strategy is described. The porphyrin core were linked with the synthetic fragments by forming ether or ester bonds to give five target compounds were prepared.
2006, 17(8): 1002-1004
Abstract:
Novel ferrocenyl-containing thiazole derivatives have been synthesized from 2-amino-4-ferrocenyl-5-(1H-1, 2, 4-triazole-1-yl)thiazole and acyl chloride. And their structures were determined by 1H NMR and elemental analysis.
Novel ferrocenyl-containing thiazole derivatives have been synthesized from 2-amino-4-ferrocenyl-5-(1H-1, 2, 4-triazole-1-yl)thiazole and acyl chloride. And their structures were determined by 1H NMR and elemental analysis.
2006, 17(8): 1005-1008
Abstract:
A mild and efficient procedure to build up various chromone-2-carboxylates was developed. Condensation of diverse 2-hydroxyacetophones with tetr-butyl oxalate in the presence of sodium ethoxide could be accomplished rapidly under mild condition. Cyclodehydration was carried out to achieve chromone-2-carboxylates in one-pot with impressive yield. Advantages over conventional methods with diethyl oxalate were observed in yield and reaction time.
A mild and efficient procedure to build up various chromone-2-carboxylates was developed. Condensation of diverse 2-hydroxyacetophones with tetr-butyl oxalate in the presence of sodium ethoxide could be accomplished rapidly under mild condition. Cyclodehydration was carried out to achieve chromone-2-carboxylates in one-pot with impressive yield. Advantages over conventional methods with diethyl oxalate were observed in yield and reaction time.
2006, 17(8): 1009-1012
Abstract:
A series of acyls (Ac, Bz and Ts) were introduced regioselectively to the 2-hydroxyl in methyl and ally 3-O-benzyl-α-L-rhamnopyranosides mediated by silver(Ⅰ) oxide in the presence of a catalytic amount of potassium iodide in 56-78% yields.
A series of acyls (Ac, Bz and Ts) were introduced regioselectively to the 2-hydroxyl in methyl and ally 3-O-benzyl-α-L-rhamnopyranosides mediated by silver(Ⅰ) oxide in the presence of a catalytic amount of potassium iodide in 56-78% yields.
2006, 17(8): 1013-1016
Abstract:
A new series of compounds, 2-(benzodioxol-2-yl)acetic acids, have been synthesized. Their structures were confirmed by MS and 1H-NMR. The preliminary pharmacological screening showed that these compounds exhibited potent human PPARδ agonist activities.
A new series of compounds, 2-(benzodioxol-2-yl)acetic acids, have been synthesized. Their structures were confirmed by MS and 1H-NMR. The preliminary pharmacological screening showed that these compounds exhibited potent human PPARδ agonist activities.
2006, 17(8): 1017-1020
Abstract:
Synthesis and characterization of two novel potentially tetradentate chelating OΛNΛC ligands: 2-(2-hydroxyphenyl)-6-p-tolylisonicotinic acid and 2-(2-hydroxyphenyl)-6-p-tolylisonicotinic acid ethyl ester were firstly reported.
Synthesis and characterization of two novel potentially tetradentate chelating OΛNΛC ligands: 2-(2-hydroxyphenyl)-6-p-tolylisonicotinic acid and 2-(2-hydroxyphenyl)-6-p-tolylisonicotinic acid ethyl ester were firstly reported.
2006, 17(8): 1021-1024
Abstract:
A new hapten, aldicarb oxime succinic ester (AOSE), was synthesized for immunoassay of aldicarb. It was conjugated to proteins by active ester method. Polyclonal antibody was raised against AOSE-BSA (bovine serum albumin) conjugate. Enzyme-linked immunosorbent assays (ELISAs) showed that this antiserum had high affinity to aldicarb and can be used for sensitive and selective immunoassay of aldicarb.
A new hapten, aldicarb oxime succinic ester (AOSE), was synthesized for immunoassay of aldicarb. It was conjugated to proteins by active ester method. Polyclonal antibody was raised against AOSE-BSA (bovine serum albumin) conjugate. Enzyme-linked immunosorbent assays (ELISAs) showed that this antiserum had high affinity to aldicarb and can be used for sensitive and selective immunoassay of aldicarb.
2006, 17(8): 1025-1028
Abstract:
The addition of platinum over the B2O3/TiO2-ZrO2 remarkably enhanced its catalytic stability in the vapor phase Beckmann rearrangement of cyclohexanone oxime under the carrier gas of H2. The content of coke deposited on catalyst surface was decreased from 1.92% over the B2O3/TiO2-ZrO2 to 1.14% over the platinum promoted B2O3/TiO2-ZrO2 after reaction of six hours. This result indicates that the platinum added on the B2O3/TiO2-ZrO2 catalyst plays an important role in reducing the coke formation on the catalyst surface.
The addition of platinum over the B2O3/TiO2-ZrO2 remarkably enhanced its catalytic stability in the vapor phase Beckmann rearrangement of cyclohexanone oxime under the carrier gas of H2. The content of coke deposited on catalyst surface was decreased from 1.92% over the B2O3/TiO2-ZrO2 to 1.14% over the platinum promoted B2O3/TiO2-ZrO2 after reaction of six hours. This result indicates that the platinum added on the B2O3/TiO2-ZrO2 catalyst plays an important role in reducing the coke formation on the catalyst surface.
2006, 17(8): 1029-1032
Abstract:
The first example of biscalixarene composed of calix[4]arene and thiacalix[4]arene subunits 3 was facilely synthesized and showed good complexation properties for metal cations and zwitterionic α-amino acids.
The first example of biscalixarene composed of calix[4]arene and thiacalix[4]arene subunits 3 was facilely synthesized and showed good complexation properties for metal cations and zwitterionic α-amino acids.
2006, 17(8): 1033-1036
Abstract:
Four novel bisoxazoline ligands 8a-d were synthesized from (S)-amino alcohols and could be formed effective catalysts (up to 77% ee for endo isomer) with Cu(OTf)2 for enantioselective Diels-Alder addition. The facility of the reaction was dependent on the nature of the substituent R in the bisoxazoline ligand.
Four novel bisoxazoline ligands 8a-d were synthesized from (S)-amino alcohols and could be formed effective catalysts (up to 77% ee for endo isomer) with Cu(OTf)2 for enantioselective Diels-Alder addition. The facility of the reaction was dependent on the nature of the substituent R in the bisoxazoline ligand.
2006, 17(8): 1037-1040
Abstract:
The addition of allyltrimethylsilane to tert-butanesulfinyl imines triggered by tetra-n-butylammonium fluoride (TBAF) in the presence of 4A molecular sieves has been studied, and homoallylsulfinamides were obtained in good yields with moderate to high diastereoselectivitics.
The addition of allyltrimethylsilane to tert-butanesulfinyl imines triggered by tetra-n-butylammonium fluoride (TBAF) in the presence of 4A molecular sieves has been studied, and homoallylsulfinamides were obtained in good yields with moderate to high diastereoselectivitics.
2006, 17(8): 1041-1044
Abstract:
3-Methylbutanal was obtained by the Strecker reaction with L-leucine and D-ribose at unelevated temperature and acidic conditions. Volatile compounds from reaction systems were analyzed by solid phase microextration (SPME) coupled with gas chromatography-mass spectroscopy (GC-MS). The formation mechanism of 3-methylbutanal was also proposed. Various reaction conditions were investigated, including reaction time, reaction temperature, pH value and salt content of the system.
3-Methylbutanal was obtained by the Strecker reaction with L-leucine and D-ribose at unelevated temperature and acidic conditions. Volatile compounds from reaction systems were analyzed by solid phase microextration (SPME) coupled with gas chromatography-mass spectroscopy (GC-MS). The formation mechanism of 3-methylbutanal was also proposed. Various reaction conditions were investigated, including reaction time, reaction temperature, pH value and salt content of the system.
2006, 17(8): 1045-1047
Abstract:
Sulphur-containing aromatic nitro compounds were rapidly reduced to the corresponding amines in high yields by employing hydrazine hydrate as a hydrogen donor in the presence of iron oxide hydroxide catalyst. It was worth noting that the catalyst exhibited extremely high activity. The reduction could be completed within 20-50 min and the yields were up to 97-99%.
Sulphur-containing aromatic nitro compounds were rapidly reduced to the corresponding amines in high yields by employing hydrazine hydrate as a hydrogen donor in the presence of iron oxide hydroxide catalyst. It was worth noting that the catalyst exhibited extremely high activity. The reduction could be completed within 20-50 min and the yields were up to 97-99%.
2006, 17(8): 1048-1050
Abstract:
Two new lavandulylated flavanones, (2R, 3R)-8-1avandulyl-2'-methoxy-5, 7, 4'-trihydroxyflavanonol (1) and 8-1avandulyl-5, 7, 4'-trihydroxyflavonol (2), were isolated from the dry roots of Sophora flavescens. Their structures were elucidated on the basis of spectroscopic data. Compounds 1 and 2 exhibited significant antibacterial activities.
Two new lavandulylated flavanones, (2R, 3R)-8-1avandulyl-2'-methoxy-5, 7, 4'-trihydroxyflavanonol (1) and 8-1avandulyl-5, 7, 4'-trihydroxyflavonol (2), were isolated from the dry roots of Sophora flavescens. Their structures were elucidated on the basis of spectroscopic data. Compounds 1 and 2 exhibited significant antibacterial activities.
2006, 17(8): 1051-1053
Abstract:
Two new flavonoid glycosides were isolated from the flowering heads of Chrysanthemum morifolium. Their structures were determined to be luteolin 4'-methoxy-7-O-(6"-O-acetyl)-β-D-glucopyranoside (1) and acacetin 7-O-(3"-O-acetyl)-β-D-glucopyranoside (2) by means of 1H and 13C NMR spectroscopic analysis, including 2D NMR technique.
Two new flavonoid glycosides were isolated from the flowering heads of Chrysanthemum morifolium. Their structures were determined to be luteolin 4'-methoxy-7-O-(6"-O-acetyl)-β-D-glucopyranoside (1) and acacetin 7-O-(3"-O-acetyl)-β-D-glucopyranoside (2) by means of 1H and 13C NMR spectroscopic analysis, including 2D NMR technique.
2006, 17(8): 1054-1056
Abstract:
A new compound, named daphnolin (1), was isolated from the stem barks of Daphne giraldii Nitsche. Its structure was elucidated as 8-hydroxy-7-O-β-D-glucopyranosyl-5-(2-oxo-2H-1-benzopyran-7-hydroxy-8-yloxy)-2H-1-benzopyran-2-one by means of NMR and MS analysis.
A new compound, named daphnolin (1), was isolated from the stem barks of Daphne giraldii Nitsche. Its structure was elucidated as 8-hydroxy-7-O-β-D-glucopyranosyl-5-(2-oxo-2H-1-benzopyran-7-hydroxy-8-yloxy)-2H-1-benzopyran-2-one by means of NMR and MS analysis.
2006, 17(8): 1057-1060
Abstract:
A rapid and sensitive HPLC-DAD method is developed for simultaneous determination of nicorandil and its degradation products, N-(2-hydroxyethyl) nicotinamide, nitrate ion and nicotinic acid, using nicotinamide (NT) as internal standard, at wavelength 204 nm. Nicotinic acid is identified by HPLC and GC/MS. The method can also be applied to study kinetic of degradation processes of nicorandil in storage.
A rapid and sensitive HPLC-DAD method is developed for simultaneous determination of nicorandil and its degradation products, N-(2-hydroxyethyl) nicotinamide, nitrate ion and nicotinic acid, using nicotinamide (NT) as internal standard, at wavelength 204 nm. Nicotinic acid is identified by HPLC and GC/MS. The method can also be applied to study kinetic of degradation processes of nicorandil in storage.
2006, 17(8): 1061-1064
Abstract:
Quasi-interpenetrating network formed by polyacrylamide and poly (N-hydroxymethylacrylamide) was designed, synthesized, and tested for DNA sequencing by capillary electrophoresis. The performance of quasi-IPN on DNA sequencing was determined by the acrylamide to N-hydroxymethylacrylamide molar ratio and sequencing temperature.
Quasi-interpenetrating network formed by polyacrylamide and poly (N-hydroxymethylacrylamide) was designed, synthesized, and tested for DNA sequencing by capillary electrophoresis. The performance of quasi-IPN on DNA sequencing was determined by the acrylamide to N-hydroxymethylacrylamide molar ratio and sequencing temperature.
2006, 17(8): 1065-1068
Abstract:
The interaction between amino acid drugs, aminobutyric acid, carbocisteine and levodopa, with chloranil was studied spectrophotometrically. The conditions were investigated and optimized. The interaction obeyed Beer's law over the range of 0.2-8.7, 1.2-20 and 2-26.4 μg/mL for aminobutyric acid, carbocisteine and levodopa, respectively. The validity was compared with that by the official methods1,3,5 and the recovery studies of standard addition method, the result is satisfactory. The proposed method has been successfully applied to the determination of the above drugs in tablets.
The interaction between amino acid drugs, aminobutyric acid, carbocisteine and levodopa, with chloranil was studied spectrophotometrically. The conditions were investigated and optimized. The interaction obeyed Beer's law over the range of 0.2-8.7, 1.2-20 and 2-26.4 μg/mL for aminobutyric acid, carbocisteine and levodopa, respectively. The validity was compared with that by the official methods1,3,5 and the recovery studies of standard addition method, the result is satisfactory. The proposed method has been successfully applied to the determination of the above drugs in tablets.
2006, 17(8): 1069-1072
Abstract:
The mass spectrometric fragmentation of 1-(benzyloxycarbonyl)amino-2-alkyl/cycloalkyl thioacetates has been studied with the aid of mass-analysed ion kinetic energy spectrometry under electron impact ionization. All compounds show a tendency to eliminate a ketene, thioacetic acid, and benzyl carbamate molecule, or an acetyl and benzyloxy radicals. A thioester pyrolysis-type rearrangement under electron impact ionizations was observed.
The mass spectrometric fragmentation of 1-(benzyloxycarbonyl)amino-2-alkyl/cycloalkyl thioacetates has been studied with the aid of mass-analysed ion kinetic energy spectrometry under electron impact ionization. All compounds show a tendency to eliminate a ketene, thioacetic acid, and benzyl carbamate molecule, or an acetyl and benzyloxy radicals. A thioester pyrolysis-type rearrangement under electron impact ionizations was observed.
2006, 17(8): 1073-1076
Abstract:
A single-drop liquid phase micro-extraction procedure using 1-butyl-3-methylimidazolium hexafluorophosphate ([C4MIM][PF6]) was demonstrated for the sensitive determination of four phenols in water samples. Under the optimized conditions, the linear range of proposed medthod was excellent in the range of 0.5-100μg·L-1,the reproducibility (RSD,n=6) were in the rang 5.4%-8.9% and detection limits(S/N=3) Were 0.3 0.3,0.5 andμg·L-1 for 2.4-dichloro-phenol, 2-naphthol, 2-nitrophenol and 4-chlorophenol, respectively. The experimental results indicated that the effect of complex matrices natural water samples could be resolved with addition of sodium ethylene diamine tetracetate (EDTA) into the samples. Excellent spiked recoveries were achieved for these four phenols ranged from 86.2%-114.9%. All these facts demonstrated that the proposed method with merits of low cost, simplicity and easy operating would be a competitive alternative procedure for the determination of such compounds at trace level.
A single-drop liquid phase micro-extraction procedure using 1-butyl-3-methylimidazolium hexafluorophosphate ([C4MIM][PF6]) was demonstrated for the sensitive determination of four phenols in water samples. Under the optimized conditions, the linear range of proposed medthod was excellent in the range of 0.5-100μg·L-1,the reproducibility (RSD,n=6) were in the rang 5.4%-8.9% and detection limits(S/N=3) Were 0.3 0.3,0.5 andμg·L-1 for 2.4-dichloro-phenol, 2-naphthol, 2-nitrophenol and 4-chlorophenol, respectively. The experimental results indicated that the effect of complex matrices natural water samples could be resolved with addition of sodium ethylene diamine tetracetate (EDTA) into the samples. Excellent spiked recoveries were achieved for these four phenols ranged from 86.2%-114.9%. All these facts demonstrated that the proposed method with merits of low cost, simplicity and easy operating would be a competitive alternative procedure for the determination of such compounds at trace level.
2006, 17(8): 1077-1080
Abstract:
An analytical method using high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for rapid simultaneous determination of Be, Mg, Al, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, Mo, Ag, Cd, Sn, Sb, Ba, Pt, Au and Pb in high purity cobalt was described. Sample digestions were performed in closed microwave vessels using HNO3 and HCl. The matrix effects due to thc presence of excess HCl and Co were evaluated. The usefulness of high mass resolution for overcoming some spectral interference was demonstrated. The optimum conditions for the determination was tested and discussed. Correction for matrix effects, Sc, Rh and Bi were used as internal standards. The detection limits is 0.003-0.57 μg/g, the recovery ratio is 92.2%-111.2%, and the RSD is less than 3.6%. The method is accurate, quick and convenient. It has been applied to the determination of trace impurities in high purity cobalt with satisfactory results.
An analytical method using high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for rapid simultaneous determination of Be, Mg, Al, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, Mo, Ag, Cd, Sn, Sb, Ba, Pt, Au and Pb in high purity cobalt was described. Sample digestions were performed in closed microwave vessels using HNO3 and HCl. The matrix effects due to thc presence of excess HCl and Co were evaluated. The usefulness of high mass resolution for overcoming some spectral interference was demonstrated. The optimum conditions for the determination was tested and discussed. Correction for matrix effects, Sc, Rh and Bi were used as internal standards. The detection limits is 0.003-0.57 μg/g, the recovery ratio is 92.2%-111.2%, and the RSD is less than 3.6%. The method is accurate, quick and convenient. It has been applied to the determination of trace impurities in high purity cobalt with satisfactory results.
2006, 17(8): 1081-1084
Abstract:
An organic-inorganic mercury coordination compound [Hg(DMSO)2(H2O)]2 [GeW12O40]·DMSO·H2O(DMSO=dimethyl sulfoxide) has been synthesized and characterized by IR, UV spectra, elemental analysis, TG-DTA and X-ray single-crystal diffraction. Structural analysis revealed that in the title compound, the mercury is three-coordinated to show the distorted trigonal cone geometry, and depending on the electrostatic interaction to connect the polyanion [α-GeW12O40]4-. TG-DTA study manifests the decomposition temperature of the polyanion framework in the title compound is 513.5℃, which is much higher than that of the anion framework. It means that the formation of the organic-inorganic mercury coordination compound made the polyanion [α-GeW12O40]4- to be more stable.
An organic-inorganic mercury coordination compound [Hg(DMSO)2(H2O)]2 [GeW12O40]·DMSO·H2O(DMSO=dimethyl sulfoxide) has been synthesized and characterized by IR, UV spectra, elemental analysis, TG-DTA and X-ray single-crystal diffraction. Structural analysis revealed that in the title compound, the mercury is three-coordinated to show the distorted trigonal cone geometry, and depending on the electrostatic interaction to connect the polyanion [α-GeW12O40]4-. TG-DTA study manifests the decomposition temperature of the polyanion framework in the title compound is 513.5℃, which is much higher than that of the anion framework. It means that the formation of the organic-inorganic mercury coordination compound made the polyanion [α-GeW12O40]4- to be more stable.
2006, 17(8): 1085-1088
Abstract:
A novel two-dimensional nanopatterned TiO2 thin film has been synthesized through the interaction between cationic Gemini surfactant molecules and the prepared TiO2 colloid nanoparticles with average diameters of 8 nm by controlling the surface pressure of the monolayer. TEM photographs from the formed Gemini-TiO2 composite monolayer confirm that the prepared TiO2 film is of a branch nanopattem.
A novel two-dimensional nanopatterned TiO2 thin film has been synthesized through the interaction between cationic Gemini surfactant molecules and the prepared TiO2 colloid nanoparticles with average diameters of 8 nm by controlling the surface pressure of the monolayer. TEM photographs from the formed Gemini-TiO2 composite monolayer confirm that the prepared TiO2 film is of a branch nanopattem.
2006, 17(8): 1089-1092
Abstract:
Preparation method of photocatalyst, using TiCl4 and SnCl2 as raw material and photocatalytic activity of nano-scaled core-shell Sn2+-doped titania photocatalyst was studied in this paper. The as-prepared samples were studied by UV-Vis, XRD, XPS, TEM. The particles of Sn2+-doped TiO2 photocatalyst, calcined from 150 to 600℃ for 5 h, possesses narrow particle size distribution and the sample was composed of anatase phase. Its photocatalytic efficiency was investigated by UV irradiation.
Preparation method of photocatalyst, using TiCl4 and SnCl2 as raw material and photocatalytic activity of nano-scaled core-shell Sn2+-doped titania photocatalyst was studied in this paper. The as-prepared samples were studied by UV-Vis, XRD, XPS, TEM. The particles of Sn2+-doped TiO2 photocatalyst, calcined from 150 to 600℃ for 5 h, possesses narrow particle size distribution and the sample was composed of anatase phase. Its photocatalytic efficiency was investigated by UV irradiation.
2006, 17(8): 1093-1096
Abstract:
A novel Ti-doped M-site deficient olivine LiFePO4, i.e. Li0.95Fe0.95Ti0.05PO4, was synthesized by a solid-state reaction method. XRD and FTIR were used to characterize the as-prepared samples. As a cathode material for lithium-ion batteries, Li0.95Fe0.95Ti0.05PO4 exhibited improved rate capability.
A novel Ti-doped M-site deficient olivine LiFePO4, i.e. Li0.95Fe0.95Ti0.05PO4, was synthesized by a solid-state reaction method. XRD and FTIR were used to characterize the as-prepared samples. As a cathode material for lithium-ion batteries, Li0.95Fe0.95Ti0.05PO4 exhibited improved rate capability.
2006, 17(8): 1097-1100
Abstract:
Three kinds of cross linked polystyrene resin (PS) supported ruthenium complexes were developed as catalysts for the synthesis of formic acid from carbon dioxide hydrogenation. Many factors, such as the functionalized supports, solvents and ligands, could influence their activities and reuse performances greatly. These immobilized catalysts also offer the industrial advantages such as easy separation.
Three kinds of cross linked polystyrene resin (PS) supported ruthenium complexes were developed as catalysts for the synthesis of formic acid from carbon dioxide hydrogenation. Many factors, such as the functionalized supports, solvents and ligands, could influence their activities and reuse performances greatly. These immobilized catalysts also offer the industrial advantages such as easy separation.
2006, 17(8): 1101-1104
Abstract:
Based on solid phase extraction method, a novel silicon-PDMS-glass microchip for high purity DNA extraction has been developed by using KI as the binding salt. The microfluidic chip fabricated by MEMS technology was composed of a silicon substrate with a coiled channel and a compounded PDMS-glass cover. With this microfluidic chip, the wall of the coiled channel was used as solid phase matrix for binding DNA and DNA was extracted by the fluxion of the binding buffer, washing buffer and elution buffer. KI as a substitute for guanidine, was used successfully as binding salt for purification DNA, obtaining higher purity of genomic DNA and about 13.9 ng DNA from 1 μL rat whole blood in 35 minutes.
Based on solid phase extraction method, a novel silicon-PDMS-glass microchip for high purity DNA extraction has been developed by using KI as the binding salt. The microfluidic chip fabricated by MEMS technology was composed of a silicon substrate with a coiled channel and a compounded PDMS-glass cover. With this microfluidic chip, the wall of the coiled channel was used as solid phase matrix for binding DNA and DNA was extracted by the fluxion of the binding buffer, washing buffer and elution buffer. KI as a substitute for guanidine, was used successfully as binding salt for purification DNA, obtaining higher purity of genomic DNA and about 13.9 ng DNA from 1 μL rat whole blood in 35 minutes.
2006, 17(8): 1105-1108
Abstract:
The effect of Epimedium extract (EE) on erythrocytes was investigated by atomic force microscopy (AFM). The images of the surface structures showed clear concave and progressive increase of surface roughness of erythrocyte after incubation with EE at concentration of 0.2 or 0.05 g/L, far below its critical hemolytic levels. The AFM results also indicated that the granules of the fine surface structure increased, which caused by aggregation of membrane protein. Further study showed that the change in surface topography of erythrocyte membrane might be connected with the increase of intracellular free Ca2+ induced by EE.
The effect of Epimedium extract (EE) on erythrocytes was investigated by atomic force microscopy (AFM). The images of the surface structures showed clear concave and progressive increase of surface roughness of erythrocyte after incubation with EE at concentration of 0.2 or 0.05 g/L, far below its critical hemolytic levels. The AFM results also indicated that the granules of the fine surface structure increased, which caused by aggregation of membrane protein. Further study showed that the change in surface topography of erythrocyte membrane might be connected with the increase of intracellular free Ca2+ induced by EE.
2006, 17(8): 1109-1112
Abstract:
Controlled radical photopolymerization of n-butyl methacrylate(n-BMA) mediated by 4-hydroxy-2,2,6,6-tetramethyl-1-piperidinyloxy(HTEMPO) was carried out in bulk at ambient temperature. It was found that obtained n-BMA homopolymers exhibited narrow polydispersities of around 1.4, which was characterized by GPC. Plots of number-average molecular weight vs. conversion and Ln([M0]/[M]) vs. time were liner respectively, indicating that was a controlled photopolymerization.
Controlled radical photopolymerization of n-butyl methacrylate(n-BMA) mediated by 4-hydroxy-2,2,6,6-tetramethyl-1-piperidinyloxy(HTEMPO) was carried out in bulk at ambient temperature. It was found that obtained n-BMA homopolymers exhibited narrow polydispersities of around 1.4, which was characterized by GPC. Plots of number-average molecular weight vs. conversion and Ln([M0]/[M]) vs. time were liner respectively, indicating that was a controlled photopolymerization.
2006, 17(8): 1113-1116
Abstract:
Novel amphiphilic triblock copolymer poly(p-dioxanone-co-5-benzyloxytrimethylene carbonate)-block-poly(ethylene glycol)-block-poly(p-dioxanone-co-5-benzyloxytrimethylene carbonate) (p(PDO-co-BTMC)-b-PEG-b-p(PDO-co-BTMC)) was successfully synthesized using immobilized porcine pancreas lipase on porous silica particles (IPPL) as the catalyst for the first time. 1H NMR, 13C NMR and GPC analysis were used to confirm the structures of resulting copolymers. The molecular weight (Mn) of the copolymer with feed ratio of 69:20:11 (BTMC:PDO:PEG) was 31300 g/mol and the polydispersity was 1.85, while the Mn decreased to 25000 g/mol and polydispersity of 1.93 with the feed ratio of 50:40:10.
Novel amphiphilic triblock copolymer poly(p-dioxanone-co-5-benzyloxytrimethylene carbonate)-block-poly(ethylene glycol)-block-poly(p-dioxanone-co-5-benzyloxytrimethylene carbonate) (p(PDO-co-BTMC)-b-PEG-b-p(PDO-co-BTMC)) was successfully synthesized using immobilized porcine pancreas lipase on porous silica particles (IPPL) as the catalyst for the first time. 1H NMR, 13C NMR and GPC analysis were used to confirm the structures of resulting copolymers. The molecular weight (Mn) of the copolymer with feed ratio of 69:20:11 (BTMC:PDO:PEG) was 31300 g/mol and the polydispersity was 1.85, while the Mn decreased to 25000 g/mol and polydispersity of 1.93 with the feed ratio of 50:40:10.
2006, 17(8): 1117-1120
Abstract:
A star-shaped multifunctional styrene-isoprene copolymer was synthesized with n-BuLi as initiator, divinyl benzene as coupling agent, cyclohexane as solvent by living anionic polymerization.Using this polymer as grafting agent, a novel star-shaped branched polymer, containing several polyisobutylene, was prepared via cationic polymerization.The star PS-b-PI and star-branched polyisobutylene were characterized by GPC, 1HNMR and FT-IR, and the effects of different adding order and the amount of grafting agent were investigated.
A star-shaped multifunctional styrene-isoprene copolymer was synthesized with n-BuLi as initiator, divinyl benzene as coupling agent, cyclohexane as solvent by living anionic polymerization.Using this polymer as grafting agent, a novel star-shaped branched polymer, containing several polyisobutylene, was prepared via cationic polymerization.The star PS-b-PI and star-branched polyisobutylene were characterized by GPC, 1HNMR and FT-IR, and the effects of different adding order and the amount of grafting agent were investigated.
2006, 17(8): 1121-1124
Abstract:
Siliconated polyurethane (Si-PU) was synthesized using isophorone diisocyanate (IPDI), hydroxybutyl-terminated polydimethylsiloxane (PDMS), polytetramethylene ether glycol (PTMG), polypropylene glycol (PPG), 1,6-hexanediol (HDO), dimethylol propionic acid (DMPA) and triethylamine (TEA). Based on butyl acrylate (BA), 2, 2, 2-trifluoroethylmethacrylate (TFEMA) and Si-PU as a seed emulsion, a novel core-shell type acrylic-polyurethane hybrid emulsion, containing siloxane and fluorine (F-Si-PU), was prepared by seeded emulsion polymerization. The contents of siloxane and fluorine were determined according to the feed ratio. Fourier transform infrared spectroscopy (FTIR) was used to identify the chain structures of Si-PU and F-Si-PU. Investigation of transmission electron microscopy (TEM) confirmed the core-shell structure of F-Si-PU emulsion. Measurement results of water contact angle and the swelling ratio in water and n-octane for cured film showed that the water and the oil resistances for F-Si-PU had been significantly improved at a suitable content of fluorine and siloxane.
Siliconated polyurethane (Si-PU) was synthesized using isophorone diisocyanate (IPDI), hydroxybutyl-terminated polydimethylsiloxane (PDMS), polytetramethylene ether glycol (PTMG), polypropylene glycol (PPG), 1,6-hexanediol (HDO), dimethylol propionic acid (DMPA) and triethylamine (TEA). Based on butyl acrylate (BA), 2, 2, 2-trifluoroethylmethacrylate (TFEMA) and Si-PU as a seed emulsion, a novel core-shell type acrylic-polyurethane hybrid emulsion, containing siloxane and fluorine (F-Si-PU), was prepared by seeded emulsion polymerization. The contents of siloxane and fluorine were determined according to the feed ratio. Fourier transform infrared spectroscopy (FTIR) was used to identify the chain structures of Si-PU and F-Si-PU. Investigation of transmission electron microscopy (TEM) confirmed the core-shell structure of F-Si-PU emulsion. Measurement results of water contact angle and the swelling ratio in water and n-octane for cured film showed that the water and the oil resistances for F-Si-PU had been significantly improved at a suitable content of fluorine and siloxane.
2006, 17(8): 1125-1128
Abstract:
A series of poly(lactic acid-4-hydroxyproline-polyethylene glycol) (PLA-Hpr-PEG) copolymers were synthesized by direct melt copolymerization of D,L-lactic acid and 4-hydroxyproline with different feed amount of polyethylene glycol (PEG) 0.1%, 0.5%, 1% and 5%, respectively. The properties of these copolymers were characterized by using IR spectroscopy, proton nuclear magnetic resonance (1H-NMR) spectroscopy, gel permeation chromatography (GPC), X-ray diffraction and differential scaning calorimetry (DSC). PLA-Hpr-PEG are amorphous copolymers. Copolymers showed increasing water uptake capacity with increasing PEG percentage in the feed, which result in an increasing degradable rate in phosphate buffer solution (pH 7.4) at 37℃.
A series of poly(lactic acid-4-hydroxyproline-polyethylene glycol) (PLA-Hpr-PEG) copolymers were synthesized by direct melt copolymerization of D,L-lactic acid and 4-hydroxyproline with different feed amount of polyethylene glycol (PEG) 0.1%, 0.5%, 1% and 5%, respectively. The properties of these copolymers were characterized by using IR spectroscopy, proton nuclear magnetic resonance (1H-NMR) spectroscopy, gel permeation chromatography (GPC), X-ray diffraction and differential scaning calorimetry (DSC). PLA-Hpr-PEG are amorphous copolymers. Copolymers showed increasing water uptake capacity with increasing PEG percentage in the feed, which result in an increasing degradable rate in phosphate buffer solution (pH 7.4) at 37℃.
2006, 17(8): 1129-1132
Abstract:
This paper gives a brief report of the synthesis of a new kind of solid-solid phase change materials (SSPCMs), nano-crystalline cellulose/polyethylene glycol (NCC/PEG). These PCMs have very high ability for energy storage, and their enthalpies reach 103.8 J/g. They are composed of two parts, PEG as functional branches for energy storage, and NCC as skeleton. The flexible polymer PEG was grafted onto the surface of rigid powder of NCC by covalent bonds. The results of DSC, FT-IR were briefly introduced, and some comments were also given.
This paper gives a brief report of the synthesis of a new kind of solid-solid phase change materials (SSPCMs), nano-crystalline cellulose/polyethylene glycol (NCC/PEG). These PCMs have very high ability for energy storage, and their enthalpies reach 103.8 J/g. They are composed of two parts, PEG as functional branches for energy storage, and NCC as skeleton. The flexible polymer PEG was grafted onto the surface of rigid powder of NCC by covalent bonds. The results of DSC, FT-IR were briefly introduced, and some comments were also given.
2006, 17(8): 1133-1136
Abstract:
Low density polyethylene film surface-grafted phenolic resole was prepared by a sequential processes. Firstly, acrylic acid was grafted to the surface of low density polyethylene by photo-grafting. Secondly, the carboxylic groups in poly(acrylic acid) chains were transferred to sulfonic groups by the reaction of carboxylic groups with sulfanilic acid. Finally, a thin layer of phenolic resole was cured onto the surface of low density polyethylene. The grafting process was characterized by FTIR-ATR and gravimetric analysis. A possible model was proposed to interpret the experimental results.
Low density polyethylene film surface-grafted phenolic resole was prepared by a sequential processes. Firstly, acrylic acid was grafted to the surface of low density polyethylene by photo-grafting. Secondly, the carboxylic groups in poly(acrylic acid) chains were transferred to sulfonic groups by the reaction of carboxylic groups with sulfanilic acid. Finally, a thin layer of phenolic resole was cured onto the surface of low density polyethylene. The grafting process was characterized by FTIR-ATR and gravimetric analysis. A possible model was proposed to interpret the experimental results.
