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2016 Volume 33 Issue 6
2016, 33(6): 611-623
doi: 10.11944/j.issn.1000-0518.2016.06.150299
Abstract:
Organic phosphorus-containing flame retardants have good characteristics, such as high efficiency, low toxicity, no pollution and smokeless. To date, research of synthesis and application in this field attracts a lot of attention. This paper reviewed recent developments, current status and potential future trends of organic phosphorus-containing flame retardants. The classification and mechanism of organic phosphorus-containing flame retardants were also introduced. The development and problems in the application were outlined considering the aspects of organic phosphorus-containing fire retardants.
Organic phosphorus-containing flame retardants have good characteristics, such as high efficiency, low toxicity, no pollution and smokeless. To date, research of synthesis and application in this field attracts a lot of attention. This paper reviewed recent developments, current status and potential future trends of organic phosphorus-containing flame retardants. The classification and mechanism of organic phosphorus-containing flame retardants were also introduced. The development and problems in the application were outlined considering the aspects of organic phosphorus-containing fire retardants.
2016, 33(6): 624-632
doi: 10.11944/j.issn.1000-0518.2016.06.150411
Abstract:
Carbon dots are a kind of novel carbon nanoparticles and have attracted intense attention due to the unique fluorescence properties, low toxicity, good biocompatibility and low cost compared with traditional semiconductor quantum dot fluorescent probes. In this review we overview the properties of carbon dots and their researching progress in chemiluminescence analysis. The application perspective is also presented.
Carbon dots are a kind of novel carbon nanoparticles and have attracted intense attention due to the unique fluorescence properties, low toxicity, good biocompatibility and low cost compared with traditional semiconductor quantum dot fluorescent probes. In this review we overview the properties of carbon dots and their researching progress in chemiluminescence analysis. The application perspective is also presented.
2016, 33(6): 633-640
doi: 10.11944/j.issn.1000-0518.2016.06.160137
Abstract:
Calixarenes, as the third generation of host molecules in supramolecular chemistry due to their facile modification and unique molecular or ion recognition ability, have received great attention during the last few decades. In the present work, three carboxyl acid-appended calix[4]arene derivatives were prepared. The compounds are characterized by four tert-butyl groups appended at the upper rim of the main body of the compounds, and one, two or four carboxyl acid moieties appended at the lower rim, of which they are denoted as CMA, CDA and CTA, respectively. The as-prepared compounds possess surfactant-like structure but insoluble in water. Gelation tests reveal that the compound with more carboxyl groups shows stronger gelation ability. For example, among the seventeen organic liquids and ten monomeric liquids tested, CTA gels seven of them, CDA gels one of then, but CMA and the control C4, which possesses none of the carboxyl acid structure, gel none of them. Further studies demonstrate that the CTA gels with monomeric liquids as solvents have good heat reversibility and can be emulsified with water, resulting in gel-emulsions. Polymerization of the gel-emulsions results in low density polymeric monoliths with porous internal structures. Preliminary test shows that the porous materials as produced are good adsorbents of organic liquids such as benzene, and heavy metal ions such as Cr(Ⅲ). Moreover, the materials can be reused via simple washing and drying process and have potential application in water purification.
Calixarenes, as the third generation of host molecules in supramolecular chemistry due to their facile modification and unique molecular or ion recognition ability, have received great attention during the last few decades. In the present work, three carboxyl acid-appended calix[4]arene derivatives were prepared. The compounds are characterized by four tert-butyl groups appended at the upper rim of the main body of the compounds, and one, two or four carboxyl acid moieties appended at the lower rim, of which they are denoted as CMA, CDA and CTA, respectively. The as-prepared compounds possess surfactant-like structure but insoluble in water. Gelation tests reveal that the compound with more carboxyl groups shows stronger gelation ability. For example, among the seventeen organic liquids and ten monomeric liquids tested, CTA gels seven of them, CDA gels one of then, but CMA and the control C4, which possesses none of the carboxyl acid structure, gel none of them. Further studies demonstrate that the CTA gels with monomeric liquids as solvents have good heat reversibility and can be emulsified with water, resulting in gel-emulsions. Polymerization of the gel-emulsions results in low density polymeric monoliths with porous internal structures. Preliminary test shows that the porous materials as produced are good adsorbents of organic liquids such as benzene, and heavy metal ions such as Cr(Ⅲ). Moreover, the materials can be reused via simple washing and drying process and have potential application in water purification.
2016, 33(6): 641-648
doi: 10.11944/j.issn.1000-0518.2016.06.150351
Abstract:
The interfacial dilational rheological method was used to study the interfacial aggregation behavior of zwitterionic imidazole surfactant 3-(1-dodecyl-3-imidazolio)propanesulfonate(C12imSP) solutions. The effect and mechanism of traditional surfactant sodium dodecyl sulfate(SDS) on the aggregation behavior of C12imSP at air/water interface were explored. The results have shown that the SDS molecules tend to fill the vacancy among C12imSP molecules when the C12imSP molecules arrange loosely at interface, and mixed-adsorption films formed by SDS and C12imSP spread on the air/water interface, correspondingly, the interfacial tension decrease dramatically. With the increase of SDS concentration, the diffusion exchange of molecules from bulk phase to interface is predominant and the interfacial layer reaches saturation adsorption gradually. Thereafter, the mixed micelles appear in the system. The "acceptance" and the further "detainment" of the rich SDS molecules in micelles to C12imSP molecules as well as the larger steric hindrance of C12imSP themselves lead to the C12imSP molecules are very difficult to revert to the interface once they are exchanged into bulk phase. Namely, SDS almost entirely occupy the air/water interface. Obviously, the interfacial aggregation behavior of SDS/C12imSP/NaCl(0.1 mol/L) system can be adjusted by tailor the system composition and thus realize the regulation to the properties of interfacial film.
The interfacial dilational rheological method was used to study the interfacial aggregation behavior of zwitterionic imidazole surfactant 3-(1-dodecyl-3-imidazolio)propanesulfonate(C12imSP) solutions. The effect and mechanism of traditional surfactant sodium dodecyl sulfate(SDS) on the aggregation behavior of C12imSP at air/water interface were explored. The results have shown that the SDS molecules tend to fill the vacancy among C12imSP molecules when the C12imSP molecules arrange loosely at interface, and mixed-adsorption films formed by SDS and C12imSP spread on the air/water interface, correspondingly, the interfacial tension decrease dramatically. With the increase of SDS concentration, the diffusion exchange of molecules from bulk phase to interface is predominant and the interfacial layer reaches saturation adsorption gradually. Thereafter, the mixed micelles appear in the system. The "acceptance" and the further "detainment" of the rich SDS molecules in micelles to C12imSP molecules as well as the larger steric hindrance of C12imSP themselves lead to the C12imSP molecules are very difficult to revert to the interface once they are exchanged into bulk phase. Namely, SDS almost entirely occupy the air/water interface. Obviously, the interfacial aggregation behavior of SDS/C12imSP/NaCl(0.1 mol/L) system can be adjusted by tailor the system composition and thus realize the regulation to the properties of interfacial film.
2016, 33(6): 649-654
doi: 10.11944/j.issn.1000-0518.2016.06.150378
Abstract:
Benzaldehyde glycol acetal was synthesized by aluminum dihydrogen tripolyphosphate supported on nitric acid modified activated carbon. The effect of the molar ratio of alcohol to aldehyde, catalyst amount and reaction time on the yield were studied by single-factor experiments. Orthogonal design was used to obtain the optimized conditions for the synthesis of benzaldehyde glycol acetal. The results show that the three main influencing factors are in the order as follows:the molar ratio of alcohol to aldehyde >the reaction time >the quantity of water carrying agent >the quantity of catalyst. The optimal technical conditions are:temperature 110℃, benzaldehyde 0.2 mol, the molar ratio of alcohol to aldehyde is 2.5, reaction time 75 min, the quantity of catalyst 4%, water-carrying agent of cyclohexane 25 mL. Under these conditions, the yield of benzaldehyde glycol acetal is above 86.5%. The catalyst can be recycled for multiple uses and the acetal yield is 86.0% after five cycles.
Benzaldehyde glycol acetal was synthesized by aluminum dihydrogen tripolyphosphate supported on nitric acid modified activated carbon. The effect of the molar ratio of alcohol to aldehyde, catalyst amount and reaction time on the yield were studied by single-factor experiments. Orthogonal design was used to obtain the optimized conditions for the synthesis of benzaldehyde glycol acetal. The results show that the three main influencing factors are in the order as follows:the molar ratio of alcohol to aldehyde >the reaction time >the quantity of water carrying agent >the quantity of catalyst. The optimal technical conditions are:temperature 110℃, benzaldehyde 0.2 mol, the molar ratio of alcohol to aldehyde is 2.5, reaction time 75 min, the quantity of catalyst 4%, water-carrying agent of cyclohexane 25 mL. Under these conditions, the yield of benzaldehyde glycol acetal is above 86.5%. The catalyst can be recycled for multiple uses and the acetal yield is 86.0% after five cycles.
2016, 33(6): 655-660
doi: 10.11944/j.issn.1000-0518.2016.06.150327
Abstract:
USY zeolite supported cobalt boride amorphous alloy catalysts(CoB/USY) were prepared via a combined impregnation and chemical reduction method. Their catalytic activities were investigated in hydrogen production from the hydrolysis of NaBH4. XRD characterization indicates that CoB active components supported by USY zeolite have excellent amorphous structure. Micro-morphology of CoB/USY supported catalysts and powdered CoB were checked using SEM. SEM images show that the amorphous CoB are well dispersed onto USY surface which brings relatively high dispersions of CoB species. In the hydrogen generation from NaBH4 hydrolysis, CoB/USY supported catalyst exhibits much higher catalytic activity compared with powdered CoB catalyst. The hydrogen generation rate of CoB/USY supported catalysts reaches about 1.5 L/(min·g), when the temperature is 30℃. The calculated apparent activation energy for NaBH4 hydrolysis is 65.9 kJ/mol based on CoB/USY supported catalysts which is obviously lower than that of powdered CoB catalyst(72.1 kJ/mol).
USY zeolite supported cobalt boride amorphous alloy catalysts(CoB/USY) were prepared via a combined impregnation and chemical reduction method. Their catalytic activities were investigated in hydrogen production from the hydrolysis of NaBH4. XRD characterization indicates that CoB active components supported by USY zeolite have excellent amorphous structure. Micro-morphology of CoB/USY supported catalysts and powdered CoB were checked using SEM. SEM images show that the amorphous CoB are well dispersed onto USY surface which brings relatively high dispersions of CoB species. In the hydrogen generation from NaBH4 hydrolysis, CoB/USY supported catalyst exhibits much higher catalytic activity compared with powdered CoB catalyst. The hydrogen generation rate of CoB/USY supported catalysts reaches about 1.5 L/(min·g), when the temperature is 30℃. The calculated apparent activation energy for NaBH4 hydrolysis is 65.9 kJ/mol based on CoB/USY supported catalysts which is obviously lower than that of powdered CoB catalyst(72.1 kJ/mol).
2016, 33(6): 661-667
doi: 10.11944/j.issn.1000-0518.2016.06.150358
Abstract:
Six benzamide derivatives were synthesized from 4-hydroxybenzoic acid via alkylation, hydrolysis and condensation reactions. The structure was confirmed by 1H NMR, 13C NMR and MS. The antitumor activity of all the newly synthesized compounds was evaluated on the in vitro growth of HepG2 cell line using sorafeinb as positive control. The anti-hepatoma biological activity in vitro of N-(1-(methylsulfonyl)piperidin-4-yl)-4-phenoxybenzamide is better than that of sorafeinb with an IC50 value of 8.42 μmol/L. The results show that the derivatives of N-(piperidin-4-yl)-4-phenoxybenzamide have good anti-hepatoma activity.
Six benzamide derivatives were synthesized from 4-hydroxybenzoic acid via alkylation, hydrolysis and condensation reactions. The structure was confirmed by 1H NMR, 13C NMR and MS. The antitumor activity of all the newly synthesized compounds was evaluated on the in vitro growth of HepG2 cell line using sorafeinb as positive control. The anti-hepatoma biological activity in vitro of N-(1-(methylsulfonyl)piperidin-4-yl)-4-phenoxybenzamide is better than that of sorafeinb with an IC50 value of 8.42 μmol/L. The results show that the derivatives of N-(piperidin-4-yl)-4-phenoxybenzamide have good anti-hepatoma activity.
2016, 33(6): 668-676
doi: 10.11944/j.issn.1000-0518.2016.06.150322
Abstract:
Based on the combination of different active groups with different herbicidal modes of action, a series of diamide compounds 3a~3v containing of 2-(aryloxy)acetyl and meta-trifluoromethylphenyl moieties were designed and synthesized via the four-component Ugi reaction. Their structures were characterized by IR, 1H NMR, EI-MS, and elemental analyses. The glass house bioassay(in vivo) shows that some of compounds 3 exhibit moderate to good herbicidal activities against B.campestris, A.retroflexus, E.crusgalli, and D.sanguinalis at a dose of 1.5 kg/ha. For example, compound 3r displays 100% inhibition aganist both of A.retroflexus and D.sanguinalis in the pre-emergence treatment, it also exhibits 100% inhibition aganist D.sanguinalis in the post-emergence treatment. In addition, the preliminary structure-activity relationships are also discussed.
Based on the combination of different active groups with different herbicidal modes of action, a series of diamide compounds 3a~3v containing of 2-(aryloxy)acetyl and meta-trifluoromethylphenyl moieties were designed and synthesized via the four-component Ugi reaction. Their structures were characterized by IR, 1H NMR, EI-MS, and elemental analyses. The glass house bioassay(in vivo) shows that some of compounds 3 exhibit moderate to good herbicidal activities against B.campestris, A.retroflexus, E.crusgalli, and D.sanguinalis at a dose of 1.5 kg/ha. For example, compound 3r displays 100% inhibition aganist both of A.retroflexus and D.sanguinalis in the pre-emergence treatment, it also exhibits 100% inhibition aganist D.sanguinalis in the post-emergence treatment. In addition, the preliminary structure-activity relationships are also discussed.
2016, 33(6): 677-684
doi: 10.11944/j.issn.1000-0518.2016.06.150316
Abstract:
A visible-light-induced cyclization reaction of activated alkenes leading to difluoroacetating isoquinolinedione was developed. By visible-light photoredox catalysis, various N-alkyl-N-methacryloyl benzamides underwent radical cascade cyclization smoothly and afforded a series of difluoroacetating isoquinolinediones in 66%~75% yields, providing a highly efficient, mild means to fluorinated isoquinolinediones with potential bioactivity.
A visible-light-induced cyclization reaction of activated alkenes leading to difluoroacetating isoquinolinedione was developed. By visible-light photoredox catalysis, various N-alkyl-N-methacryloyl benzamides underwent radical cascade cyclization smoothly and afforded a series of difluoroacetating isoquinolinediones in 66%~75% yields, providing a highly efficient, mild means to fluorinated isoquinolinediones with potential bioactivity.
2016, 33(6): 685-692
doi: 10.11944/j.issn.1000-0518.2016.06.150317
Abstract:
A visible-light-induced radical cascade addition cyclization reaction of activated alkenes with perfluoroalkyl iodide toward perfluorinated isoquinolinediones was developed. By visible-light photoredox catalysis, various N-alkyl-N-methacryloyl benamides underwent radical cyclization smoothly and afforded a series of synthetically important perfluorinated isoquinolinediones in 54%~80% yields. This work provides a highly efficient, mild condition, "green" means to pharmaceutically important perfluorinated isoquinolinediones.
A visible-light-induced radical cascade addition cyclization reaction of activated alkenes with perfluoroalkyl iodide toward perfluorinated isoquinolinediones was developed. By visible-light photoredox catalysis, various N-alkyl-N-methacryloyl benamides underwent radical cyclization smoothly and afforded a series of synthetically important perfluorinated isoquinolinediones in 54%~80% yields. This work provides a highly efficient, mild condition, "green" means to pharmaceutically important perfluorinated isoquinolinediones.
2016, 33(6): 693-700
doi: 10.11944/j.issn.1000-0518.2016.06.150309
Abstract:
Block copolymers with different block raties(n(St):n(G8-2-8)) were prepared through in-situ polymerization in the acetic acid casting solution of quaternized chitosan(QCS), using styrene(St) and Gemini-type cationic molecules maleic acid diethyl brace base pairs[essien alkyl dimethyl chloride/ammonium bromide](G8-2-8) as raw materials and potassium persulfate(KPS) as the initiator. A series of semi-interpenetrating network structure(Semi-IPN) of anion conducting membranes was prepared using glutaraldehyde(GA) as the crosslinking agent. The above linear block polymer was locked in the QCS network structure. The experimental results show that the anion conducting membrane has high mechanical properties and high anionic conductivity. The anion conducting membrane(n(St):n(G8-2-8)=5:1, m(G8-2-8):m(QCS)=20:100) shows the highest ion exchange capacity(1.35 mmol/g), elongation at break(26.47%) and conductivity(70℃, 6.97×10-2 S/cm). TGA results show that the membrane has good thermal stability and the initiate decomposition temperature is higher than 210℃.
Block copolymers with different block raties(n(St):n(G8-2-8)) were prepared through in-situ polymerization in the acetic acid casting solution of quaternized chitosan(QCS), using styrene(St) and Gemini-type cationic molecules maleic acid diethyl brace base pairs[essien alkyl dimethyl chloride/ammonium bromide](G8-2-8) as raw materials and potassium persulfate(KPS) as the initiator. A series of semi-interpenetrating network structure(Semi-IPN) of anion conducting membranes was prepared using glutaraldehyde(GA) as the crosslinking agent. The above linear block polymer was locked in the QCS network structure. The experimental results show that the anion conducting membrane has high mechanical properties and high anionic conductivity. The anion conducting membrane(n(St):n(G8-2-8)=5:1, m(G8-2-8):m(QCS)=20:100) shows the highest ion exchange capacity(1.35 mmol/g), elongation at break(26.47%) and conductivity(70℃, 6.97×10-2 S/cm). TGA results show that the membrane has good thermal stability and the initiate decomposition temperature is higher than 210℃.
2016, 33(6): 701-709
doi: 10.11944/j.issn.1000-0518.2016.06.150413
Abstract:
A well-defined polymer with pendant salicylaldehyde groups(PHVB) was achieved by reversible addition-fragmentation chain transfer(RAFT) polymerization with S-1-dodecyl-S'-(α,α'-dimethyl-α"-acetic acid) trithiocarbonate as the RAFT agent and a salicylaldehyde-functionalized vinyl monomer, 2-hydroxy-5-vinylbenzaldehyde(HVB) in THF at 65℃. The resulting well-defined polymer with pendant salicylaldehyde groups can react directly with monoamine-terminated PEG(PEG-NH2, number-average relative molecular mass 2000 g/mL, 0.5 stoichiometric number of the -CHO group in PolyHVB) to afford an amphiphilic graft copolymer bearing a pendant salicylidene Schiff base PHVB-graft-PEG with 50% grafting density. These new polymers were characterized by GPC and 1HNMR. Owing to the presence of hydrophilic PEG pendants, PHVB-graft-PEG is capable of self-assembling into nano-sized micelles with salicylidene Schiff base functioned cores, PEG coronas in ethanol. Coordination of the pre-assembled PHVB-graft-PEG micelles with Zn(OAc)2 will endow the polymeric micelles with fluorescence features, and simultaneously the resulting luminescent micelles may be stabilized by ionic cross-linking in consequence of the complex reaction at the core. Thus, the luminescence properties and form of the obtained micelles were investigated by UV-Vis spectra(UV-Vis), fluorescence spectra(FLL), dynamic light scattering(DLS), transmission electron microscopy(TEM).After removing ethanol by drying, the resultant Zn2+ coordinated particles can be re-dispersed readily in water or common organic solvent to form a micellar solution, which display blue fluorescence with maximum emission peak around 460 nm, indicating the same aggregate size(nearly 100 nm) as before re-dispersion. The obtained luminescent nanoparticles can be used as a highly selective fluorescent probe for Cu2+ ion over other metal ions such as Cd2 +, Mg2+, Ni2+, Pb2+, Ca2+, Hg2+, Al3+, Mn2+ in aqueous solution, and exhibit a linear range of 0~50 μmol/L and detection limit of 0.05 μmol/L Cu2+, respectively.
A well-defined polymer with pendant salicylaldehyde groups(PHVB) was achieved by reversible addition-fragmentation chain transfer(RAFT) polymerization with S-1-dodecyl-S'-(α,α'-dimethyl-α"-acetic acid) trithiocarbonate as the RAFT agent and a salicylaldehyde-functionalized vinyl monomer, 2-hydroxy-5-vinylbenzaldehyde(HVB) in THF at 65℃. The resulting well-defined polymer with pendant salicylaldehyde groups can react directly with monoamine-terminated PEG(PEG-NH2, number-average relative molecular mass 2000 g/mL, 0.5 stoichiometric number of the -CHO group in PolyHVB) to afford an amphiphilic graft copolymer bearing a pendant salicylidene Schiff base PHVB-graft-PEG with 50% grafting density. These new polymers were characterized by GPC and 1HNMR. Owing to the presence of hydrophilic PEG pendants, PHVB-graft-PEG is capable of self-assembling into nano-sized micelles with salicylidene Schiff base functioned cores, PEG coronas in ethanol. Coordination of the pre-assembled PHVB-graft-PEG micelles with Zn(OAc)2 will endow the polymeric micelles with fluorescence features, and simultaneously the resulting luminescent micelles may be stabilized by ionic cross-linking in consequence of the complex reaction at the core. Thus, the luminescence properties and form of the obtained micelles were investigated by UV-Vis spectra(UV-Vis), fluorescence spectra(FLL), dynamic light scattering(DLS), transmission electron microscopy(TEM).After removing ethanol by drying, the resultant Zn2+ coordinated particles can be re-dispersed readily in water or common organic solvent to form a micellar solution, which display blue fluorescence with maximum emission peak around 460 nm, indicating the same aggregate size(nearly 100 nm) as before re-dispersion. The obtained luminescent nanoparticles can be used as a highly selective fluorescent probe for Cu2+ ion over other metal ions such as Cd2 +, Mg2+, Ni2+, Pb2+, Ca2+, Hg2+, Al3+, Mn2+ in aqueous solution, and exhibit a linear range of 0~50 μmol/L and detection limit of 0.05 μmol/L Cu2+, respectively.
2016, 33(6): 710-718
doi: 10.11944/j.issn.1000-0518.2016.06.150350
Abstract:
Two complexes {[Ni(H2biim)3](phth)}(H2biim=2,2'-biimidazole, phth=phthalate)(1) and[Cd(H3biim)2Cl4](2) were synthesized under hydrothermal and common solution conditions, and characterized by elemental analysis, IR spectroscopy and single crystal X-ray diffraction analysis. Complex 1 consists of[Ni(H2biim)3]2+ cations hydrogen bonds with phthalate dianions. Each Ni atom coordinates six N atoms of three chelating biimidazole ligands in a pseudo-octahedral geometry. Complex 2 is a neutral compound. One N atom in H2biim is protonated, forming a H3biim+ cation. The central metal Cd is coordinated by two unidentate H3biim+ ligands and four Cl atoms. The binding of the complexes with calf thymus DNA has been investigated by UV and fluorescence spectroscopy and viscosity measurement. All of the results indicate that the complexes 1 and 2 bind to DNA base pairs in intercalation and partial intercalation modes, respectively.
Two complexes {[Ni(H2biim)3](phth)}(H2biim=2,2'-biimidazole, phth=phthalate)(1) and[Cd(H3biim)2Cl4](2) were synthesized under hydrothermal and common solution conditions, and characterized by elemental analysis, IR spectroscopy and single crystal X-ray diffraction analysis. Complex 1 consists of[Ni(H2biim)3]2+ cations hydrogen bonds with phthalate dianions. Each Ni atom coordinates six N atoms of three chelating biimidazole ligands in a pseudo-octahedral geometry. Complex 2 is a neutral compound. One N atom in H2biim is protonated, forming a H3biim+ cation. The central metal Cd is coordinated by two unidentate H3biim+ ligands and four Cl atoms. The binding of the complexes with calf thymus DNA has been investigated by UV and fluorescence spectroscopy and viscosity measurement. All of the results indicate that the complexes 1 and 2 bind to DNA base pairs in intercalation and partial intercalation modes, respectively.
2016, 33(6): 719-726
doi: 10.11944/j.issn.1000-0518.2016.06.150323
Abstract:
To analyze the chemical constituents of the essential oils of leaf, stem, and fruit from Euonymus japonicus Thunb. and study their antiviral activities, the volatile oils were extracted by supercritical carbon dioxide and were separated and identified by GC-MS. Their antiviral activities in vitro were inspected. There are 133 components identified, in which the main constituents are 2-ethoxy-propane(41.92%), (E)-2-hexen-1-ol(17.80%), (E)-3,7-dimethyl-2,6-octadien-1-ol(7.86%), methyl cyclohexane(6.60%) from the leaf volatile oil, methoxy phenyl oxime(33.10%), octacosane(14.34%), α-methyl-α-[4-methyl-3-pentenyl]oxiranemethanol(12.48%), toluene(11.88%)and heneicosane(7.74%) from the stem volatile oil and benzaldehyde(15.52%), toluene(15.03%), methyl cyclohexane(14.76%) and (Z)-3-hexen-1-ol(10.98%) from the fruit volatile oil. The volatile oils of the leaf, stem and fruit extracted by cyclonexane and ether show special inhibiting activities against some viruses. Chemical compositions of the volatile oils of the leaf, stem, and fruit show significant differences and special antiviral activities.
To analyze the chemical constituents of the essential oils of leaf, stem, and fruit from Euonymus japonicus Thunb. and study their antiviral activities, the volatile oils were extracted by supercritical carbon dioxide and were separated and identified by GC-MS. Their antiviral activities in vitro were inspected. There are 133 components identified, in which the main constituents are 2-ethoxy-propane(41.92%), (E)-2-hexen-1-ol(17.80%), (E)-3,7-dimethyl-2,6-octadien-1-ol(7.86%), methyl cyclohexane(6.60%) from the leaf volatile oil, methoxy phenyl oxime(33.10%), octacosane(14.34%), α-methyl-α-[4-methyl-3-pentenyl]oxiranemethanol(12.48%), toluene(11.88%)and heneicosane(7.74%) from the stem volatile oil and benzaldehyde(15.52%), toluene(15.03%), methyl cyclohexane(14.76%) and (Z)-3-hexen-1-ol(10.98%) from the fruit volatile oil. The volatile oils of the leaf, stem and fruit extracted by cyclonexane and ether show special inhibiting activities against some viruses. Chemical compositions of the volatile oils of the leaf, stem, and fruit show significant differences and special antiviral activities.
2016, 33(6): 727-732
doi: 10.11944/j.issn.1000-0518.2016.06.150325
Abstract:
In this paper, a beta-glucan binding protein of horseshoe crab(limulus polyphemus) factor G-subunit α fragment-a was cloned, expressed and purified. A turbidimetry assay for the detection of beta-glucan was established. The DNA fragment of the binding protein gene was cloned into an expressional plasmid pET-15b. The protein was expressed with 6x-Histag on N-terminal and purified with Ni-column. The purified protein has relative molecular mass of 40000(1251 bp) on SDS-PAGE and the concentration is 2 g/L with the purity of >98%. The highly purified protein can combine with beta-glucan specifically with an affinity constant KD of 3.14×10-9 mol/L. The absorbance measurement at 340 nm using the ultraviolet spectrophotometer shows that the absorbance is linearly correlated with the concentration of beta-glucan. The linear range is 3.125~200 mg/L, R2 is 0.997, and the detection limit is 3.125 mg/L. The novel turbidimetry assay for the detection of beta-glucan has low cost, rapid, and highly sensitive and specific.
In this paper, a beta-glucan binding protein of horseshoe crab(limulus polyphemus) factor G-subunit α fragment-a was cloned, expressed and purified. A turbidimetry assay for the detection of beta-glucan was established. The DNA fragment of the binding protein gene was cloned into an expressional plasmid pET-15b. The protein was expressed with 6x-Histag on N-terminal and purified with Ni-column. The purified protein has relative molecular mass of 40000(1251 bp) on SDS-PAGE and the concentration is 2 g/L with the purity of >98%. The highly purified protein can combine with beta-glucan specifically with an affinity constant KD of 3.14×10-9 mol/L. The absorbance measurement at 340 nm using the ultraviolet spectrophotometer shows that the absorbance is linearly correlated with the concentration of beta-glucan. The linear range is 3.125~200 mg/L, R2 is 0.997, and the detection limit is 3.125 mg/L. The novel turbidimetry assay for the detection of beta-glucan has low cost, rapid, and highly sensitive and specific.
