A novel water-soluble cystine C60 derivative was synthesized in the presence of the catalyst, tetrabutylammonium hydroxide （TBAH）. The product was characterized by FT-IR, UV, ^1H NMR, ^13C NMR, MS and elemental anal...A novel water-soluble cystine C60 derivative was synthesized in the presence of the catalyst, tetrabutylammonium hydroxide （TBAH）. The product was characterized by FT-IR, UV, ^1H NMR, ^13C NMR, MS and elemental analysis. Furthermore, the scavenging ability to superoxygen anion radical O2^·- and hydroxyl radical ^·OH was studied by chemiluminescence. It was found that cystine C60 derivative showed an excellent efficiency in eliminating superoxygen anion radical and hydroxyl radical. The 50% inhibition concentration （IC50） for superoxygen anion radical and hydroxyl radical were 0.167 and 0.008 mg/mL, respectively.展开更多
Inclusion complexes between β-cyclodextrin （β-CD） and a series of dicarboxylic acids （DAn, n=11-15） were prepared by co-grinding and co-precipitation methods and the [3]pseudorotaxane structure of them was eluci...Inclusion complexes between β-cyclodextrin （β-CD） and a series of dicarboxylic acids （DAn, n=11-15） were prepared by co-grinding and co-precipitation methods and the [3]pseudorotaxane structure of them was elucidated by FTIR, DTA and XRD characterizations. Inclusion complexes of β-CD and α,ω-alkanedicarboxylate anions （DAn^2-） were acquired by neutralizing β-CD/DAn different inclusion complexes with sodium hydroxide and the structure was also proved to be a pseudorotaxane structure by ^1H-NMR spectra and NOESY spectrum. Both the inclusion complexes of β-CD/DAn and β-CD/DAn^2- adopt the [3]pseudorotaxane structure with β-CD arranged in dimers threaded onto one aliphatic chain and the binding mode of 1：1 inclusion complex was excluded based on the consideration of chain conformations.展开更多
Inclusion of Acyclodextrin (ACD) with phenothiazine 1 and Nalkylpheno-thiazine derivatives (alkyl = ethyl 2, isobutyl 3 and isopentyl 4) in aqueous solution was studied by means of UV-vis spectroscopy. The association...Inclusion of Acyclodextrin (ACD) with phenothiazine 1 and Nalkylpheno-thiazine derivatives (alkyl = ethyl 2, isobutyl 3 and isopentyl 4) in aqueous solution was studied by means of UV-vis spectroscopy. The association constant Ka values for the inclusion of β-CD with 1, 2, 3 and 4 were determined to be 188, 214, 129 and 80 L/mol, respectively. It indicates that the stability of the inclusion complexes is dependent on the structure and the volume of the substituents in the vip compounds.展开更多
Novel highly sensitive chiral organic field-effect transistors(COFET)were developed by directly assembling imidazolium3,5-dimethylphenylcabamoylated-β-cyclodextrin(lm^+-Ph-β-CD)and 3,5-dimethylphenylcarbamoylated-β...Novel highly sensitive chiral organic field-effect transistors(COFET)were developed by directly assembling imidazolium3,5-dimethylphenylcabamoylated-β-cyclodextrin(lm^+-Ph-β-CD)and 3,5-dimethylphenylcarbamoylated-β-CD(Ph-β-CD)respectively onto the semiconductor layer as sensing units.The Im+-Ph-β-CD/COFET afforded better enantioselectivity and a lowest detection concentration of10^-18 L/mol as well as the potentiality in quantitative analysis of commercial medicines.展开更多
A review of methods for the anionic synthesis of well-defined, amine-functionalized polymers using imines as functionalizing agents is provided. The disparate results in the literature regarding functionalizations wit...A review of methods for the anionic synthesis of well-defined, amine-functionalized polymers using imines as functionalizing agents is provided. The disparate results in the literature regarding functionalizations with N -(benzylidene)trimethylsilylamine to form primary amine functionalized polymers are discussed; the efficiency of functionalization depends on the molecular weight of the polymeric organolithium(PLi). Efficient functionalizations are observed for PLi with n>10 000 g/mol. The poor functionalization yields using ketimines with enolizable hydrogens is explained. The use of N -trimethylsilyldiphenylcarbimide as a quantitative primary amine functionalizing reagent is described. Recent results on the anionic synthesis of secondary amine-functionalized polymers using N -(benzylidene)methylamine as the functionalization agent are presented.展开更多
The structural changes of silicate anions in the desilication process with the addition of calcium hydrate alumino-carbonate were studied by measuring Raman spectra, infrared spectra and corresponding second derivativ...The structural changes of silicate anions in the desilication process with the addition of calcium hydrate alumino-carbonate were studied by measuring Raman spectra, infrared spectra and corresponding second derivative spectra. The results show that the desilication ratio in the solution prepared by the addition of sodium silicate(solution-SS) is much greater than that in the solution by the addition of green liquor(solution-GL), and low alumina concentration in the sodium aluminate solutions facilitates the desilication process. It is also shown that alumino-silicate anions in the solution-GL, and Q^3 polymeric silicate anions in solution-SS are predominant, respectively. In addition, increasing the concentration of silica favors respectively the formation of the alumino-silicate or the Q^3 silicate anions in the solution-GL or the solution-SS. Therefore, it can be inferred that the low desilication ratio in the silicate-bearing aluminate solution is mainly attributed to the existence of alumino-silicate anions.展开更多
Inclusion behavior of oxybutynin （OBN） with hydroxypropyl-β-cyclodextrin （HP-β-CD） was investigated by ultraviolet absorption spectrum and fluorescence spectrum. A reliable determination of the complex stoichiom...Inclusion behavior of oxybutynin （OBN） with hydroxypropyl-β-cyclodextrin （HP-β-CD） was investigated by ultraviolet absorption spectrum and fluorescence spectrum. A reliable determination of the complex stoichiometry was provided by the continuous variation technique. Alcohol was added to further investigate the mechanism of the inclusion behavior. Thermodynamic constants AG, AH and AS for inclusion interaction of OBN and HP-β-CD were determined. The results show that host-vip complex with molar ratio of 1：1 is formed, and inclusion stability constant between OBN and HP-β-CD is 54.9 L/mol determined by ultraviolet spectrum and 11.1 L/mol determined by fluorescence spectrum. OBN has weak binding ability with HP-β-CD in aqueous solution （stability constant 〈102 L/mol） and addition of alcohol leads to a decrease of stability constant, which indicates that the hydrophobic force contributes to the inclusion process. AG, AH and AS are all less than zero, which indicates that the inclusion process is a spontaneous and exothermic process.展开更多
Study of molecular recognition has been playing an important role in biomimeticchemistry. β-cyclodextrin (β-CD), the cyclic heptamer of glucopyranose, can form inclusioncomplexes with various types of organic compou...Study of molecular recognition has been playing an important role in biomimeticchemistry. β-cyclodextrin (β-CD), the cyclic heptamer of glucopyranose, can form inclusioncomplexes with various types of organic compounds (substrates) through its展开更多
β-Cyclodextrin （β-CD） and its derivatives functionalized magnetic nanoparticles （MNPs） with high saturated magnetism were fabricated successfully by an effective grafting method. The resultant carboxymethyl/hydr...β-Cyclodextrin （β-CD） and its derivatives functionalized magnetic nanoparticles （MNPs） with high saturated magnetism were fabricated successfully by an effective grafting method. The resultant carboxymethyl/hydroxy- propyl/sulfobutyl ether-β-CD-MNPs （CM/HP/SBE-β-CD-MNPs） nanocomposites were characterized by the TEM, FTIR, DLS, Zeta potential, XRD and VSM. In addition, the loading and release performance of the as-prepared nanocarriers for the hydrophobic anti-cancer drug curcumin was also investigated. The results revealed that the SBE-fl-CD-MNPs possessed the highest loading and release capacity in comparison with other two nanosystems. Cellular uptake and imaging suggested that the SBE-β-CD-MNPs entered into the cell, and curcumin could be suc-cessfully delivered into the cell by SBE-β-CD-MNPs nanocarrier. Moreover, cell toxicity experiments demonstrated the SBE-β-CD-MNPs were non-toxic, while curcumin loaded SBE-β-CD-MNPs showed high potential to kill the HepG2 cells. The as-prepared magnetic composites were expected to expand their potential applications in bio- medical field.展开更多
A new series of bisthiosemicarbazone derivative receptors （1, 2 and 3） have been synthesized by simple steps in good yields. Their anion recognition properties were studied by UV-Vis and ^1H NMR spectroscopy. The re...A new series of bisthiosemicarbazone derivative receptors （1, 2 and 3） have been synthesized by simple steps in good yields. Their anion recognition properties were studied by UV-Vis and ^1H NMR spectroscopy. The result showed that the receptors 1, 2 and 3 all had a better selectivity to F^-, CH3COO^- and H2PO4^-, but no evident binding with Cl^-, Br^-, I^-, NO3^- and HSO4^-. Upon addition of the three anions to the receptors in DMSO, the solution acquired a color change from colorless to dark yellow that can be observed by the naked-eyes, thus the receptors can act as fluoride ion sensors even in the presence of other halide ions. The data showed that it was regular that the three receptors had different binding ability with the three anions. For the same anion, the association constants followed the trend： receptor 1〉3〉2. The UV-Vis data indicates that a 1 ： 1 stoichiometry complex is formed through hydrogen bonding interactions between compound 1, 2 or 3 and anions.展开更多
A series of 8-hydroxyquinoline azo derivatives with diverse conjugated structures were synthesized and studied to chromogenicaUy detect anions.All the dyes allowed selective detection for fluoride anion in CH3CN via i...A series of 8-hydroxyquinoline azo derivatives with diverse conjugated structures were synthesized and studied to chromogenicaUy detect anions.All the dyes allowed selective detection for fluoride anion in CH3CN via instant deprotonation of the compounds,which was affirmed by UV-Vis absorption and 1H NMR spectra.The chromogenically responding ability increases as the substituent changes from phenyl to naphthyl or anthryl.This result is likely to be related to the enhancement of intramolecular charge transfer(ICT)induced by extension of conjugated structure.展开更多
目的建立超高效液相色谱-串联质谱法检测各类动物源性食品中五氯酚残留的方法。方法采用三乙胺-乙腈水提取、混合阴离子交换柱净化,经超高效液相色谱-串联质谱仪检测。研究提取、净化、氮吹、过滤、色谱-质谱分离分析及定性定量等关键...目的建立超高效液相色谱-串联质谱法检测各类动物源性食品中五氯酚残留的方法。方法采用三乙胺-乙腈水提取、混合阴离子交换柱净化,经超高效液相色谱-串联质谱仪检测。研究提取、净化、氮吹、过滤、色谱-质谱分离分析及定性定量等关键控制点,通过优化提取溶剂的比例、去除氮吹浓缩过程,最终建立适用于肌肉(猪肉、牛肉、羊肉、鸡肉)、肝脏(猪肝、牛肝、羊肝、鸡肝)、肾脏(猪肾、牛肾、羊肾、鸡肾)、鱼、虾、蟹、贝类、禽蛋(鸡蛋、鸭蛋、鹅蛋、鹌鹑蛋)、牛奶及奶粉中五氯酚残留量的测定方法。结果五氯酚在0.2~8.0ng/mL质量浓度范围内线性关系良好(r^(2)>0.99),检出限(S/N≥3)为0.3μg/kg,定量限(limits of quantification,LOQ)(S/N≥10)为1.0μg/kg。不同基质在LOQ、2LOQ和10LOQ加标水平的回收率均在64.5%~119.0%,批内、批间相对标准偏差(relative standard deviation,RSD)均小于15%。结论方法操作简单、准确度高、适用性好,可满足不同动物性食品中五氯酚残留量的检测。展开更多
基金The project supported by the National Natural Science Foundation of China(No.20474020).
文摘A novel water-soluble cystine C60 derivative was synthesized in the presence of the catalyst, tetrabutylammonium hydroxide （TBAH）. The product was characterized by FT-IR, UV, ^1H NMR, ^13C NMR, MS and elemental analysis. Furthermore, the scavenging ability to superoxygen anion radical O2^·- and hydroxyl radical ^·OH was studied by chemiluminescence. It was found that cystine C60 derivative showed an excellent efficiency in eliminating superoxygen anion radical and hydroxyl radical. The 50% inhibition concentration （IC50） for superoxygen anion radical and hydroxyl radical were 0.167 and 0.008 mg/mL, respectively.
文摘Inclusion complexes between β-cyclodextrin （β-CD） and a series of dicarboxylic acids （DAn, n=11-15） were prepared by co-grinding and co-precipitation methods and the [3]pseudorotaxane structure of them was elucidated by FTIR, DTA and XRD characterizations. Inclusion complexes of β-CD and α,ω-alkanedicarboxylate anions （DAn^2-） were acquired by neutralizing β-CD/DAn different inclusion complexes with sodium hydroxide and the structure was also proved to be a pseudorotaxane structure by ^1H-NMR spectra and NOESY spectrum. Both the inclusion complexes of β-CD/DAn and β-CD/DAn^2- adopt the [3]pseudorotaxane structure with β-CD arranged in dimers threaded onto one aliphatic chain and the binding mode of 1：1 inclusion complex was excluded based on the consideration of chain conformations.
文摘Inclusion of Acyclodextrin (ACD) with phenothiazine 1 and Nalkylpheno-thiazine derivatives (alkyl = ethyl 2, isobutyl 3 and isopentyl 4) in aqueous solution was studied by means of UV-vis spectroscopy. The association constant Ka values for the inclusion of β-CD with 1, 2, 3 and 4 were determined to be 188, 214, 129 and 80 L/mol, respectively. It indicates that the stability of the inclusion complexes is dependent on the structure and the volume of the substituents in the vip compounds.
基金financially supported by the National Natural Science Foundation of China (No.21575100)Tianjin Research Program of Application Foundation and Advanced Technology (Nos.18JCZDJC37500,17JCYBJC20500)
文摘Novel highly sensitive chiral organic field-effect transistors(COFET)were developed by directly assembling imidazolium3,5-dimethylphenylcabamoylated-β-cyclodextrin(lm^+-Ph-β-CD)and 3,5-dimethylphenylcarbamoylated-β-CD(Ph-β-CD)respectively onto the semiconductor layer as sensing units.The Im+-Ph-β-CD/COFET afforded better enantioselectivity and a lowest detection concentration of10^-18 L/mol as well as the potentiality in quantitative analysis of commercial medicines.
文摘A review of methods for the anionic synthesis of well-defined, amine-functionalized polymers using imines as functionalizing agents is provided. The disparate results in the literature regarding functionalizations with N -(benzylidene)trimethylsilylamine to form primary amine functionalized polymers are discussed; the efficiency of functionalization depends on the molecular weight of the polymeric organolithium(PLi). Efficient functionalizations are observed for PLi with n>10 000 g/mol. The poor functionalization yields using ketimines with enolizable hydrogens is explained. The use of N -trimethylsilyldiphenylcarbimide as a quantitative primary amine functionalizing reagent is described. Recent results on the anionic synthesis of secondary amine-functionalized polymers using N -(benzylidene)methylamine as the functionalization agent are presented.
基金Project(51274242)supported by the National Natural Science Foundation of ChinaProject(2015CX001)supported by the Innovation-driven Plan in Central South University,China
文摘The structural changes of silicate anions in the desilication process with the addition of calcium hydrate alumino-carbonate were studied by measuring Raman spectra, infrared spectra and corresponding second derivative spectra. The results show that the desilication ratio in the solution prepared by the addition of sodium silicate(solution-SS) is much greater than that in the solution by the addition of green liquor(solution-GL), and low alumina concentration in the sodium aluminate solutions facilitates the desilication process. It is also shown that alumino-silicate anions in the solution-GL, and Q^3 polymeric silicate anions in solution-SS are predominant, respectively. In addition, increasing the concentration of silica favors respectively the formation of the alumino-silicate or the Q^3 silicate anions in the solution-GL or the solution-SS. Therefore, it can be inferred that the low desilication ratio in the silicate-bearing aluminate solution is mainly attributed to the existence of alumino-silicate anions.
基金Project(20976041) supported by the National Natural Science Foundation of China
文摘Inclusion behavior of oxybutynin （OBN） with hydroxypropyl-β-cyclodextrin （HP-β-CD） was investigated by ultraviolet absorption spectrum and fluorescence spectrum. A reliable determination of the complex stoichiometry was provided by the continuous variation technique. Alcohol was added to further investigate the mechanism of the inclusion behavior. Thermodynamic constants AG, AH and AS for inclusion interaction of OBN and HP-β-CD were determined. The results show that host-vip complex with molar ratio of 1：1 is formed, and inclusion stability constant between OBN and HP-β-CD is 54.9 L/mol determined by ultraviolet spectrum and 11.1 L/mol determined by fluorescence spectrum. OBN has weak binding ability with HP-β-CD in aqueous solution （stability constant 〈102 L/mol） and addition of alcohol leads to a decrease of stability constant, which indicates that the hydrophobic force contributes to the inclusion process. AG, AH and AS are all less than zero, which indicates that the inclusion process is a spontaneous and exothermic process.
文摘Study of molecular recognition has been playing an important role in biomimeticchemistry. β-cyclodextrin (β-CD), the cyclic heptamer of glucopyranose, can form inclusioncomplexes with various types of organic compounds (substrates) through its
文摘β-Cyclodextrin （β-CD） and its derivatives functionalized magnetic nanoparticles （MNPs） with high saturated magnetism were fabricated successfully by an effective grafting method. The resultant carboxymethyl/hydroxy- propyl/sulfobutyl ether-β-CD-MNPs （CM/HP/SBE-β-CD-MNPs） nanocomposites were characterized by the TEM, FTIR, DLS, Zeta potential, XRD and VSM. In addition, the loading and release performance of the as-prepared nanocarriers for the hydrophobic anti-cancer drug curcumin was also investigated. The results revealed that the SBE-fl-CD-MNPs possessed the highest loading and release capacity in comparison with other two nanosystems. Cellular uptake and imaging suggested that the SBE-β-CD-MNPs entered into the cell, and curcumin could be suc-cessfully delivered into the cell by SBE-β-CD-MNPs nanocarrier. Moreover, cell toxicity experiments demonstrated the SBE-β-CD-MNPs were non-toxic, while curcumin loaded SBE-β-CD-MNPs showed high potential to kill the HepG2 cells. The as-prepared magnetic composites were expected to expand their potential applications in bio- medical field.
基金Project supported by the Natural Science Foundation of China （No. 20371040）, the Key Chinese Project of Ministry of Education （No. 205161 ） and the Foundation of Gansu Province （No. 3YS051-A25-010）.
文摘A new series of bisthiosemicarbazone derivative receptors （1, 2 and 3） have been synthesized by simple steps in good yields. Their anion recognition properties were studied by UV-Vis and ^1H NMR spectroscopy. The result showed that the receptors 1, 2 and 3 all had a better selectivity to F^-, CH3COO^- and H2PO4^-, but no evident binding with Cl^-, Br^-, I^-, NO3^- and HSO4^-. Upon addition of the three anions to the receptors in DMSO, the solution acquired a color change from colorless to dark yellow that can be observed by the naked-eyes, thus the receptors can act as fluoride ion sensors even in the presence of other halide ions. The data showed that it was regular that the three receptors had different binding ability with the three anions. For the same anion, the association constants followed the trend： receptor 1〉3〉2. The UV-Vis data indicates that a 1 ： 1 stoichiometry complex is formed through hydrogen bonding interactions between compound 1, 2 or 3 and anions.
基金Project supported by the National Science Foundation of China(Nos.20490210,20501006)the Shanghai Science Technology Foundation(No.05DJ 14004).
文摘A series of 8-hydroxyquinoline azo derivatives with diverse conjugated structures were synthesized and studied to chromogenicaUy detect anions.All the dyes allowed selective detection for fluoride anion in CH3CN via instant deprotonation of the compounds,which was affirmed by UV-Vis absorption and 1H NMR spectra.The chromogenically responding ability increases as the substituent changes from phenyl to naphthyl or anthryl.This result is likely to be related to the enhancement of intramolecular charge transfer(ICT)induced by extension of conjugated structure.
文摘目的建立超高效液相色谱-串联质谱法检测各类动物源性食品中五氯酚残留的方法。方法采用三乙胺-乙腈水提取、混合阴离子交换柱净化,经超高效液相色谱-串联质谱仪检测。研究提取、净化、氮吹、过滤、色谱-质谱分离分析及定性定量等关键控制点,通过优化提取溶剂的比例、去除氮吹浓缩过程,最终建立适用于肌肉(猪肉、牛肉、羊肉、鸡肉)、肝脏(猪肝、牛肝、羊肝、鸡肝)、肾脏(猪肾、牛肾、羊肾、鸡肾)、鱼、虾、蟹、贝类、禽蛋(鸡蛋、鸭蛋、鹅蛋、鹌鹑蛋)、牛奶及奶粉中五氯酚残留量的测定方法。结果五氯酚在0.2~8.0ng/mL质量浓度范围内线性关系良好(r^(2)>0.99),检出限(S/N≥3)为0.3μg/kg,定量限(limits of quantification,LOQ)(S/N≥10)为1.0μg/kg。不同基质在LOQ、2LOQ和10LOQ加标水平的回收率均在64.5%~119.0%,批内、批间相对标准偏差(relative standard deviation,RSD)均小于15%。结论方法操作简单、准确度高、适用性好,可满足不同动物性食品中五氯酚残留量的检测。
