建立了超高效液相色谱-串联质谱检测枳实药材中辛弗林、N-甲基酪胺的方法。以甲醇为提取溶剂,经QuECHERS分散净化,采用资生堂CAPCELL PAK CR色谱柱(150mm×2.0mm,5μm;C_(18)和SCX比例为1∶4)分离,质谱以正离子扫描,反应监测模式测...建立了超高效液相色谱-串联质谱检测枳实药材中辛弗林、N-甲基酪胺的方法。以甲醇为提取溶剂,经QuECHERS分散净化,采用资生堂CAPCELL PAK CR色谱柱(150mm×2.0mm,5μm;C_(18)和SCX比例为1∶4)分离,质谱以正离子扫描,反应监测模式测定。辛弗林和N-甲基酪胺在10~2000ng/mL范围内线性关系良好(R^(2)>0.997),检出限和定量限分别为0.3ng/mL和1.0ng/mL,回收率范围为94.3%~105.7%,相对标准偏差(RSD)均小于3%。该方法避免了使用磷酸盐和离子对试剂,仅在流动相中添加甲酸和甲酸铵,分析物就能有较好的保留,具有极高的质谱响应。相较于传统方法,该方法分析时间短、操作简单、专属性强,在强极性生物碱分离检测方面具有较好的应用价值。展开更多
Novel dual-responsive superhydrophobic hybrid materials, ZnO/SAMs （self-assembled monolayers） of ionic liquids （ILs） with different counter-anions （I^-, BF4^-, PF6^- and Tf2N^-）, were synthesized and characteriz...Novel dual-responsive superhydrophobic hybrid materials, ZnO/SAMs （self-assembled monolayers） of ionic liquids （ILs） with different counter-anions （I^-, BF4^-, PF6^- and Tf2N^-）, were synthesized and characterized. ZnO nanoparticles were first deposited on glass surfaces to produce roughness. Next, SAMs of fluorinated-alkyl-3-（3-triethoxysilylpropyl）-4,5-dihydro-imidazoliumiodide （abb. [C8Ftespim]I） were grafted onto these surfaces via -Si-O- covalent bonds using self-assembly technique. The I- ion could be subsequently exchanged with BF4, PF6-or Tf2N- through a simple aqueous anion-exchange reaction. The ZnO/ILs hybrid layers were characterized by atomic-force microscopy （AFM）, scanning-electron microscopy （SEM） and X-ray photoelectron spectroscopy （XPS）. Their wettability was estimated through the measurements of static and dynamic contact angles （CAs）. Compared to corresponding films of ZnO/[CsFtespim]I with CAs 140.7° ±2.0°, films of ZnO/[CsFtespim]PF6 and ZnO/[CsFtespim]Tf2N showed CAs with 154.0° ± 2.0° and 152.0° ± 2.0°, respectively that remained for a long time. This result suggests that anion-exchange can afford superhydrophobic materials. In addition, the wettability of ZnO/[CsFtespim]X hybrid layers can be reversibly switched by altering ultraviolet （UV） irradiation and dark storage, which shows a photo-induced reversible switch of wettability. The synergistic action of ZnO nanoparticles and SAMs of ILs produced light-anion dual-responsive superhydrophobic materials with ideal stability.展开更多
A new polymeric nanocomposite photocatalyst A15-CdS with large spherical beads (0.70-0.80 mm in diameter) was fabricated for efficient Rhodamine B (RhB) photodegradation with facile separation during cyclic runs,and p...A new polymeric nanocomposite photocatalyst A15-CdS with large spherical beads (0.70-0.80 mm in diameter) was fabricated for efficient Rhodamine B (RhB) photodegradation with facile separation during cyclic runs,and photocorrosion,a congenital drawback of CdS,was successfully inhibited for A15-CdS.The nanocomposite catalyst was obtained by impregnating CdS nanoparticles within porous polymeric cation exchanger A15 through a facile inner-surface deposition.CdS nanoparticles (<20 nm) immobilized in A15 were deliberately distributed within an outside ring-like region of 40-50 m in depth,which is dominant for photoreaction because visible light is not expected to permeate through the inner region of nontransparent A15.As expected,efficient RhB photodegradation by A15-CdS was achieved under visible light irradiation,and large-size A15-CdS beads are expected to result in their facile separation from solution for repeated use.More significantly,negligible photocorrosion for the hybrid catalyst A15-CdS was demonstrated by the constant photodegradation efficiency and negligible CdS loss during five-cycle runs.The results indicated that nano-CdS immobilization within A15 would greatly improve the applicability of CdS nanoparticles in practical environmental remediation.展开更多
文摘建立了超高效液相色谱-串联质谱检测枳实药材中辛弗林、N-甲基酪胺的方法。以甲醇为提取溶剂,经QuECHERS分散净化,采用资生堂CAPCELL PAK CR色谱柱(150mm×2.0mm,5μm;C_(18)和SCX比例为1∶4)分离,质谱以正离子扫描,反应监测模式测定。辛弗林和N-甲基酪胺在10~2000ng/mL范围内线性关系良好(R^(2)>0.997),检出限和定量限分别为0.3ng/mL和1.0ng/mL,回收率范围为94.3%~105.7%,相对标准偏差(RSD)均小于3%。该方法避免了使用磷酸盐和离子对试剂,仅在流动相中添加甲酸和甲酸铵,分析物就能有较好的保留,具有极高的质谱响应。相较于传统方法,该方法分析时间短、操作简单、专属性强,在强极性生物碱分离检测方面具有较好的应用价值。
基金financially supported by the National Natural Science Foundation of China(21033005,21273134)the National Basic Research Program of China(2009CB930103)+2 种基金the Natural Science Foundation of Shandong Province(Combination Research Projects,ZR2013EML003&ZR2013BL001)National Undergraduate Training Programs for Innovation and Entrepreneurship(201310448008)Research Projects of Solar Energy of Dezhou University(311416&SYJS-B13003)
文摘Novel dual-responsive superhydrophobic hybrid materials, ZnO/SAMs （self-assembled monolayers） of ionic liquids （ILs） with different counter-anions （I^-, BF4^-, PF6^- and Tf2N^-）, were synthesized and characterized. ZnO nanoparticles were first deposited on glass surfaces to produce roughness. Next, SAMs of fluorinated-alkyl-3-（3-triethoxysilylpropyl）-4,5-dihydro-imidazoliumiodide （abb. [C8Ftespim]I） were grafted onto these surfaces via -Si-O- covalent bonds using self-assembly technique. The I- ion could be subsequently exchanged with BF4, PF6-or Tf2N- through a simple aqueous anion-exchange reaction. The ZnO/ILs hybrid layers were characterized by atomic-force microscopy （AFM）, scanning-electron microscopy （SEM） and X-ray photoelectron spectroscopy （XPS）. Their wettability was estimated through the measurements of static and dynamic contact angles （CAs）. Compared to corresponding films of ZnO/[CsFtespim]I with CAs 140.7° ±2.0°, films of ZnO/[CsFtespim]PF6 and ZnO/[CsFtespim]Tf2N showed CAs with 154.0° ± 2.0° and 152.0° ± 2.0°, respectively that remained for a long time. This result suggests that anion-exchange can afford superhydrophobic materials. In addition, the wettability of ZnO/[CsFtespim]X hybrid layers can be reversibly switched by altering ultraviolet （UV） irradiation and dark storage, which shows a photo-induced reversible switch of wettability. The synergistic action of ZnO nanoparticles and SAMs of ILs produced light-anion dual-responsive superhydrophobic materials with ideal stability.
基金support from the National Natural Science Foundation of China (51008151 & 51078179)Jiangsu Natural Science Foundation (BK2009253)+1 种基金the Ministry of Education of China (200802840034)the National High Technology Research and Development Program of China (2009AA06A418)
文摘A new polymeric nanocomposite photocatalyst A15-CdS with large spherical beads (0.70-0.80 mm in diameter) was fabricated for efficient Rhodamine B (RhB) photodegradation with facile separation during cyclic runs,and photocorrosion,a congenital drawback of CdS,was successfully inhibited for A15-CdS.The nanocomposite catalyst was obtained by impregnating CdS nanoparticles within porous polymeric cation exchanger A15 through a facile inner-surface deposition.CdS nanoparticles (<20 nm) immobilized in A15 were deliberately distributed within an outside ring-like region of 40-50 m in depth,which is dominant for photoreaction because visible light is not expected to permeate through the inner region of nontransparent A15.As expected,efficient RhB photodegradation by A15-CdS was achieved under visible light irradiation,and large-size A15-CdS beads are expected to result in their facile separation from solution for repeated use.More significantly,negligible photocorrosion for the hybrid catalyst A15-CdS was demonstrated by the constant photodegradation efficiency and negligible CdS loss during five-cycle runs.The results indicated that nano-CdS immobilization within A15 would greatly improve the applicability of CdS nanoparticles in practical environmental remediation.
