The triphenyltin complex with salicylidene-2-aminophenol （C31H24NO2Sn, 1） has been synthesized and characterized by elemental analysis, IR spectroscopy, thermogravimetric analysis, and X-ray single-crystal diffracti...The triphenyltin complex with salicylidene-2-aminophenol （C31H24NO2Sn, 1） has been synthesized and characterized by elemental analysis, IR spectroscopy, thermogravimetric analysis, and X-ray single-crystal diffraction. The complex crystallizes in monoclinic system, P21/c space group with a = 1.09515（8）, b = 1.17739（8）, c = 2.29075（14） nm, β = 117.070（4）°, V = 2.6302（3） nm3, Z = 4, Dc = 1.417 g/cm3, ？ = 0.999 mm–1, F（000） = 1123, R = 0.0472 and wR = 0.1169. X-ray single-crystal diffraction showed that 1 demonstrates a one-dimensional chain structure. The quantum chemical calculation of 1 has been investigated. Complex 1 emits fluo- rescence at 558 nm and exhibits certain inhibitory activity against NCI-H460, A549 and MCF-7.展开更多
The production of Ph3Sn–O–SBA-15(Ph3Sn SBA)was achieved by heating triphenyltin chloride and SBA-15in N-methylpyrrolidone at 190°C for 5 h using triethylamine as a catalyst.The composition,structure,and surface...The production of Ph3Sn–O–SBA-15(Ph3Sn SBA)was achieved by heating triphenyltin chloride and SBA-15in N-methylpyrrolidone at 190°C for 5 h using triethylamine as a catalyst.The composition,structure,and surface physical and chemical properties of Ph3Sn SBA were characterized using inductively coupled plasma-atomic emission spectroscopy(ICP-AES),13C,119Sn and29Si solid-state nuclear magnetic resonance(NMR)spectroscopy in situ pyridine infrared spectroscopy(Py-IR),N2adsorption–desorption isotherms,X-ray diffraction(XRD)and transmission electron microscopy(TEM).The results of ICP-AES and organic elemental analysis showed that the grafting yield of Sn was 17%(by mass)for Ph3Sn SBA.The elemental analysis and solid-state NMR results for Ph3Sn SBA were consistent with grafting of triphenyltin on SBA-15.The N2adsorption–desorption,XRD and TEM analyses showed that Ph3Sn SBA retained an ordered hexagonal mesoporous structure,resulting in decreases in the surface area,pore size and mesopore volume,and an increase in acidity as compared with SBA-15.The Hammett acidity function(H0)value and the number of acid sites for Ph3Sn SBA,obtained by the Hammett methods,were 2.77–3.30 and 2.07 mmol·g-1,respectively.The Friedel–Crafts acylation of toluene and acetic anhydride over Ph3Sn SBA was investigated.The yield of methylacetophenone(MAP)and the selectivity for 4-methylacetophenone(PMAP)were 79.56%and 97.12%,respectively,when the conditions were n(toluene):n(anhydride)=2.0:1.0 with 6%(by mass)catalyst,and heating under reflux for 5 h.The PMAP selectivity still reached 93.11%when Ph3Sn SBA was used for the fifth time under the same reaction conditions.展开更多
A rapid, precise, sensitive and simple method has been developed for the extraction and determination of TPT （triphenyltin）, DPT （diphenyltin） and MPT （monophenyltin） in seawater samples. The procedure is based ...A rapid, precise, sensitive and simple method has been developed for the extraction and determination of TPT （triphenyltin）, DPT （diphenyltin） and MPT （monophenyltin） in seawater samples. The procedure is based on the use of the dual functionalization of mesoporous silica with diol and Cl6 alkane groups for the collection of TPT and its derivatives, DPT and MPT, from seawater samples, followed by ethylation of the target matrices using sodium tetraethylborate （NaBEt4） and quantification by gas chromatography with pulsed flame photometric detection. The modified extraction method replaces conventional solid- and liquid-phase extraction with solid dispersion of silica nanoparticles. The partitioning of the analyte between a carefully size-selected silica nanoparticles （solid phase） and a liquid phase occurs as the solid moves through the sample as a colloidal sol. By tailoring the size of the particles to approximately 250 nm in diameter, they can be easily dispersed in aqueous solution, without the need for any mechanical or hand shaking and the solid can then be readily recovered, together with the analytes, by simple filtration or centrifugation. Recoveries of TPT, DPT and MPT chloride spiked matrices rang from 87.3±1.1 to 98.1±1.3 in seawater samples （n = I 1 samples）. The limit of detection obtained was typically in the range of 0.1-3 ng Sn/L. The proposed method shows excellent linearity in the range of 0.5-2 ng Sn/L and good repeatability （RSD 〈 5% at 0.02 ng TPT （as Sn）/L）. The method performance is demonstrated with real seawater samples.展开更多
Triphenyltin thiazole-2-carboxylate (1) and triphenyltin 3-pyridinylcarboxylate (2) were synthesized by the reaction of sodium thiazole-2-carboxylate or sodium 3-pyridinylcarboxylate with the triphenyltin chloride and...Triphenyltin thiazole-2-carboxylate (1) and triphenyltin 3-pyridinylcarboxylate (2) were synthesized by the reaction of sodium thiazole-2-carboxylate or sodium 3-pyridinylcarboxylate with the triphenyltin chloride and their crystal structures were determined by single crystal X-ray diffraction analysis. In the structure of 1, the tin atom is five-coordinated in a distorted trigonal bipyramidal structure. Due to the presence of a close intermolecular Sn...S interaction distance of 0.3666 nm, the structure can be described as a weakly-bridged one-dimensional chain compound. In the structure of 2, the tin atom is five-coordinated with bridging 3-pyridinylcarboxylate ligands N atom and resulting structure is one-dimensional chain compound.展开更多
Xenopus tropicalis embryos were exposed for 48 hr to the mixtures of 5 μg Sn/L triphenyltin （TPT）, which is a well-known endocrine disruptor, and 0.25-5 μg/L 9-cis retinoic acid （9c-RA）, which is the natural lig...Xenopus tropicalis embryos were exposed for 48 hr to the mixtures of 5 μg Sn/L triphenyltin （TPT）, which is a well-known endocrine disruptor, and 0.25-5 μg/L 9-cis retinoic acid （9c-RA）, which is the natural ligand of retinoid X receptor. The phenotypes induced by combined exposure were more variable than those resulting from single exposure to either TPT or 9c-RA. The prominent phenotypes included underdeveloped head structures, abnormal eyes, narrow fins, enlarged proctodaeum, etc. Especially, combined exposure induced unexpected notochord malformations, which ranged from small swellings of the surface of the tails to the extension and extrusion of notochord out of the posterior tails. Compared with the 5 μg Sn/L TPT-treated group, the index of fin deficiency was not affected, and the index of axis deficiency was significantly increased with increasing RA concentrations in the mixtures. Our results suggest that combined exposure to TPT and 9c-RA induced not only more variable phenotypes of malformations than exposure to single compound but also some new and unexpected phenotypes.展开更多
Triphenyltin (TPT) widely exists as environmental pollutant, but its toxicity towards nerve cells and the related mechanism remain unclear. In this research, SHSY-5Y cells were exposed to TPT, and the cellular proteas...Triphenyltin (TPT) widely exists as environmental pollutant, but its toxicity towards nerve cells and the related mechanism remain unclear. In this research, SHSY-5Y cells were exposed to TPT, and the cellular proteasome activity, Iκb proteins, Bax and α-synuclein levels were investigated. The results show that TPT can inhibit the cellular proteasome activity, and result in the accumulation of ubiquitinized proteins. TPT exposure can change the protein levels of IκB, Bax, and α-synuclein, affect NFκB pathway, activate the process of cell death, and induce α-synuclein aggregation. Our results indicate that TPT exposure can lead to neuotoxicity.展开更多
基金Supported by the Open Fund Project of Key Laboratory of Functional Organometallic Materials of Hengyang Normal University(15K017,14K014,13K105)Natural Science Foundation of Hunan Province(No.13JJ3112)+3 种基金Scientific&Technological Projects of Hunan Province(No.2014NK3086)Aid programs for Science and Technology Innovative Research Team in Higher Educational Institutions of Hunan Provincethe Key Discipline of Hunan ProvinceProject funding for research and innovation experiment of university students in Hunan Province
文摘The triphenyltin complex with salicylidene-2-aminophenol （C31H24NO2Sn, 1） has been synthesized and characterized by elemental analysis, IR spectroscopy, thermogravimetric analysis, and X-ray single-crystal diffraction. The complex crystallizes in monoclinic system, P21/c space group with a = 1.09515（8）, b = 1.17739（8）, c = 2.29075（14） nm, β = 117.070（4）°, V = 2.6302（3） nm3, Z = 4, Dc = 1.417 g/cm3, ？ = 0.999 mm–1, F（000） = 1123, R = 0.0472 and wR = 0.1169. X-ray single-crystal diffraction showed that 1 demonstrates a one-dimensional chain structure. The quantum chemical calculation of 1 has been investigated. Complex 1 emits fluo- rescence at 558 nm and exhibits certain inhibitory activity against NCI-H460, A549 and MCF-7.
基金Supported by the National Science Foundation of Heilongjiang Province(B201010)the Education Department of Heilongjiang Province(12511595)
文摘The production of Ph3Sn–O–SBA-15(Ph3Sn SBA)was achieved by heating triphenyltin chloride and SBA-15in N-methylpyrrolidone at 190°C for 5 h using triethylamine as a catalyst.The composition,structure,and surface physical and chemical properties of Ph3Sn SBA were characterized using inductively coupled plasma-atomic emission spectroscopy(ICP-AES),13C,119Sn and29Si solid-state nuclear magnetic resonance(NMR)spectroscopy in situ pyridine infrared spectroscopy(Py-IR),N2adsorption–desorption isotherms,X-ray diffraction(XRD)and transmission electron microscopy(TEM).The results of ICP-AES and organic elemental analysis showed that the grafting yield of Sn was 17%(by mass)for Ph3Sn SBA.The elemental analysis and solid-state NMR results for Ph3Sn SBA were consistent with grafting of triphenyltin on SBA-15.The N2adsorption–desorption,XRD and TEM analyses showed that Ph3Sn SBA retained an ordered hexagonal mesoporous structure,resulting in decreases in the surface area,pore size and mesopore volume,and an increase in acidity as compared with SBA-15.The Hammett acidity function(H0)value and the number of acid sites for Ph3Sn SBA,obtained by the Hammett methods,were 2.77–3.30 and 2.07 mmol·g-1,respectively.The Friedel–Crafts acylation of toluene and acetic anhydride over Ph3Sn SBA was investigated.The yield of methylacetophenone(MAP)and the selectivity for 4-methylacetophenone(PMAP)were 79.56%and 97.12%,respectively,when the conditions were n(toluene):n(anhydride)=2.0:1.0 with 6%(by mass)catalyst,and heating under reflux for 5 h.The PMAP selectivity still reached 93.11%when Ph3Sn SBA was used for the fifth time under the same reaction conditions.
文摘A rapid, precise, sensitive and simple method has been developed for the extraction and determination of TPT （triphenyltin）, DPT （diphenyltin） and MPT （monophenyltin） in seawater samples. The procedure is based on the use of the dual functionalization of mesoporous silica with diol and Cl6 alkane groups for the collection of TPT and its derivatives, DPT and MPT, from seawater samples, followed by ethylation of the target matrices using sodium tetraethylborate （NaBEt4） and quantification by gas chromatography with pulsed flame photometric detection. The modified extraction method replaces conventional solid- and liquid-phase extraction with solid dispersion of silica nanoparticles. The partitioning of the analyte between a carefully size-selected silica nanoparticles （solid phase） and a liquid phase occurs as the solid moves through the sample as a colloidal sol. By tailoring the size of the particles to approximately 250 nm in diameter, they can be easily dispersed in aqueous solution, without the need for any mechanical or hand shaking and the solid can then be readily recovered, together with the analytes, by simple filtration or centrifugation. Recoveries of TPT, DPT and MPT chloride spiked matrices rang from 87.3±1.1 to 98.1±1.3 in seawater samples （n = I 1 samples）. The limit of detection obtained was typically in the range of 0.1-3 ng Sn/L. The proposed method shows excellent linearity in the range of 0.5-2 ng Sn/L and good repeatability （RSD 〈 5% at 0.02 ng TPT （as Sn）/L）. The method performance is demonstrated with real seawater samples.
基金ProjectsupportedbytheNaturalScienceFoundationofShandongProvince (No .Z2 0 0 1B0 2 )andtheFoundationofStateKeyLaborato ryofCrystalMaterials,ShandongUniversity
文摘Triphenyltin thiazole-2-carboxylate (1) and triphenyltin 3-pyridinylcarboxylate (2) were synthesized by the reaction of sodium thiazole-2-carboxylate or sodium 3-pyridinylcarboxylate with the triphenyltin chloride and their crystal structures were determined by single crystal X-ray diffraction analysis. In the structure of 1, the tin atom is five-coordinated in a distorted trigonal bipyramidal structure. Due to the presence of a close intermolecular Sn...S interaction distance of 0.3666 nm, the structure can be described as a weakly-bridged one-dimensional chain compound. In the structure of 2, the tin atom is five-coordinated with bridging 3-pyridinylcarboxylate ligands N atom and resulting structure is one-dimensional chain compound.
基金supported by the National Natural Science Foundation of China(No.21277049)the State Key Laboratory of Estuarine and Coastal Research(No.2012KYYW04)
文摘Xenopus tropicalis embryos were exposed for 48 hr to the mixtures of 5 μg Sn/L triphenyltin （TPT）, which is a well-known endocrine disruptor, and 0.25-5 μg/L 9-cis retinoic acid （9c-RA）, which is the natural ligand of retinoid X receptor. The phenotypes induced by combined exposure were more variable than those resulting from single exposure to either TPT or 9c-RA. The prominent phenotypes included underdeveloped head structures, abnormal eyes, narrow fins, enlarged proctodaeum, etc. Especially, combined exposure induced unexpected notochord malformations, which ranged from small swellings of the surface of the tails to the extension and extrusion of notochord out of the posterior tails. Compared with the 5 μg Sn/L TPT-treated group, the index of fin deficiency was not affected, and the index of axis deficiency was significantly increased with increasing RA concentrations in the mixtures. Our results suggest that combined exposure to TPT and 9c-RA induced not only more variable phenotypes of malformations than exposure to single compound but also some new and unexpected phenotypes.
基金supported by the National Natural Science Foundation of China (Grant No 20677068)State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sci-ences, Chinese Academy of Sciences (Grant No KF-2008-12)
文摘Triphenyltin (TPT) widely exists as environmental pollutant, but its toxicity towards nerve cells and the related mechanism remain unclear. In this research, SHSY-5Y cells were exposed to TPT, and the cellular proteasome activity, Iκb proteins, Bax and α-synuclein levels were investigated. The results show that TPT can inhibit the cellular proteasome activity, and result in the accumulation of ubiquitinized proteins. TPT exposure can change the protein levels of IκB, Bax, and α-synuclein, affect NFκB pathway, activate the process of cell death, and induce α-synuclein aggregation. Our results indicate that TPT exposure can lead to neuotoxicity.
