3-bromo-4,5-bis（2,3-dibromo-4,5-dihydroxybenzyl）-l,2-benzenediol （1） is a natural bromophenol isolated from the red algae Rhodomela confervoides that exhibits significant inhibition against protein tyrosine phosph...3-bromo-4,5-bis（2,3-dibromo-4,5-dihydroxybenzyl）-l,2-benzenediol （1） is a natural bromophenol isolated from the red algae Rhodomela confervoides that exhibits significant inhibition against protein tyrosine phosphatase 1B （PTP1B）. Based on its activity, we synthesized two new synthetic bromophenols and their methoxy derivatives from vanillin using the structure of natural bromophenol 1 as a scaffold. The structures of these bromophenols were elucidated from H NMR, 13C NMR, and high resolution electron ionization mass spectrometry as 2,3-dibromo-1-（2＇-bromo-6＇-（3＂,4＂-dimethoxybenzyl）- 3 ＇,4 ＇-dimethoxybenzyl）-4,5 -dimethoxybenzene （2）, 2,3-dibromo- 1 -（2 ＇-bromo-6＇-（2 ＂-bromo-4＂,5 ＂-dimethoxy- benzyl）-3＇,4＇-dimethoxybenzyl）-4,5-dimethoxybenzene （3）, 3,4-dibromo-5-（2＇-bromo-6＇-（2＂-bromo-4＂,5＂- dihydroxybenzyl）-3＇,4＇-dihydroxybenzyl）pyrocatechol （4） and 3,4-dibromo-5-（2＇-bromo-6＇-（3＂,4＂- dihydroxybenzyl）-3＇,4＇-dihydroxybenzyl）pyrocatechol （5）. PTP1B inhibition activities of these compounds were evaluated using a colorimetric assay, and compounds 3 and 4 demonstrated interesting activity against PTP1B.展开更多
The bromine （Br） and iodine （I） in raw coal, bottom ash （BA） and fly ash （FA） from seven thermal power plants （TPP） digested with pyrohydrolysis were determined by using inductively coupled plasma mass spect...The bromine （Br） and iodine （I） in raw coal, bottom ash （BA） and fly ash （FA） from seven thermal power plants （TPP） digested with pyrohydrolysis were determined by using inductively coupled plasma mass spectrometry （ICP-MS）. The distribution behavior of Br and I during coal combustion were researched and the environmental effects of Br and I in BA, FA and gas phase were analyzed. The results show that both elements Br and I in combustion products from TPP are usually pre- sent in decreasing order of the distribution rate as gas phase, FA and BA. In FA and BA, the distribution rate of Br （8.11% and 1.68%, respectively） are generally lower than that of I （9.26% and 4.67%, respectively）; on the contrary, in gas phase, the former （90.2%） is higher than the latter （86.9%）. In addition, for gas phase, the percentage of Br： （2.0%-75%） in total Br is generally larger than that of I2 （1.0%-10%） in total I. The environmental effects for Br and I emitted into atmosphere from TPP may be larger than those remained and captured by both FA and BA.展开更多
An analytical method, using sector field inductively coupled plasma mass spectrometry （SF-ICP-MS） for rapid simultaneous determination of Be, Na, Mg, Si, Ca, Ti, V, Cr, Fe, Co, Ni, Cu, Zn, As, Sn, Sb, Pb and Bi in e...An analytical method, using sector field inductively coupled plasma mass spectrometry （SF-ICP-MS） for rapid simultaneous determination of Be, Na, Mg, Si, Ca, Ti, V, Cr, Fe, Co, Ni, Cu, Zn, As, Sn, Sb, Pb and Bi in electrolytic manganese metal, was described. At the beginning, the samples were decomposed by HNO3 and H2504, and then analyzed by SF-ICP-MS. Most of the spectral interferences could be avoided by measuring in different mass resolution modes. The matrix effects due to the excess of sulfuric acid and Mn were evaluated. Correction of matrix effects was conducted by using the internal standard elements. The optimum condition for the determination was investigated and discussed. The detection limit is in the range of 0.001-0.169 gg/L. The current method is applied to the determination of trace impurities in electrolytic manganese metal. And experiments show that good results can be obtained much faster, more accurately and conveniently by current method.展开更多
We collected eleven bench samples of No. 6 coal from the Heidaigou Surface Mine, Jungar Coalfield, Inner Mongolia, China, and four samples from the affiliated coal preparation plant. Based on these samples, we used in...We collected eleven bench samples of No. 6 coal from the Heidaigou Surface Mine, Jungar Coalfield, Inner Mongolia, China, and four samples from the affiliated coal preparation plant. Based on these samples, we used inductively coupled-plasma mass spectroscopy, X-ray diffraction, scanning electron microscope with an energy-dispersive X-ray spectrometer techniques, and borehole exploration data, to investigate the distribution, occurrence and enrichment causes of gallium （Ga） in the coals. Our results show： （1） Gallium is significantly enriched in the coal seams from the study area, with an average content of 18.8-26.0 ppm. Gallium is distributed heterogeneously in the coals, and reaches ore-forming scales only in No. 6 coal of Heidaigou Surface Mine, not in the other mining districts of Jungar Coalfield. （2） On the horizontal plane, Ga is enriched in the main minable coals from the northern and middle part of the coalfield. In the vertical profile, Ga content in the coal seams is higher at the base of Taiyuan Formation （Nos. 8 and 9） and Shanxi Formation （Nos. 3 and 4） than at the top of the Taiyuan Formation. Within the identical coal seam, Ga content is higher in the benches near the roof and floor than in the middle section. （3） Gallium in the coals is associated mainly with kaolinite and boehmite. Additionally, Ga may be adsorbed to some extent by humic acid, resulting in a high level in weathering coal. （4） Geological factors affect Ga enrichment in coal, such as the prop- erty of parent rocks in the source area, the sedimentary environment, organic matter, structure, and past magmatic hydrothermal activity. Especially, Ga content in parent rocks plays a leading role. （5） The mobility and precipitation of trace elements like Ga are controlled principally by the geochemical behavior of the major element A1. Terrestrial and transgressive environments can cause the precipitation of bauxite, whereas marine-continental depositional environments may cause the separation of Ga from A1. In addition, Ga may migrate in the form of gas tively enriched in high-volatile coal. and may be affected by the ground temperature. Thus, it is relatively enriched in high-volatile coal.展开更多
Protonation and alkali-metal cation adduction are the most important ionization processes in soft-ionization mass spectrometry.Studies on the fragmentation mechanism of protonated and alkali-metal-cationized compounds...Protonation and alkali-metal cation adduction are the most important ionization processes in soft-ionization mass spectrometry.Studies on the fragmentation mechanism of protonated and alkali-metal-cationized compounds in tandem mass spectrometry are essential and helpful for structural analysis.In some cases,it was often observed that a compound attached by different alkali-metal cations(or proton)exhibits similar fragmentation patterns but the relative abundances of product ions are different.This difference was considered to derive from the different electrostatic interactions of alkali-metal cations(or the bonded effect of proton)with the analyte.The alkali-metal cation with a smaller ionic radius shows stronger electrostatic interaction with the molecule because of its higher charge density.In addition,the bonded effect of the proton is stronger than the electrostatic interaction of the alkali-metal cation.In the present study,which used McLafferty-type rearrangements of even-electron ions([M+Cat]+,Cat=H,Li,Na,K)as model reactions,the effect of cation size in mass spectrometric fragmentation reactions is highlighted.These considerations were also successfully applied to interpret the similar but distinct fragmentation behavior of proton and alkali-metal cation adducts of a synthetic compound(2-(acetamido(phenyl)methyl)-3-oxobutanoate)and a drug(entecavir).展开更多
基金National Natural Science Foundation of China(21705033)Natural Science Foundation of Henan Provincial Science and Technology Department(162300410043,182102410077)
基金Supported by the National Major Research Program of China"The Creation for Significant Innovative Drugs"(No.2009ZX09103-148)the Natural Science Foundation of Shandong(No.BS2009YY011)+1 种基金the Natural Science Foundation of Qingdao(No.10-3-4-8-2-JCH)the Program of Qingdao Shinan District(No.2009-HY-2-14)
文摘3-bromo-4,5-bis（2,3-dibromo-4,5-dihydroxybenzyl）-l,2-benzenediol （1） is a natural bromophenol isolated from the red algae Rhodomela confervoides that exhibits significant inhibition against protein tyrosine phosphatase 1B （PTP1B）. Based on its activity, we synthesized two new synthetic bromophenols and their methoxy derivatives from vanillin using the structure of natural bromophenol 1 as a scaffold. The structures of these bromophenols were elucidated from H NMR, 13C NMR, and high resolution electron ionization mass spectrometry as 2,3-dibromo-1-（2＇-bromo-6＇-（3＂,4＂-dimethoxybenzyl）- 3 ＇,4 ＇-dimethoxybenzyl）-4,5 -dimethoxybenzene （2）, 2,3-dibromo- 1 -（2 ＇-bromo-6＇-（2 ＂-bromo-4＂,5 ＂-dimethoxy- benzyl）-3＇,4＇-dimethoxybenzyl）-4,5-dimethoxybenzene （3）, 3,4-dibromo-5-（2＇-bromo-6＇-（2＂-bromo-4＂,5＂- dihydroxybenzyl）-3＇,4＇-dihydroxybenzyl）pyrocatechol （4） and 3,4-dibromo-5-（2＇-bromo-6＇-（3＂,4＂- dihydroxybenzyl）-3＇,4＇-dihydroxybenzyl）pyrocatechol （5）. PTP1B inhibition activities of these compounds were evaluated using a colorimetric assay, and compounds 3 and 4 demonstrated interesting activity against PTP1B.
基金Supported by the National Natural Science Foundation of China （40133010, 40973080）
文摘The bromine （Br） and iodine （I） in raw coal, bottom ash （BA） and fly ash （FA） from seven thermal power plants （TPP） digested with pyrohydrolysis were determined by using inductively coupled plasma mass spectrometry （ICP-MS）. The distribution behavior of Br and I during coal combustion were researched and the environmental effects of Br and I in BA, FA and gas phase were analyzed. The results show that both elements Br and I in combustion products from TPP are usually pre- sent in decreasing order of the distribution rate as gas phase, FA and BA. In FA and BA, the distribution rate of Br （8.11% and 1.68%, respectively） are generally lower than that of I （9.26% and 4.67%, respectively）; on the contrary, in gas phase, the former （90.2%） is higher than the latter （86.9%）. In addition, for gas phase, the percentage of Br： （2.0%-75%） in total Br is generally larger than that of I2 （1.0%-10%） in total I. The environmental effects for Br and I emitted into atmosphere from TPP may be larger than those remained and captured by both FA and BA.
基金Project(21075138)supported by the National Natural Science Foundation of ChinaProject(cstc2013jcyjA10088)supported by Chongqing Natural Science Foundation,ChinaProject(KJ121311)supported by Scientific and Technological Research Program of Chongqing Municipal Education Commission,China
文摘An analytical method, using sector field inductively coupled plasma mass spectrometry （SF-ICP-MS） for rapid simultaneous determination of Be, Na, Mg, Si, Ca, Ti, V, Cr, Fe, Co, Ni, Cu, Zn, As, Sn, Sb, Pb and Bi in electrolytic manganese metal, was described. At the beginning, the samples were decomposed by HNO3 and H2504, and then analyzed by SF-ICP-MS. Most of the spectral interferences could be avoided by measuring in different mass resolution modes. The matrix effects due to the excess of sulfuric acid and Mn were evaluated. Correction of matrix effects was conducted by using the internal standard elements. The optimum condition for the determination was investigated and discussed. The detection limit is in the range of 0.001-0.169 gg/L. The current method is applied to the determination of trace impurities in electrolytic manganese metal. And experiments show that good results can be obtained much faster, more accurately and conveniently by current method.
基金supported by National Natural Science Foundation of China (Grant Nos. 40772102 and 40730422)Program for New Century Excellent Talents in University (Grant No. NCET-08-0839)+2 种基金National Key Basic Research and Development Program of China (Grant No. 2007CB209400)the Fundamental Research Funds for the Central Universities (Grant No. 2010LKDZ02)Sci-Tech Project "Evaluation of coal resources in first batch national planning mining areas" of the Ministry of Land and Resources
文摘We collected eleven bench samples of No. 6 coal from the Heidaigou Surface Mine, Jungar Coalfield, Inner Mongolia, China, and four samples from the affiliated coal preparation plant. Based on these samples, we used inductively coupled-plasma mass spectroscopy, X-ray diffraction, scanning electron microscope with an energy-dispersive X-ray spectrometer techniques, and borehole exploration data, to investigate the distribution, occurrence and enrichment causes of gallium （Ga） in the coals. Our results show： （1） Gallium is significantly enriched in the coal seams from the study area, with an average content of 18.8-26.0 ppm. Gallium is distributed heterogeneously in the coals, and reaches ore-forming scales only in No. 6 coal of Heidaigou Surface Mine, not in the other mining districts of Jungar Coalfield. （2） On the horizontal plane, Ga is enriched in the main minable coals from the northern and middle part of the coalfield. In the vertical profile, Ga content in the coal seams is higher at the base of Taiyuan Formation （Nos. 8 and 9） and Shanxi Formation （Nos. 3 and 4） than at the top of the Taiyuan Formation. Within the identical coal seam, Ga content is higher in the benches near the roof and floor than in the middle section. （3） Gallium in the coals is associated mainly with kaolinite and boehmite. Additionally, Ga may be adsorbed to some extent by humic acid, resulting in a high level in weathering coal. （4） Geological factors affect Ga enrichment in coal, such as the prop- erty of parent rocks in the source area, the sedimentary environment, organic matter, structure, and past magmatic hydrothermal activity. Especially, Ga content in parent rocks plays a leading role. （5） The mobility and precipitation of trace elements like Ga are controlled principally by the geochemical behavior of the major element A1. Terrestrial and transgressive environments can cause the precipitation of bauxite, whereas marine-continental depositional environments may cause the separation of Ga from A1. In addition, Ga may migrate in the form of gas tively enriched in high-volatile coal. and may be affected by the ground temperature. Thus, it is relatively enriched in high-volatile coal.
基金financially supported by the National Natural Science Foundation of China(21025207,21372199)
文摘Protonation and alkali-metal cation adduction are the most important ionization processes in soft-ionization mass spectrometry.Studies on the fragmentation mechanism of protonated and alkali-metal-cationized compounds in tandem mass spectrometry are essential and helpful for structural analysis.In some cases,it was often observed that a compound attached by different alkali-metal cations(or proton)exhibits similar fragmentation patterns but the relative abundances of product ions are different.This difference was considered to derive from the different electrostatic interactions of alkali-metal cations(or the bonded effect of proton)with the analyte.The alkali-metal cation with a smaller ionic radius shows stronger electrostatic interaction with the molecule because of its higher charge density.In addition,the bonded effect of the proton is stronger than the electrostatic interaction of the alkali-metal cation.In the present study,which used McLafferty-type rearrangements of even-electron ions([M+Cat]+,Cat=H,Li,Na,K)as model reactions,the effect of cation size in mass spectrometric fragmentation reactions is highlighted.These considerations were also successfully applied to interpret the similar but distinct fragmentation behavior of proton and alkali-metal cation adducts of a synthetic compound(2-(acetamido(phenyl)methyl)-3-oxobutanoate)and a drug(entecavir).
