[Objectives] To develop a method for separation and purification of acetophenones from Cynanchum bengei Decne root bark by combination of silica gel and high-speed counter-current chromatography( HSCCC). [Methods]The ...[Objectives] To develop a method for separation and purification of acetophenones from Cynanchum bengei Decne root bark by combination of silica gel and high-speed counter-current chromatography( HSCCC). [Methods]The crude extract of Cynanchum bengei Decne root bark was separated by silica gel column chromatography,and parts A and B containing acetophenones were obtained. Then,parts A and B were separated by HSCCC with a two-phase solvent system composed of petroleum ether-ethyl acetate-methanol-water( 4∶ 6∶ 4. 5∶ 5. 5 and4∶ 6 ∶ 3 ∶ 7, V/V), respectively. [Results] From 260 mg of part A, four compounds with p-dihydroxybenzene 3. 9 mg(Ⅰ),4-hydroxyacetophenone 17. 1 mg( Ⅱ),2,5-di-hydroxyacetophenone 13. 3 mg(Ⅲ) and 2,4-dihydroxyaceto-phenone 21. 0 mg(Ⅳ) were obtained. And from 300 mg of part B,136 mg of Radix Cynanchi Bungei benzophenone(Ⅴ) was obtained. The purity of compounds determined by HPLC was 97. 0%,96. 6%,99. 2%,99. 7%,99. 5%,respectively. [Conclusions] The established method is simple and efficient. It can be used for separation of acetophenones from Cynanchum bengei Decne root bark and has better practical value,which could provide a reference basis for development and utilization of Cynanchum bengei Decne root bark.展开更多
The variation in arc characteristics and behavior of metal transfer with the change in pulse parameters has been studied by high speed video camera during pulse current flux-cored arc weld deposition.A comparative stu...The variation in arc characteristics and behavior of metal transfer with the change in pulse parameters has been studied by high speed video camera during pulse current flux-cored arc weld deposition.A comparative study of similar nature has also been carried out during flux-cored arc weld deposition in globular and spray transfer modes.The effect of pulse parameters has been studied by considering their mean current and arc voltage.The arc characteristics studied by its root diameter,projected diameter and length,and the behavior of metal transfer noted by the metal transfer model and the droplet diameter have been found to vary significantly with the pulse parameters.The observation may help in understanding the arc characteristics with respect to the variation in pulse parameters which may be beneficial in using pulse current FCAW to produce desired weld quality.展开更多
基金Supported by National Natural Science Foundation Item of 2014(81373941)Shandong Natural Science Foundation Item of 2012(ZR2012HM047)+1 种基金Science and Technology Development Plan Item of Shandong(2014G2X219003)Major Project of the State Administration of Traditional Chinese Medicine(201407002)
文摘[Objectives] To develop a method for separation and purification of acetophenones from Cynanchum bengei Decne root bark by combination of silica gel and high-speed counter-current chromatography( HSCCC). [Methods]The crude extract of Cynanchum bengei Decne root bark was separated by silica gel column chromatography,and parts A and B containing acetophenones were obtained. Then,parts A and B were separated by HSCCC with a two-phase solvent system composed of petroleum ether-ethyl acetate-methanol-water( 4∶ 6∶ 4. 5∶ 5. 5 and4∶ 6 ∶ 3 ∶ 7, V/V), respectively. [Results] From 260 mg of part A, four compounds with p-dihydroxybenzene 3. 9 mg(Ⅰ),4-hydroxyacetophenone 17. 1 mg( Ⅱ),2,5-di-hydroxyacetophenone 13. 3 mg(Ⅲ) and 2,4-dihydroxyaceto-phenone 21. 0 mg(Ⅳ) were obtained. And from 300 mg of part B,136 mg of Radix Cynanchi Bungei benzophenone(Ⅴ) was obtained. The purity of compounds determined by HPLC was 97. 0%,96. 6%,99. 2%,99. 7%,99. 5%,respectively. [Conclusions] The established method is simple and efficient. It can be used for separation of acetophenones from Cynanchum bengei Decne root bark and has better practical value,which could provide a reference basis for development and utilization of Cynanchum bengei Decne root bark.
文摘The variation in arc characteristics and behavior of metal transfer with the change in pulse parameters has been studied by high speed video camera during pulse current flux-cored arc weld deposition.A comparative study of similar nature has also been carried out during flux-cored arc weld deposition in globular and spray transfer modes.The effect of pulse parameters has been studied by considering their mean current and arc voltage.The arc characteristics studied by its root diameter,projected diameter and length,and the behavior of metal transfer noted by the metal transfer model and the droplet diameter have been found to vary significantly with the pulse parameters.The observation may help in understanding the arc characteristics with respect to the variation in pulse parameters which may be beneficial in using pulse current FCAW to produce desired weld quality.
