[Objectives]To establish an efficient and environmentally friendly separation and purification method for the large-scale preparation of the major active components-eleutherol,eleutherine,and isoeleutherine-from the e...[Objectives]To establish an efficient and environmentally friendly separation and purification method for the large-scale preparation of the major active components-eleutherol,eleutherine,and isoeleutherine-from the ethnomedicinal plant Eleutherine americana Merr.et K.Heyne.[Methods]The sample of E.americana bulbs was initially extracted with ethanol,followed by three successive extractions with ethyl acetate-water(2:1,V/V)to obtain the target component-enriched fraction.Eight solvent systems were systematically optimized,and a mixture of petroleum ether-ethyl acetate-ethanol-water(5:5:6:4,V/V/V/V)was identified as the optimal solvent system for high-speed counter-current chromatography(HSCCC)separation under conditions of 900 rpm,2 mL/min,and 35℃.The crude HSCCC product was further purified by silica gel column chromatography(200-300 mesh)using gradient elution with a solvent system of n-hexane-dichloromethane-ethyl acetate(varying from 10:5:1 to 4:5:1,V/V/V).UPLC-PDA(Agilent SB-C_(18)column)and nuclear magnetic resonance spectroscopy(600 MHz)were comprehensively employed to assess compound purity and confirm molecular structures.[Results]An optimized technique integrating HSCCC and silica gel column chromatography was established,successfully enabling the large-scale preparation of three bioactive components:eleutherol(purity 99%),eleutherine(purity 98%),and isoeleutherine(purity 98%).Structural identification results were consistent with those reported in the literature.Compared to traditional methods,the new approach demonstrated improved separation efficiency and reduced solvent consumption.[Conclusions]The combined separation method utilizing HSCCC and silica gel column chromatography established in this study demonstrates notable advantages,including high efficiency,environmental friendliness,and cost-effectiveness,enabling the large-scale preparation of the three major active components from E.americana.This approach outperforms conventional methods by offering higher separation efficiency,reduced solvent consumption,and superior product purity,providing a robust technical solution for the development and utilization of bioactive compounds from E.americana.Moreover,it offers a novel methodological reference for the isolation and purification of other natural products.展开更多
A high-speed counter-current chromatography （HSCCC） method was successfully developed for the preparative separation and purification of deoxyschizandrin from Schisandrae Sphenantherae Fructus in one step. The purit...A high-speed counter-current chromatography （HSCCC） method was successfully developed for the preparative separation and purification of deoxyschizandrin from Schisandrae Sphenantherae Fructus in one step. The purity of deoxyschizandrin was 98.5%, and the structure was identified by MS, UV and NMR. This method was simple, fast, convenient and appropriate to prepare pure compound as reference substances for related research on Schisandrae Sphenantherae Fmctus.展开更多
A new chromatographic purification of single-walled carbon nanotubes using high-speed countercurrent chromatography is reported. The purification was accomplished on the basis of experiment that dispersed the single-w...A new chromatographic purification of single-walled carbon nanotubes using high-speed countercurrent chromatography is reported. The purification was accomplished on the basis of experiment that dispersed the single-walled carbon nanotubes with sodium dodecyl sulfate, and the result mixture was separated using the two phase system composed of n-butanol/water = 1/1 （v/v）. The sizes of SWNTs separated were observed by scanning electron microscopy. The results demonstrated that the high-speed countercurrent chromatography possessed a good efficency for purification of single-walled carbon nanotubes.展开更多
Coptis chinensis Franch, a widely used Traditional Chinese Medicine, shows various kinds of bioactivity. The major active components of the herb are considered to be alkaloids. Thus, preparative separation of these al...Coptis chinensis Franch, a widely used Traditional Chinese Medicine, shows various kinds of bioactivity. The major active components of the herb are considered to be alkaloids. Thus, preparative separation of these alkaloids is critical important for further pharmacology and mechanism studies. In the paper, five alkaloids from C. chinensis were purified by HSCCC using the solvent system composed of chloro-form-metha- nol-water (2:1:1, v/v/v) single prepared. The content of each solvent in solvent system were determined by gas chromatography (GC), then according the ratios of solvents in each phase to prepare the mobile and stationary phase respectively. And a comparative study was carried out between together preparation and single preparation of the solvent system. The purities and recoveries of all the products were over 98.5% and 92%. However, 134 mL chloroform, 336 mL methanol and 452 mL water were saved when the two phase were singled by GC. Our research showed an economical method for separating alkaloids from C. chinensis by HSCCC using the solvent system single prepared by GC.展开更多
[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
This paper studies the structural response of high-speed train wipers under the combined action of complex flow fields and scraping actions.The stress concentration areas are determined through simulation analysis,and...This paper studies the structural response of high-speed train wipers under the combined action of complex flow fields and scraping actions.The stress concentration areas are determined through simulation analysis,and the stress and aerodynamic load measurement points are reasonably arranged accordingly.The actual measurement is carried out in combination with the operating conditions of the existing lines.The stress variations and spectral characteristics of the train under different speed levels(80,160,180,200 km/h),tunnel entry and exit,and scraper action conditions were compared and analyzed.The stress amplification factors under tunnel intersection and scraper action were obtained,providing boundary conditions for the design of wipers for highspeed s.The research results show that the maximum stress of the wiper structure obtained through simulation calculation is concentrated at the connection of the wiper arm.Structural stress increases with the rise of speed grade.The stress increases by 1.11 times when the tunnel meets.When the scraper operates,the stress on the scraper arm increases by 4.1–7.6 times.Due to the broadband excitation effect of the aerodynamic load,the spectral energy of the structure is relatively high at the natural frequency,which excites the natural mode of the wiper.展开更多
As the main component of the aircraft leading edge,the radome is often the first to be hit by raindrops and cause structural damage when passing through a rain field.Rain resistant coating is usually applied to ensure...As the main component of the aircraft leading edge,the radome is often the first to be hit by raindrops and cause structural damage when passing through a rain field.Rain resistant coating is usually applied to ensure the performance protection requirements.In order to clarify the rain erosion damage mechanism of radome coating and explore the influencing factors and mechanisms of coating material damage under different jet impact conditions,impact tests were conducted on three types of skin coating samples,and the damage mode was observed through electron microscopy characterization.The experimental results show that the typical morphology of rain erosion damage is annular surface peeling damage.The damage area and volume of the three coating samples increase with the continuous increase of raindrop impact velocity.The threshold velocity for initial damage to the coating is about 360 m/s;under the influence of the velocity component,the reduction in impact angle leads to a gradual reduction in the degree of damage to the sample.ABAQUS finite element simulation software was used to establish a constitutive model for coating rain erosion simulation and obtain the propagation law of stress waves during the impact process.The simulation results show that at the 75°impact angle,the jet impacts the surface of the specimen at different velocities,and as the impact velocity increases,the Mises equivalent stress on the surface shows an increasing trend,which is one of the main factors causing damage with increasing velocity.The effectiveness,rain erosion damage mode,and influencing mechanism of the model were verified based on the test results;the dynamic failure mechanism of the sample was further studied,and the stress propagation process at different impact angles was compared,revealing the influence mechanism and damage law of the impact angle on the high-speed raindrop impact of the material.展开更多
This paper proposes a passive control method to reduce peak values of slipstream and turbulent kinetic energy in a high-speed train wake by attaching vortex generators(VGs)onto the upper surface of the tail car.The im...This paper proposes a passive control method to reduce peak values of slipstream and turbulent kinetic energy in a high-speed train wake by attaching vortex generators(VGs)onto the upper surface of the tail car.The impact of the VGs is assessed through the improved delayed detached eddy simulations(IDDES)after validating predictions against previous experimental measurements and other numerical predictions for the base case.The simulations indicate that strategically installed VGs can reduce the average slipstream velocity(U slipstream)and the upper limit of slipstream velocity(U_(slipstream,max))by~17%and~15%,respectively,as well as moving the peaks downstream by approximately train height,thus reducing the danger posed by slipstream to waiting passengers and trackside workers.Analysis shows that the wake turbulent kinetic energy diminishes as the vortex generators decelerate the downwash flow and reduce shear production in the wake.It is also found that the presence of VGs significantly impacts the flow on the upper surface near the tail by modifying the unsteady trailing longitudinal vortices through the formation of additional counter-rotating longitudinal vortices from the VGs.These latter vortices prevent the merging of vortical airflow around the trailing nose tip,which is otherwise induced by the longitudinal vortex of the train.They also reduce vortex intensity through cross-annihilation and cross diffusion as the wake advects downstream,limiting outwards advection through interaction with the image pair,and contributing to a decrease in the peak slipstream value.The method proposed offers a simple approach to wake control leading to significant slipstream benefits.展开更多
The axle box bearings of high-speed trains often operate in extremely harsh environments,bearing loads from different directions.Long-term operation and frequent changes in working conditions can easily lead to axle b...The axle box bearings of high-speed trains often operate in extremely harsh environments,bearing loads from different directions.Long-term operation and frequent changes in working conditions can easily lead to axle box bearing failures.Therefore,it is extremely important to study the mechanism of axle box bearings.Firstly,the medium of thermal deformation establishes a coupling relationship between the system dynamics model and the thermal grid model,and then obtains the thermal force coupling model of the high-speed train axle box bearing.The coupling model is validated from the perspectives of system dynamics response and temperature response,proving its effectiveness in system dynamics response and temperature characteristic response.Comparing the coupling model with the dynamics model,it is found that thermal deformation complicates the dynamic re-sponse.Finally,using the Lundberg-Palmgren(L-P)bearing fatigue calculation method and damage accumu-lation theory,the bearing fatigue life is calculated,and it is found that thermal deformation deteriorates the bearing operating environment,reducing the bearing fatigue life.Finally,by comparing the bearing fatigue life under different working conditions,it is concluded that the faster the vehicle speed,the greater the load,and the smaller the initial radial clearance of the bearing,the fatigue life of the bearing is reduced.The shorter the lifespan.展开更多
Research on high-speed railways is a relatively new yet highly significant field in Vietnam.Among its key components,train control signaling plays a critical role,as it directly affects various interconnected systems,...Research on high-speed railways is a relatively new yet highly significant field in Vietnam.Among its key components,train control signaling plays a critical role,as it directly affects various interconnected systems,including infrastructure,traction power supply,operational planning,and overall railway safety.This article focuses on evaluating the capacity of the line based on the types of signals suitable for high-speed railways that have been effectively implemented in several European countries and successfully adapted in China.The research and simulation are conducted using MATLAB software,a reliable and widely adopted tool in the scientific community.The findings demonstrate that under normal conditions,the European Railway Traffic Management System/European Train Control System(ERTMS/ETCS)Level 2 signaling can support up to 23.7485 trains/hour/direction.Meanwhile,ERTMS/ETCS Level 3 with full moving block can accommodate up to 30.8735 trains/hour/direction,and ERTMS/ETCS Level 3 with fixed virtual blocks up to 29.4694 trains/hour/direction.In emergency scenarios,ERTMS/ETCS Level 3 with full moving block reduces headway by 33.27%compared to CTCS Level 3,while ERTMS/ETCS Level 3 with fixed virtual blocks achieves a 28.78%reduction.Overall,the ERTMS/ETCS Level 3 emerges as a state-of-the-art signaling technology offering high capacity and operational efficiency,and is recommended as a forward-looking solution for future implementation in Vietnam.展开更多
As China's high-speed railway technology advances,high-speed trains have emerged as a pivotal mode of transportation,instrumental in facilitating passenger and freight mobility while fostering robust regional eco-...As China's high-speed railway technology advances,high-speed trains have emerged as a pivotal mode of transportation,instrumental in facilitating passenger and freight mobility while fostering robust regional eco-nomic and trade interactions.Nonetheless,the safety of train operations remains a paramount concern,prompting extensive research into the dynamic behavior of critical components,which is essential to ensuring seamless and secure transportation services.This article commences by comprehensively reviewing the current landscape and evolutionary trajectory of dynamic model analysis for both traditional bearings and axle box bearings.Emphasis is placed on elucidating the profound influence of diverse bearing fault types on the system's kinematic state,alongside delving into the research methodologies employed in developing multi-physics field coupling models.Subsequently,it expounds on the content of investigations focusing on various wheel and track impairments,grounded in the dynamic modeling of the bearing vehicle coupling system.Concurrently,the intricate interplay between wheel-rail excitation and axle box bearing faults on the system's performance is elucidated.Concludingly,the article underscores the inadequacy of current multi-source fault diagnosis meth-odologies in tackling the intricacies of complex train operating environments,thereby highlighting its sig-nificance as a pressing and vital research agenda for the future.展开更多
The spatial offset of bridge has a significant impact on the safety,comfort,and durability of high-speed railway(HSR)operations,so it is crucial to rapidly and effectively detect the spatial offset of operational HSR ...The spatial offset of bridge has a significant impact on the safety,comfort,and durability of high-speed railway(HSR)operations,so it is crucial to rapidly and effectively detect the spatial offset of operational HSR bridges.Drive-by monitoring of bridge uneven settlement demonstrates significant potential due to its practicality,cost-effectiveness,and efficiency.However,existing drive-by methods for detecting bridge offset have limitations such as reliance on a single data source,low detection accuracy,and the inability to identify lateral deformations of bridges.This paper proposes a novel drive-by inspection method for spatial offset of HSR bridge based on multi-source data fusion of comprehensive inspection train.Firstly,dung beetle optimizer-variational mode decomposition was employed to achieve adaptive decomposition of non-stationary dynamic signals,and explore the hidden temporal relationships in the data.Subsequently,a long short-term memory neural network was developed to achieve feature fusion of multi-source signal and accurate prediction of spatial settlement of HSR bridge.A dataset of track irregularities and CRH380A high-speed train responses was generated using a 3D train-track-bridge interaction model,and the accuracy and effectiveness of the proposed hybrid deep learning model were numerically validated.Finally,the reliability of the proposed drive-by inspection method was further validated by analyzing the actual measurement data obtained from comprehensive inspection train.The research findings indicate that the proposed approach enables rapid and accurate detection of spatial offset in HSR bridge,ensuring the long-term operational safety of HSR bridges.展开更多
Railway noise barriers are an essential piece of infrastructure for reducing noise propagation.However,these barriers experience aerodynamic loads generated by high-speed trains,leading to dynamic effects that may com...Railway noise barriers are an essential piece of infrastructure for reducing noise propagation.However,these barriers experience aerodynamic loads generated by high-speed trains,leading to dynamic effects that may compromise their fatigue capacity.The most common structural design for railway noise barriers consists of vertical configurations of posts and panels.However,there have been few dynamic analyses of steel post/wood panel noise barriers under train-induced aerodynamic loads.This study used dynamic finite element analysis to assess the dynamic behavior of such noise barriers.Analysis of a 40-m-long noise barrier model and a triangular simplified load model,the latter of which effectively represented the detailed aerodynamic load,were first used to establish the model and input of the moving load during dynamic simulation.Then,the effects of different parameters on the dynamic response of the noise barrier were evaluated,including the damping ratio,the profile of the steel post,the span length of the panel,the barrier height,and the train speed.Gray relational analysis indicated that barrier height exhibited the highest correlations with the dynamic responses,followed by train speed,post profile,span length,and damping ratio.A reduction in the natural frequency and an increase in the train speed result in a higher peak response and more pronounced fluctuations between the nose and tail waves.The dynamic amplification factor(DAF)was found to be related to both the natural frequency and train speed.A model was proposed showing that the DAF significantly increases as the square of the natural frequency decreases and the cube of the train speed rises.展开更多
We demonstrate a high-speed rotating slit beam shaping method for femtosecond(fs)laser three-dimensional(3D)isotropic inscription in glass materials.By integrating fs laser direct writing with a real-time rotating sli...We demonstrate a high-speed rotating slit beam shaping method for femtosecond(fs)laser three-dimensional(3D)isotropic inscription in glass materials.By integrating fs laser direct writing with a real-time rotating slit mechanism,a 3D symmetric spherical focal field distribution is created in the laser-irradiated regions of transparent substrates.The corresponding focal field distribution is theoretically calculated and validated by examining the features of laser-inscribed lines in glass samples.Moreover,we investigate the influences of laser writing speed and slit rotational speed on the fabrication resolution in glass,and discuss the formation mechanism of the generated periodic microstructures.To showcase its powerful capability for3D isotropic fabrication,the high-speed rotating slit beam shaping method is applied to create straight optical waveguides,bending optical waveguides,and hollow microchannels in the glass.The proposed method holds great potential for the facile manufacture of diverse 3D isotropic microstructures and devices within transparent materials across various applications,including advanced photonics,microoptics,micro-electromechanical systems,and microfluidics.展开更多
Under the background of‘the Belt and Road’and‘China-Mongolia-Russia Economic Corridor’initiatives,this paper studied the urban accessibility level,regional accessibility pattern and regional spatial effects along ...Under the background of‘the Belt and Road’and‘China-Mongolia-Russia Economic Corridor’initiatives,this paper studied the urban accessibility level,regional accessibility pattern and regional spatial effects along the Primorsky No.1 and No.2 transportation corridors.First,the evaluation of urban accessibility level with and without Primorsky No.1 and No.2 high-speed rails(HSRs)opening was conducted with two indicators,i.e.,the weighted average travel time,and the economic potential.After the evaluation,the spatial differentiation pattern of the accessibility changes with and without Primorsky No.1 and No.2 HSRs opening was performed respectively using ArcGIS.On these bases,the regional spatial effects brought by Primorsky No.1 and No.2 HSRs opening were studied.The results are as following.First,the urban accessibility level will be greatly improved by the opening of Primorsky No.1 and No.2 HSRs.All adjacent cities will be integrated into‘1 h HSR communication circle’and the whole journey will be integrated into‘4 h HSR communication circle’along Primorsky No.1 and No.2 corridors,respectively.The HSR accessibility of Primorsky No.1 corridor is stronger than that of Primorsky No.2 corridor.But the HSR accessibility improvement degree of Primorsky No.1 corridor is weaker than that of Primorsky No.2 corridor.Second,spatially,along Primorsky No.1 and No.2 corridors,the HSR accessibility level of the cities which are located in China is stronger than those cities located in Russia,showing the‘High West,Low East’patterns.The HSR accessibility improvement degree of the cities which are located in Russia and Sino-Russian border is stronger than those cities located in China,showing the‘High East,Low West’patterns.Third,Primorsky No.1 and No.2 corridors could connect the China’s‘Heilongjiang Land Sea Silk Road Economic Belt’and‘Changchun-Jilin-Tumen Development Pilot Zone’respectively,gradually involving into the development of China’s Harbin-Changchun Megalopolis.Relying on Harbin(China)and Changchun(China),Primorsky No.1 and No.2 HSRs could connect Northeast China-Beijing HSR,accelerating the diffusion of population,economy and other flows from China’s Beijing-Tianjin-Hebei Urban Agglomeration to Northeast China,and then to Russia’s Far East Federal District.Relying on Suifenhe(China)and Hunchun(China),Primorsky No.1 and No.2 HSRs could be conducive to the development of the second largest sea channels for Northeast China,creating the Northeast Asian Urban Belt,and new sea-rail intermodal pattern among China,Russia,Democratic People’s Republic of Korea,Japan and Republic of Korea.Relying on Vladivostok(Russia)and Zarubino(Russia),Primorsky No.1 and No.2 corridors could connect the‘Ice Silk Road’,building the‘Sino-Russian Northern Maritime Corridor’and‘Sino-Russian Arctic Blue Economic Areas’.展开更多
Purpose–Regarding that Ultraviolet radiation,pollutant adsorption,and environmental changes may be the main reasons for the aging and yellowing on windshield rubber in high-speed trains,countermeasures are proposed t...Purpose–Regarding that Ultraviolet radiation,pollutant adsorption,and environmental changes may be the main reasons for the aging and yellowing on windshield rubber in high-speed trains,countermeasures are proposed to solve the aging and yellowing of windshield rubber and reduce the adverse effects caused by rubber yellowing.Design/methodology/approach–Scanning electron microscopy(SEM)and energy dispersive spectroscopy(EDS)were used to test the yellowed windshield rubber.Aging tests,including UVaging,natural aging and salt spray aging,were conducted to analyze the effects of aging on the windshield rubber.Different cleaning agents were selected to soak the windshield rubber,and the quality,hardness,and surface appearance of the rubber samples were tested.Findings–After UV aging,antioxidants migrated to the surface of the windshield rubber,but due to oxidation failure,they could not capture free radicals,leading to continued oxidation reactions within the material and resulting in yellowing of the rubber in a short period of time.Originality/value–Cleaning agents have a minimal impact on windshield rubber,UV aging has the greatest impact and natural aging is a gradual and slow deterioration process.Through daily deep cleaning and maintenance with protective agents at regular intervals,the deterioration of windshield rubber yellowing in high-speed trains can be effectively suppressed.展开更多
Objective To develop a suitable method for the large-scale separation of quinolone alkaloids from the fruits of Evodia rutaecarpa by high-speed counter-current chromatography （HSCCC）. Methods Two solvent systems wer...Objective To develop a suitable method for the large-scale separation of quinolone alkaloids from the fruits of Evodia rutaecarpa by high-speed counter-current chromatography （HSCCC）. Methods Two solvent systems were developed for the separation method. The upper phase was used as the stationary phase, and the lower phase was used as the mobile phase at 35 oCwith the flow rate of 2 mL/min and rotation speed of 855 r/min. Results Using the described method, 1-methyl-2-undecyl- 4（1H）-quinoione （1）, evocarpine （2）, 1-methy-2-[（6Z,9Z}]-6,9-pentade-cadienyl-4- （1H）-quinolone （3）, dihydroevocarpine （4）, and the mixture （5） of 1-methyl-2-[（z^- 10-pentadecenyl]-4（1H）-quinolone （Va） and 1 -methyl-2-[（Z^-6-pentadecenyl]- 4（1H）-quinolone （Vb） could be isolated from a petroleum ether extract. They were identified by 1H-NMR, ~3C-NMR, and MS/MS, and the purities were 94.3%, 95.2%, 96.8%, 98.3%, and 96.8%, respectively. Conclusion Five quinolone alkaloids from the fruits of E. rutaecarpa could be systematically isolated and purified using HSCCC. The presented method is simple and efficient with good potentials on the preparation of reference substances, especially on the quality control of Chinese materia medica.展开更多
Objective To develop an efficient preparative method for the separation of Gelsemium alkaloids from Gelsemium elegans. Methods High-speed counter-current chromatography （HSCCC） with several two-phase solvent systems...Objective To develop an efficient preparative method for the separation of Gelsemium alkaloids from Gelsemium elegans. Methods High-speed counter-current chromatography （HSCCC） with several two-phase solvent systems was investigated for the separation of Gelsemium alkaloids. The purity and structure identification of the purified compounds were performed with HPLC and NMR spectra, respectively. Results In a single operation, 206.6 mg of crude alkaloid sample was separated to yield 28.7 mg of koumine, 24.9 mg of gelsemine, 26.9 mg of humantenine, and 7.2 mg of gelsevirine, with the purities of 97.8%, 95.4%, 97.4%, and 93.5%, respectively. Conclusion A preparative HSCCC method is successfully established for the separation of four Gelsemium alkaloids from G. elegans with a modified two-phase solvent system com posed of n-hexane-ethyl acetate-ethanol-O. 5% triethylamine-H2O （3：5：3：4）.展开更多
Objective To develop an efficient method to isolate and purify the main components isoaloeresin D and aloin from Aloe vera for its industrial production.Methods High-speed counter-current chromatography was used to is...Objective To develop an efficient method to isolate and purify the main components isoaloeresin D and aloin from Aloe vera for its industrial production.Methods High-speed counter-current chromatography was used to isolate isoaloeresin D and aloin in a one-step separation from dried crude extract of A.vera.The biphasic solvent system composed of hexane-ethyl acetate-acetone-water(0.2:5:1.5:5)was used at a flow rate of 1.0 mL/min,while the lipophilic phase was selected as the mobile phase and the apparatus was rotated at 840 r/min.The effluent was detected at 254 nm.Results Isoaloeresin D(53.1 mg)and aloin(106.9 mg)were separated from the crude extract(384.7 mg)with the purities of 98.6%and 99.5%,respectively.Conclusion HSCCC is a powerful technique for isolation and separation of chemical composition from aloe.展开更多
Rice false smut is an emerging plant disease worldwide.Ustiloxin A(UstA)is the major mycotoxin found in rice false smut balls,which are fungal colonies in rice florets.In this study,a new method consisting of macropor...Rice false smut is an emerging plant disease worldwide.Ustiloxin A(UstA)is the major mycotoxin found in rice false smut balls,which are fungal colonies in rice florets.In this study,a new method consisting of macroporous resin column chromatography and high-speed countercurrent chromatography(HSCCC)was developed for UstA separation.UstA was extracted by a 3.81%HCOOH solution and adsorbed by XAD-4 resin.UstA was then eluted by a 40%methanol solution supplemented with 0.1%trifluoroacetic acid(TFA).Further purification was achieved by HSCCC using a two-phase solvent system consisting of n-butanol/TFA/H_(2)O(1/0.05/1,v/v/v).Under the optimized conditions,225 mg of UstA was obtained with a purity of 97.39%in a single run,with a final recovery of 65.2%.An inhibitory effect on seed germination of wheat and maize caused by UstA was observed in a preliminary phytotoxicity assay.展开更多
基金Supported by Natural Science Foundation of Tibet Autonomous Region,Science and Technology Department of Tibet(XZ202501ZR0118).
文摘[Objectives]To establish an efficient and environmentally friendly separation and purification method for the large-scale preparation of the major active components-eleutherol,eleutherine,and isoeleutherine-from the ethnomedicinal plant Eleutherine americana Merr.et K.Heyne.[Methods]The sample of E.americana bulbs was initially extracted with ethanol,followed by three successive extractions with ethyl acetate-water(2:1,V/V)to obtain the target component-enriched fraction.Eight solvent systems were systematically optimized,and a mixture of petroleum ether-ethyl acetate-ethanol-water(5:5:6:4,V/V/V/V)was identified as the optimal solvent system for high-speed counter-current chromatography(HSCCC)separation under conditions of 900 rpm,2 mL/min,and 35℃.The crude HSCCC product was further purified by silica gel column chromatography(200-300 mesh)using gradient elution with a solvent system of n-hexane-dichloromethane-ethyl acetate(varying from 10:5:1 to 4:5:1,V/V/V).UPLC-PDA(Agilent SB-C_(18)column)and nuclear magnetic resonance spectroscopy(600 MHz)were comprehensively employed to assess compound purity and confirm molecular structures.[Results]An optimized technique integrating HSCCC and silica gel column chromatography was established,successfully enabling the large-scale preparation of three bioactive components:eleutherol(purity 99%),eleutherine(purity 98%),and isoeleutherine(purity 98%).Structural identification results were consistent with those reported in the literature.Compared to traditional methods,the new approach demonstrated improved separation efficiency and reduced solvent consumption.[Conclusions]The combined separation method utilizing HSCCC and silica gel column chromatography established in this study demonstrates notable advantages,including high efficiency,environmental friendliness,and cost-effectiveness,enabling the large-scale preparation of the three major active components from E.americana.This approach outperforms conventional methods by offering higher separation efficiency,reduced solvent consumption,and superior product purity,providing a robust technical solution for the development and utilization of bioactive compounds from E.americana.Moreover,it offers a novel methodological reference for the isolation and purification of other natural products.
基金supported by the International Scientific and Technological Cooperation Program of China(No.2009DFA31230)the Industry-University-Research Cooperation Program from Science and Technology Department of Guangdong Province(No.2010B090400533)
文摘A high-speed counter-current chromatography （HSCCC） method was successfully developed for the preparative separation and purification of deoxyschizandrin from Schisandrae Sphenantherae Fructus in one step. The purity of deoxyschizandrin was 98.5%, and the structure was identified by MS, UV and NMR. This method was simple, fast, convenient and appropriate to prepare pure compound as reference substances for related research on Schisandrae Sphenantherae Fmctus.
基金supported by National Natural Science Foundation (No.20775066)Yunnan Province's Natural Science Foundations of China (Nos.2005E0006Z and 2007B203M).
文摘A new chromatographic purification of single-walled carbon nanotubes using high-speed countercurrent chromatography is reported. The purification was accomplished on the basis of experiment that dispersed the single-walled carbon nanotubes with sodium dodecyl sulfate, and the result mixture was separated using the two phase system composed of n-butanol/water = 1/1 （v/v）. The sizes of SWNTs separated were observed by scanning electron microscopy. The results demonstrated that the high-speed countercurrent chromatography possessed a good efficency for purification of single-walled carbon nanotubes.
文摘Coptis chinensis Franch, a widely used Traditional Chinese Medicine, shows various kinds of bioactivity. The major active components of the herb are considered to be alkaloids. Thus, preparative separation of these alkaloids is critical important for further pharmacology and mechanism studies. In the paper, five alkaloids from C. chinensis were purified by HSCCC using the solvent system composed of chloro-form-metha- nol-water (2:1:1, v/v/v) single prepared. The content of each solvent in solvent system were determined by gas chromatography (GC), then according the ratios of solvents in each phase to prepare the mobile and stationary phase respectively. And a comparative study was carried out between together preparation and single preparation of the solvent system. The purities and recoveries of all the products were over 98.5% and 92%. However, 134 mL chloroform, 336 mL methanol and 452 mL water were saved when the two phase were singled by GC. Our research showed an economical method for separating alkaloids from C. chinensis by HSCCC using the solvent system single prepared by GC.
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This paper studies the structural response of high-speed train wipers under the combined action of complex flow fields and scraping actions.The stress concentration areas are determined through simulation analysis,and the stress and aerodynamic load measurement points are reasonably arranged accordingly.The actual measurement is carried out in combination with the operating conditions of the existing lines.The stress variations and spectral characteristics of the train under different speed levels(80,160,180,200 km/h),tunnel entry and exit,and scraper action conditions were compared and analyzed.The stress amplification factors under tunnel intersection and scraper action were obtained,providing boundary conditions for the design of wipers for highspeed s.The research results show that the maximum stress of the wiper structure obtained through simulation calculation is concentrated at the connection of the wiper arm.Structural stress increases with the rise of speed grade.The stress increases by 1.11 times when the tunnel meets.When the scraper operates,the stress on the scraper arm increases by 4.1–7.6 times.Due to the broadband excitation effect of the aerodynamic load,the spectral energy of the structure is relatively high at the natural frequency,which excites the natural mode of the wiper.
基金supported by the National Natural Science Foundation of China(Nos.12261131505,U2241274)the Russian Science Fund(No.23-49-00133)+3 种基金the Aeronautical Science Foundation of China(No.20240002053002)the Natural Science Basic Research Program of Shaanxi,China(No.2025JC-YBMS-005)the Key Research and Development Program of Shaanxi,China(No.2024GX-YBXM-037)the Basic Research Programs of Taicang,China(No.TC2024JC10)。
文摘As the main component of the aircraft leading edge,the radome is often the first to be hit by raindrops and cause structural damage when passing through a rain field.Rain resistant coating is usually applied to ensure the performance protection requirements.In order to clarify the rain erosion damage mechanism of radome coating and explore the influencing factors and mechanisms of coating material damage under different jet impact conditions,impact tests were conducted on three types of skin coating samples,and the damage mode was observed through electron microscopy characterization.The experimental results show that the typical morphology of rain erosion damage is annular surface peeling damage.The damage area and volume of the three coating samples increase with the continuous increase of raindrop impact velocity.The threshold velocity for initial damage to the coating is about 360 m/s;under the influence of the velocity component,the reduction in impact angle leads to a gradual reduction in the degree of damage to the sample.ABAQUS finite element simulation software was used to establish a constitutive model for coating rain erosion simulation and obtain the propagation law of stress waves during the impact process.The simulation results show that at the 75°impact angle,the jet impacts the surface of the specimen at different velocities,and as the impact velocity increases,the Mises equivalent stress on the surface shows an increasing trend,which is one of the main factors causing damage with increasing velocity.The effectiveness,rain erosion damage mode,and influencing mechanism of the model were verified based on the test results;the dynamic failure mechanism of the sample was further studied,and the stress propagation process at different impact angles was compared,revealing the influence mechanism and damage law of the impact angle on the high-speed raindrop impact of the material.
基金Project(52372370)supported by the National Natural Science Foundation of ChinaProject(2023ZZTS0379)supported by the Graduate Student Independent Innovation Project of Central South University,ChinaProject(202206370058)supported by the China Scholarship Council。
文摘This paper proposes a passive control method to reduce peak values of slipstream and turbulent kinetic energy in a high-speed train wake by attaching vortex generators(VGs)onto the upper surface of the tail car.The impact of the VGs is assessed through the improved delayed detached eddy simulations(IDDES)after validating predictions against previous experimental measurements and other numerical predictions for the base case.The simulations indicate that strategically installed VGs can reduce the average slipstream velocity(U slipstream)and the upper limit of slipstream velocity(U_(slipstream,max))by~17%and~15%,respectively,as well as moving the peaks downstream by approximately train height,thus reducing the danger posed by slipstream to waiting passengers and trackside workers.Analysis shows that the wake turbulent kinetic energy diminishes as the vortex generators decelerate the downwash flow and reduce shear production in the wake.It is also found that the presence of VGs significantly impacts the flow on the upper surface near the tail by modifying the unsteady trailing longitudinal vortices through the formation of additional counter-rotating longitudinal vortices from the VGs.These latter vortices prevent the merging of vortical airflow around the trailing nose tip,which is otherwise induced by the longitudinal vortex of the train.They also reduce vortex intensity through cross-annihilation and cross diffusion as the wake advects downstream,limiting outwards advection through interaction with the image pair,and contributing to a decrease in the peak slipstream value.The method proposed offers a simple approach to wake control leading to significant slipstream benefits.
基金Supported by the National Natural Science Foundation of China(Grant Nos.12393780,12032017,12302067)College Education Scientific Research Project of Hebei Province(Grant No.JZX2024006)Hebei Provincial S&T Program(Grant No.21567622 H).
文摘The axle box bearings of high-speed trains often operate in extremely harsh environments,bearing loads from different directions.Long-term operation and frequent changes in working conditions can easily lead to axle box bearing failures.Therefore,it is extremely important to study the mechanism of axle box bearings.Firstly,the medium of thermal deformation establishes a coupling relationship between the system dynamics model and the thermal grid model,and then obtains the thermal force coupling model of the high-speed train axle box bearing.The coupling model is validated from the perspectives of system dynamics response and temperature response,proving its effectiveness in system dynamics response and temperature characteristic response.Comparing the coupling model with the dynamics model,it is found that thermal deformation complicates the dynamic re-sponse.Finally,using the Lundberg-Palmgren(L-P)bearing fatigue calculation method and damage accumu-lation theory,the bearing fatigue life is calculated,and it is found that thermal deformation deteriorates the bearing operating environment,reducing the bearing fatigue life.Finally,by comparing the bearing fatigue life under different working conditions,it is concluded that the faster the vehicle speed,the greater the load,and the smaller the initial radial clearance of the bearing,the fatigue life of the bearing is reduced.The shorter the lifespan.
文摘Research on high-speed railways is a relatively new yet highly significant field in Vietnam.Among its key components,train control signaling plays a critical role,as it directly affects various interconnected systems,including infrastructure,traction power supply,operational planning,and overall railway safety.This article focuses on evaluating the capacity of the line based on the types of signals suitable for high-speed railways that have been effectively implemented in several European countries and successfully adapted in China.The research and simulation are conducted using MATLAB software,a reliable and widely adopted tool in the scientific community.The findings demonstrate that under normal conditions,the European Railway Traffic Management System/European Train Control System(ERTMS/ETCS)Level 2 signaling can support up to 23.7485 trains/hour/direction.Meanwhile,ERTMS/ETCS Level 3 with full moving block can accommodate up to 30.8735 trains/hour/direction,and ERTMS/ETCS Level 3 with fixed virtual blocks up to 29.4694 trains/hour/direction.In emergency scenarios,ERTMS/ETCS Level 3 with full moving block reduces headway by 33.27%compared to CTCS Level 3,while ERTMS/ETCS Level 3 with fixed virtual blocks achieves a 28.78%reduction.Overall,the ERTMS/ETCS Level 3 emerges as a state-of-the-art signaling technology offering high capacity and operational efficiency,and is recommended as a forward-looking solution for future implementation in Vietnam.
基金Supported by the National Natural Science Foundation of China(Grant Nos.12393783,12302067,12172235,52072249)Joint Funds of the National Natural Science Foundation of China(Grant No.U24A2003)+3 种基金College Education Scientific Research Project of Hebei Province(Grant No.JZX2024006)Central Guiding Local Scientific and Technological Development Funding Project(Grant No.246Z2206G)the Key Research Project of China State Railway Group Co.,Ltd.(Grant No.N2024T009)S&T Program of Hebei(Grant No.21567622H).
文摘As China's high-speed railway technology advances,high-speed trains have emerged as a pivotal mode of transportation,instrumental in facilitating passenger and freight mobility while fostering robust regional eco-nomic and trade interactions.Nonetheless,the safety of train operations remains a paramount concern,prompting extensive research into the dynamic behavior of critical components,which is essential to ensuring seamless and secure transportation services.This article commences by comprehensively reviewing the current landscape and evolutionary trajectory of dynamic model analysis for both traditional bearings and axle box bearings.Emphasis is placed on elucidating the profound influence of diverse bearing fault types on the system's kinematic state,alongside delving into the research methodologies employed in developing multi-physics field coupling models.Subsequently,it expounds on the content of investigations focusing on various wheel and track impairments,grounded in the dynamic modeling of the bearing vehicle coupling system.Concurrently,the intricate interplay between wheel-rail excitation and axle box bearing faults on the system's performance is elucidated.Concludingly,the article underscores the inadequacy of current multi-source fault diagnosis meth-odologies in tackling the intricacies of complex train operating environments,thereby highlighting its sig-nificance as a pressing and vital research agenda for the future.
基金sponsored by the National Natural Science Foundation of China(Grant No.52178100).
文摘The spatial offset of bridge has a significant impact on the safety,comfort,and durability of high-speed railway(HSR)operations,so it is crucial to rapidly and effectively detect the spatial offset of operational HSR bridges.Drive-by monitoring of bridge uneven settlement demonstrates significant potential due to its practicality,cost-effectiveness,and efficiency.However,existing drive-by methods for detecting bridge offset have limitations such as reliance on a single data source,low detection accuracy,and the inability to identify lateral deformations of bridges.This paper proposes a novel drive-by inspection method for spatial offset of HSR bridge based on multi-source data fusion of comprehensive inspection train.Firstly,dung beetle optimizer-variational mode decomposition was employed to achieve adaptive decomposition of non-stationary dynamic signals,and explore the hidden temporal relationships in the data.Subsequently,a long short-term memory neural network was developed to achieve feature fusion of multi-source signal and accurate prediction of spatial settlement of HSR bridge.A dataset of track irregularities and CRH380A high-speed train responses was generated using a 3D train-track-bridge interaction model,and the accuracy and effectiveness of the proposed hybrid deep learning model were numerically validated.Finally,the reliability of the proposed drive-by inspection method was further validated by analyzing the actual measurement data obtained from comprehensive inspection train.The research findings indicate that the proposed approach enables rapid and accurate detection of spatial offset in HSR bridge,ensuring the long-term operational safety of HSR bridges.
基金financially supported by the Swedish Transport Administration(Trafikverket)through the“Excellence Area 4”and FOI-BBT program(Grant Nos.BBT-2019-022 and BBT-TRV 2024/132497).
文摘Railway noise barriers are an essential piece of infrastructure for reducing noise propagation.However,these barriers experience aerodynamic loads generated by high-speed trains,leading to dynamic effects that may compromise their fatigue capacity.The most common structural design for railway noise barriers consists of vertical configurations of posts and panels.However,there have been few dynamic analyses of steel post/wood panel noise barriers under train-induced aerodynamic loads.This study used dynamic finite element analysis to assess the dynamic behavior of such noise barriers.Analysis of a 40-m-long noise barrier model and a triangular simplified load model,the latter of which effectively represented the detailed aerodynamic load,were first used to establish the model and input of the moving load during dynamic simulation.Then,the effects of different parameters on the dynamic response of the noise barrier were evaluated,including the damping ratio,the profile of the steel post,the span length of the panel,the barrier height,and the train speed.Gray relational analysis indicated that barrier height exhibited the highest correlations with the dynamic responses,followed by train speed,post profile,span length,and damping ratio.A reduction in the natural frequency and an increase in the train speed result in a higher peak response and more pronounced fluctuations between the nose and tail waves.The dynamic amplification factor(DAF)was found to be related to both the natural frequency and train speed.A model was proposed showing that the DAF significantly increases as the square of the natural frequency decreases and the cube of the train speed rises.
基金supported by the National Key Research and Development Program of China(2022YFA1404800)National Natural Science Foundation of China(12174107,12004221,12192254,92250304,W2441005,12334014,12192251)+4 种基金Natural Science Foundation of Shandong Province(ZR2024QA024,ZR2021ZD02)Postdoctoral Innovation Talents Support Program of Shandong Province(No.SDBX2019005)Shanghai Municipal Science and Technology Major ProjectFundamental Research Funds for the Central UniversitiesEngineering Research Center for Nanophotonics&Advanced Instrument,Ministry of Education,East China Normal University(No.2023nmc005)。
文摘We demonstrate a high-speed rotating slit beam shaping method for femtosecond(fs)laser three-dimensional(3D)isotropic inscription in glass materials.By integrating fs laser direct writing with a real-time rotating slit mechanism,a 3D symmetric spherical focal field distribution is created in the laser-irradiated regions of transparent substrates.The corresponding focal field distribution is theoretically calculated and validated by examining the features of laser-inscribed lines in glass samples.Moreover,we investigate the influences of laser writing speed and slit rotational speed on the fabrication resolution in glass,and discuss the formation mechanism of the generated periodic microstructures.To showcase its powerful capability for3D isotropic fabrication,the high-speed rotating slit beam shaping method is applied to create straight optical waveguides,bending optical waveguides,and hollow microchannels in the glass.The proposed method holds great potential for the facile manufacture of diverse 3D isotropic microstructures and devices within transparent materials across various applications,including advanced photonics,microoptics,micro-electromechanical systems,and microfluidics.
基金Under the auspices of Heilongjiang Provincial Natural Science Foundation of China(No.YQ2024D012),National Natural Science Foundation of China(No.42071162,42101165,42501220)。
文摘Under the background of‘the Belt and Road’and‘China-Mongolia-Russia Economic Corridor’initiatives,this paper studied the urban accessibility level,regional accessibility pattern and regional spatial effects along the Primorsky No.1 and No.2 transportation corridors.First,the evaluation of urban accessibility level with and without Primorsky No.1 and No.2 high-speed rails(HSRs)opening was conducted with two indicators,i.e.,the weighted average travel time,and the economic potential.After the evaluation,the spatial differentiation pattern of the accessibility changes with and without Primorsky No.1 and No.2 HSRs opening was performed respectively using ArcGIS.On these bases,the regional spatial effects brought by Primorsky No.1 and No.2 HSRs opening were studied.The results are as following.First,the urban accessibility level will be greatly improved by the opening of Primorsky No.1 and No.2 HSRs.All adjacent cities will be integrated into‘1 h HSR communication circle’and the whole journey will be integrated into‘4 h HSR communication circle’along Primorsky No.1 and No.2 corridors,respectively.The HSR accessibility of Primorsky No.1 corridor is stronger than that of Primorsky No.2 corridor.But the HSR accessibility improvement degree of Primorsky No.1 corridor is weaker than that of Primorsky No.2 corridor.Second,spatially,along Primorsky No.1 and No.2 corridors,the HSR accessibility level of the cities which are located in China is stronger than those cities located in Russia,showing the‘High West,Low East’patterns.The HSR accessibility improvement degree of the cities which are located in Russia and Sino-Russian border is stronger than those cities located in China,showing the‘High East,Low West’patterns.Third,Primorsky No.1 and No.2 corridors could connect the China’s‘Heilongjiang Land Sea Silk Road Economic Belt’and‘Changchun-Jilin-Tumen Development Pilot Zone’respectively,gradually involving into the development of China’s Harbin-Changchun Megalopolis.Relying on Harbin(China)and Changchun(China),Primorsky No.1 and No.2 HSRs could connect Northeast China-Beijing HSR,accelerating the diffusion of population,economy and other flows from China’s Beijing-Tianjin-Hebei Urban Agglomeration to Northeast China,and then to Russia’s Far East Federal District.Relying on Suifenhe(China)and Hunchun(China),Primorsky No.1 and No.2 HSRs could be conducive to the development of the second largest sea channels for Northeast China,creating the Northeast Asian Urban Belt,and new sea-rail intermodal pattern among China,Russia,Democratic People’s Republic of Korea,Japan and Republic of Korea.Relying on Vladivostok(Russia)and Zarubino(Russia),Primorsky No.1 and No.2 corridors could connect the‘Ice Silk Road’,building the‘Sino-Russian Northern Maritime Corridor’and‘Sino-Russian Arctic Blue Economic Areas’.
文摘Purpose–Regarding that Ultraviolet radiation,pollutant adsorption,and environmental changes may be the main reasons for the aging and yellowing on windshield rubber in high-speed trains,countermeasures are proposed to solve the aging and yellowing of windshield rubber and reduce the adverse effects caused by rubber yellowing.Design/methodology/approach–Scanning electron microscopy(SEM)and energy dispersive spectroscopy(EDS)were used to test the yellowed windshield rubber.Aging tests,including UVaging,natural aging and salt spray aging,were conducted to analyze the effects of aging on the windshield rubber.Different cleaning agents were selected to soak the windshield rubber,and the quality,hardness,and surface appearance of the rubber samples were tested.Findings–After UV aging,antioxidants migrated to the surface of the windshield rubber,but due to oxidation failure,they could not capture free radicals,leading to continued oxidation reactions within the material and resulting in yellowing of the rubber in a short period of time.Originality/value–Cleaning agents have a minimal impact on windshield rubber,UV aging has the greatest impact and natural aging is a gradual and slow deterioration process.Through daily deep cleaning and maintenance with protective agents at regular intervals,the deterioration of windshield rubber yellowing in high-speed trains can be effectively suppressed.
基金National Natural Science Foundation of China(811735648127402881274102)
文摘Objective To develop a suitable method for the large-scale separation of quinolone alkaloids from the fruits of Evodia rutaecarpa by high-speed counter-current chromatography （HSCCC）. Methods Two solvent systems were developed for the separation method. The upper phase was used as the stationary phase, and the lower phase was used as the mobile phase at 35 oCwith the flow rate of 2 mL/min and rotation speed of 855 r/min. Results Using the described method, 1-methyl-2-undecyl- 4（1H）-quinoione （1）, evocarpine （2）, 1-methy-2-[（6Z,9Z}]-6,9-pentade-cadienyl-4- （1H）-quinolone （3）, dihydroevocarpine （4）, and the mixture （5） of 1-methyl-2-[（z^- 10-pentadecenyl]-4（1H）-quinolone （Va） and 1 -methyl-2-[（Z^-6-pentadecenyl]- 4（1H）-quinolone （Vb） could be isolated from a petroleum ether extract. They were identified by 1H-NMR, ~3C-NMR, and MS/MS, and the purities were 94.3%, 95.2%, 96.8%, 98.3%, and 96.8%, respectively. Conclusion Five quinolone alkaloids from the fruits of E. rutaecarpa could be systematically isolated and purified using HSCCC. The presented method is simple and efficient with good potentials on the preparation of reference substances, especially on the quality control of Chinese materia medica.
文摘Objective To develop an efficient preparative method for the separation of Gelsemium alkaloids from Gelsemium elegans. Methods High-speed counter-current chromatography （HSCCC） with several two-phase solvent systems was investigated for the separation of Gelsemium alkaloids. The purity and structure identification of the purified compounds were performed with HPLC and NMR spectra, respectively. Results In a single operation, 206.6 mg of crude alkaloid sample was separated to yield 28.7 mg of koumine, 24.9 mg of gelsemine, 26.9 mg of humantenine, and 7.2 mg of gelsevirine, with the purities of 97.8%, 95.4%, 97.4%, and 93.5%, respectively. Conclusion A preparative HSCCC method is successfully established for the separation of four Gelsemium alkaloids from G. elegans with a modified two-phase solvent system com posed of n-hexane-ethyl acetate-ethanol-O. 5% triethylamine-H2O （3：5：3：4）.
基金Science and Technology Project of Zhuhai(PC20051072),2005
文摘Objective To develop an efficient method to isolate and purify the main components isoaloeresin D and aloin from Aloe vera for its industrial production.Methods High-speed counter-current chromatography was used to isolate isoaloeresin D and aloin in a one-step separation from dried crude extract of A.vera.The biphasic solvent system composed of hexane-ethyl acetate-acetone-water(0.2:5:1.5:5)was used at a flow rate of 1.0 mL/min,while the lipophilic phase was selected as the mobile phase and the apparatus was rotated at 840 r/min.The effluent was detected at 254 nm.Results Isoaloeresin D(53.1 mg)and aloin(106.9 mg)were separated from the crude extract(384.7 mg)with the purities of 98.6%and 99.5%,respectively.Conclusion HSCCC is a powerful technique for isolation and separation of chemical composition from aloe.
基金This work was financially supported by the National Key Research and Development Project(2018YFE0206000)National Natural Science Foundation of China(31901805,U1604234,31872914)Jiangsu Agriculture Science and Technology Innovation Fund(CX(19)3004).
文摘Rice false smut is an emerging plant disease worldwide.Ustiloxin A(UstA)is the major mycotoxin found in rice false smut balls,which are fungal colonies in rice florets.In this study,a new method consisting of macroporous resin column chromatography and high-speed countercurrent chromatography(HSCCC)was developed for UstA separation.UstA was extracted by a 3.81%HCOOH solution and adsorbed by XAD-4 resin.UstA was then eluted by a 40%methanol solution supplemented with 0.1%trifluoroacetic acid(TFA).Further purification was achieved by HSCCC using a two-phase solvent system consisting of n-butanol/TFA/H_(2)O(1/0.05/1,v/v/v).Under the optimized conditions,225 mg of UstA was obtained with a purity of 97.39%in a single run,with a final recovery of 65.2%.An inhibitory effect on seed germination of wheat and maize caused by UstA was observed in a preliminary phytotoxicity assay.
