A rate model, which considers axial dispersion, external mass transfer, intraparticle diffusion and nonlinear isotherms, and ports periodic switching is adopted to simulate the simulated moving bed （SMB） process. Th...A rate model, which considers axial dispersion, external mass transfer, intraparticle diffusion and nonlinear isotherms, and ports periodic switching is adopted to simulate the simulated moving bed （SMB） process. The effects of flow rate in Sections 2 and 3 and switching time on the operating performance parameters： purity, recovery, productivity and dcsorbent consumption are studied. A simulation approach is applied to simulate the operation and performance of the SMB. The model predicts the performance of the transient and cyclic steady state behavior to a reasonably good extent, and provides guidance operation condition of the SMB process.展开更多
The parameter identification model of largr scale chromatography separation process is proposed. The Phase equilibrium constants and lumped mass transfer coefficients of sugar and reducing sugar adsorption on D1, D2 a...The parameter identification model of largr scale chromatography separation process is proposed. The Phase equilibrium constants and lumped mass transfer coefficients of sugar and reducing sugar adsorption on D1, D2 and D3 resins as well as the axial dispersion coefficients of the fluid through packed columns are determined by means of the pulse-response experiment technique with an inert substance as a tracer and the chromatography measuring technique. The elution curve calculated from these parameters is good agreement with the experimental elution curve. The sensitivity analysis of these parameters is carried out, and the ressult shows that the elation curves of chromatography separation are more sensitive to the variations Of the Phase equilibrium relationship than to the variation of the axial dispersion as well as the lumped mass transfer coefficients.展开更多
Sediment samples obtained from the South Mid-Atlantic Ridge were analyzed for the major and trace elements by inductively coupled plasma atomic emission spectroscopy and inductively coupled plasma mass spectrometry. R...Sediment samples obtained from the South Mid-Atlantic Ridge were analyzed for the major and trace elements by inductively coupled plasma atomic emission spectroscopy and inductively coupled plasma mass spectrometry. Results revealed that the contents of elements(e.g., Fe, Mn, Cu, Zn, V, Co) were high in samples 22V-TVG10 and 26V-TVG05 from the sites near the hydrothermal areas, and low in sample 22V-TVG14, which was collected far from the hydrothermal areas. The contents of Ca, Sr and Ba in the samples showed opposite trends. A positive correlation between the concentrations of metallic elements(Cu, Zn, Co, Ni, Pb, V) and Fe in the samples were observed. These results are consistent with chemical evolution of the dispersing hydrothermal plume.展开更多
Two-color resonant two-photon mass-analyzed threshold ionization （MATI） spectroscopy was used to record the vibrationally resolved cation spectra of the selected rotamers of p- ethoxyphenol. The adiabatic ionization...Two-color resonant two-photon mass-analyzed threshold ionization （MATI） spectroscopy was used to record the vibrationally resolved cation spectra of the selected rotamers of p- ethoxyphenol. The adiabatic ionization energies of the trans and cis rotamers are determined to be 61565±5 and 61670±5 cm^-1, which are less than that of p-methoxyphenol by 645 and 643 cm^-1, respectively. Analysis on the MATI spectra of the selected rotamers of p-ethoxyphenol cation shows that the relative orientation of the ethoxy group has little effect on the in-plane ring vibrations. The low-frequency OC2H5 bending vibrations appear to be active for both forms of the cation.展开更多
The emission of CuInSe2-based spark discharge plasma at atmospheric pressure in air has been investigated by optical emission spectroscopy method. The plasma was formed by action of the high voltage pulse generator （...The emission of CuInSe2-based spark discharge plasma at atmospheric pressure in air has been investigated by optical emission spectroscopy method. The plasma was formed by action of the high voltage pulse generator （with nanosecond pulse） on the corresponding electrodes （CulnSe2 compound）. The emission characteristics have been obtained for the spark discharge plasma at 3 mm interelectrode distance. It was established that the spark discharge plasma radiation was determined by decay products of the compound from which electrodes were made. The most suitable spectral lines for plasma diagnostics is atomic copper lines in the visible spectrum and atomic indium lines in UV （ultraviolet） and visible spectrum.展开更多
The Spurge family （Euphorbiaceae） is a large family of flowering plants. Two plant species of this family were collected from the Egyptian desert, extracted with methanol subjected to silica gel column chromatograph...The Spurge family （Euphorbiaceae） is a large family of flowering plants. Two plant species of this family were collected from the Egyptian desert, extracted with methanol subjected to silica gel column chromatography to give six compounds, three compounds from each plant. The compounds isolated from the methanol extract of Euphorbia retusa Forssk were identified as kaempferol-3-beta-D glucopyranosyl （1）, 3-O-alpha-L-xylopyranosyl （1→3）-alpha-L xylopyranosyl （1→2）, beta-D glucopyranosyllup 1,12-diene-3,21-diol （2） and 5,7,8,3＇,4＇-pentahydroxy-3-methoxyflavone （3） and the compounds isolated from Euphorbia paralais L. identified as 3,5,3＇-trihydroxy-6,7-d-methoxy-4＇ （7＂-hydroxygeranyl-1＂-ether） flavones （4）, 3-O-syringic acid （1→4）-alpha-L- xylopyranosyl （1→3）, beta-D-rahminopyranosyl hederagenin （5） and 3-O-syringic acid （1→4）, beta-D-rahminopyranosyl （1→3）,beta-D-rahminopyranosyl hederagenin （6）. The structure of the isolated compounds was elucidated by chemical and spectrometric analysis such as Infera red （IR）, proton and carbon nuclear magnetic resonance （1H-, 13C-NMR） and chemical ionization mass spectrometry （CI-MS）.展开更多
In this paper, we proposed a novel resolution criterion（improved calibrated normalized resolution product, r＊＇） to evaluate separation quality of fingerprints. By comparing with the calibrated normalized resolutio...In this paper, we proposed a novel resolution criterion（improved calibrated normalized resolution product, r＊＇） to evaluate separation quality of fingerprints. By comparing with the calibrated normalized resolution product（r＊） and the hierarchical chromatographic response function（HCRF）, the validity of this criterion was demonstrated by experimental chromatograms. The soy isoflavone extract was selected as the analytical object. The initial and end percentages of methanol and elution time affecting gradient elution were tested by orthogonal design. The final optimized conditions were as follows. It was detected by UV absorbance at 254 nm, column temperature was maintained at 36 oC, solvent A was 0.1%（v/v） acetic acid, solvent B was methanol, gradient elution was from 34% to 65% B in a linear gradient in 25 min, and the flow-rate was set at 1.0 m L/min. In addition, the main ingredients of the soy isoflavone extract were confirmed by LC-ESI/MS.展开更多
The objective of the present study is to develop a method for large-scale separating and purifying salidroside from rhodiola kirilowii roots and for preparing injectable medicinal ingredient.Crude extract of salidrosi...The objective of the present study is to develop a method for large-scale separating and purifying salidroside from rhodiola kirilowii roots and for preparing injectable medicinal ingredient.Crude extract of salidroside was prepared by water-ethanol system,and purified by column chromatography of macroporous resins.Static adsorption and desorption studies were performed on six kinds of macroporous resins,and SP825 resin was chosen,followed by optimizing process parameters.The optimum sample volume,feed concentration,ratio of diameter to height,and feeding flow rate were 1.5 bed volumes(BV),15 mg/mL,1:10 and 1 BV/h,respectively.Dynamic desorption was performed consecutively with 8 BV of distilled water,3 BV of 5% ethanol and 8 BV of 10% ethanol at a flow rate of 2 BV/h.After three cycles in separating 3.5 tons of rhodiola kirilowii roots,salidroside purity was increased from 3.4% in the crude extract to 93.6% in purified salidroside product.This study provides a novel method to separate salidroside for injectable use.展开更多
Several gentamicin bulk samples from different origins were investigated using an LC/MS method.LC equipped with ion trap MS with positive ionization was performed on a Capcell Pak C18(AQ) column with the mobile phase ...Several gentamicin bulk samples from different origins were investigated using an LC/MS method.LC equipped with ion trap MS with positive ionization was performed on a Capcell Pak C18(AQ) column with the mobile phase containing 50 mM trifluoroacetic(TFA) and methanol.Impurities present in batches of gentamicin bulk samples were elucidated and compared according to their fragmentation behavior.In total seventeen impurities present in samples,five impurities were not elucidated and two compounds were identified preliminarily.It was observed that the impurity profiles were different in samples from different origins which indicate necessity in the quality control of gentamicin.展开更多
基金Supported by the Doctoral Program Foundation of the Institution of Higher Education of China (No.20040335045).
文摘A rate model, which considers axial dispersion, external mass transfer, intraparticle diffusion and nonlinear isotherms, and ports periodic switching is adopted to simulate the simulated moving bed （SMB） process. The effects of flow rate in Sections 2 and 3 and switching time on the operating performance parameters： purity, recovery, productivity and dcsorbent consumption are studied. A simulation approach is applied to simulate the operation and performance of the SMB. The model predicts the performance of the transient and cyclic steady state behavior to a reasonably good extent, and provides guidance operation condition of the SMB process.
文摘The parameter identification model of largr scale chromatography separation process is proposed. The Phase equilibrium constants and lumped mass transfer coefficients of sugar and reducing sugar adsorption on D1, D2 and D3 resins as well as the axial dispersion coefficients of the fluid through packed columns are determined by means of the pulse-response experiment technique with an inert substance as a tracer and the chromatography measuring technique. The elution curve calculated from these parameters is good agreement with the experimental elution curve. The sensitivity analysis of these parameters is carried out, and the ressult shows that the elation curves of chromatography separation are more sensitive to the variations Of the Phase equilibrium relationship than to the variation of the axial dispersion as well as the lumped mass transfer coefficients.
基金the National Natural Science Foundation of China (No. 41306053)the Open Fund of the Key Laboratory of Marine Geology and Environment, Chinese Academy of Sciences (Nos. MGE 2015KG04 and MGE2015KG01)+2 种基金the Open Fund of the Key Laboratory of Submarine Geosciences, State Oceanic Administration, People’s Republic of China (No. KSLG 1503)the Special Fund for the Taishan Scholar Program of Shandong Province (No. ts201511061)The authors would like to thank the crews of the COMRA cruises (DY115-22 and DY115-26)
文摘Sediment samples obtained from the South Mid-Atlantic Ridge were analyzed for the major and trace elements by inductively coupled plasma atomic emission spectroscopy and inductively coupled plasma mass spectrometry. Results revealed that the contents of elements(e.g., Fe, Mn, Cu, Zn, V, Co) were high in samples 22V-TVG10 and 26V-TVG05 from the sites near the hydrothermal areas, and low in sample 22V-TVG14, which was collected far from the hydrothermal areas. The contents of Ca, Sr and Ba in the samples showed opposite trends. A positive correlation between the concentrations of metallic elements(Cu, Zn, Co, Ni, Pb, V) and Fe in the samples were observed. These results are consistent with chemical evolution of the dispersing hydrothermal plume.
文摘Two-color resonant two-photon mass-analyzed threshold ionization （MATI） spectroscopy was used to record the vibrationally resolved cation spectra of the selected rotamers of p- ethoxyphenol. The adiabatic ionization energies of the trans and cis rotamers are determined to be 61565±5 and 61670±5 cm^-1, which are less than that of p-methoxyphenol by 645 and 643 cm^-1, respectively. Analysis on the MATI spectra of the selected rotamers of p-ethoxyphenol cation shows that the relative orientation of the ethoxy group has little effect on the in-plane ring vibrations. The low-frequency OC2H5 bending vibrations appear to be active for both forms of the cation.
文摘The emission of CuInSe2-based spark discharge plasma at atmospheric pressure in air has been investigated by optical emission spectroscopy method. The plasma was formed by action of the high voltage pulse generator （with nanosecond pulse） on the corresponding electrodes （CulnSe2 compound）. The emission characteristics have been obtained for the spark discharge plasma at 3 mm interelectrode distance. It was established that the spark discharge plasma radiation was determined by decay products of the compound from which electrodes were made. The most suitable spectral lines for plasma diagnostics is atomic copper lines in the visible spectrum and atomic indium lines in UV （ultraviolet） and visible spectrum.
文摘The Spurge family （Euphorbiaceae） is a large family of flowering plants. Two plant species of this family were collected from the Egyptian desert, extracted with methanol subjected to silica gel column chromatography to give six compounds, three compounds from each plant. The compounds isolated from the methanol extract of Euphorbia retusa Forssk were identified as kaempferol-3-beta-D glucopyranosyl （1）, 3-O-alpha-L-xylopyranosyl （1→3）-alpha-L xylopyranosyl （1→2）, beta-D glucopyranosyllup 1,12-diene-3,21-diol （2） and 5,7,8,3＇,4＇-pentahydroxy-3-methoxyflavone （3） and the compounds isolated from Euphorbia paralais L. identified as 3,5,3＇-trihydroxy-6,7-d-methoxy-4＇ （7＂-hydroxygeranyl-1＂-ether） flavones （4）, 3-O-syringic acid （1→4）-alpha-L- xylopyranosyl （1→3）, beta-D-rahminopyranosyl hederagenin （5） and 3-O-syringic acid （1→4）, beta-D-rahminopyranosyl （1→3）,beta-D-rahminopyranosyl hederagenin （6）. The structure of the isolated compounds was elucidated by chemical and spectrometric analysis such as Infera red （IR）, proton and carbon nuclear magnetic resonance （1H-, 13C-NMR） and chemical ionization mass spectrometry （CI-MS）.
基金National Higher-Education Institution General Research and Development Funding(Grant No.JKP2011010)
文摘In this paper, we proposed a novel resolution criterion（improved calibrated normalized resolution product, r＊＇） to evaluate separation quality of fingerprints. By comparing with the calibrated normalized resolution product（r＊） and the hierarchical chromatographic response function（HCRF）, the validity of this criterion was demonstrated by experimental chromatograms. The soy isoflavone extract was selected as the analytical object. The initial and end percentages of methanol and elution time affecting gradient elution were tested by orthogonal design. The final optimized conditions were as follows. It was detected by UV absorbance at 254 nm, column temperature was maintained at 36 oC, solvent A was 0.1%（v/v） acetic acid, solvent B was methanol, gradient elution was from 34% to 65% B in a linear gradient in 25 min, and the flow-rate was set at 1.0 m L/min. In addition, the main ingredients of the soy isoflavone extract were confirmed by LC-ESI/MS.
基金supported by Puning Kangmei Pharmaceutical Co.,Ltd.in part by Comprehensive Center for Drug Discovery and Development of Peking University
文摘The objective of the present study is to develop a method for large-scale separating and purifying salidroside from rhodiola kirilowii roots and for preparing injectable medicinal ingredient.Crude extract of salidroside was prepared by water-ethanol system,and purified by column chromatography of macroporous resins.Static adsorption and desorption studies were performed on six kinds of macroporous resins,and SP825 resin was chosen,followed by optimizing process parameters.The optimum sample volume,feed concentration,ratio of diameter to height,and feeding flow rate were 1.5 bed volumes(BV),15 mg/mL,1:10 and 1 BV/h,respectively.Dynamic desorption was performed consecutively with 8 BV of distilled water,3 BV of 5% ethanol and 8 BV of 10% ethanol at a flow rate of 2 BV/h.After three cycles in separating 3.5 tons of rhodiola kirilowii roots,salidroside purity was increased from 3.4% in the crude extract to 93.6% in purified salidroside product.This study provides a novel method to separate salidroside for injectable use.
文摘Several gentamicin bulk samples from different origins were investigated using an LC/MS method.LC equipped with ion trap MS with positive ionization was performed on a Capcell Pak C18(AQ) column with the mobile phase containing 50 mM trifluoroacetic(TFA) and methanol.Impurities present in batches of gentamicin bulk samples were elucidated and compared according to their fragmentation behavior.In total seventeen impurities present in samples,five impurities were not elucidated and two compounds were identified preliminarily.It was observed that the impurity profiles were different in samples from different origins which indicate necessity in the quality control of gentamicin.
