To develop a simple and rapid purification method of rohitukine from the stem bark of Dysoxylum binectariferum. A L9 (34) orthogonal test was designed to optimize the extraction condition. Rohitukine in the plant e...To develop a simple and rapid purification method of rohitukine from the stem bark of Dysoxylum binectariferum. A L9 (34) orthogonal test was designed to optimize the extraction condition. Rohitukine in the plant extract was purified by using solvent-solvent partition and cation exchange resion (CER). Five different types of packing materials, including XAD-2 resin, polyamide, Sephadex LH-20, ODS and CER, were compared and CER showed the best capacity for rohitukine separation. The purification procedure was optimized as follows: the plant material powder was extracted with 70% ethanol (v/m = 60) by ultrasonic agitation for 60 min, then the 70% ethanol extract was dissolved in aqueous solution (pH 1, adjusted with 0.5 mol/L HCl) and extracted with equal volume of n-butanol. The aqueous layer was retained and the pH was adjusted to 10 with 25% aqueous ammonia and a solventsolvent partition was performed with equal volume of n-butanol. The obtained n-butanol extract was dissolved in aqueous solution (pH 1, adjusted with 0.5 mol/L HCl), and purified by a CER column eluting with H2O and 70% ethanol (pH 10, adjusted with 25% aqueous ammonia), successively. Rohitukine existed in 70% ethanol eluate, with a purity up to 53.3%. The method developed in this study provides a simple and rapid approach for the preparation of rohitukine from the stem bark ofD. binectariferum.展开更多
The solvent extraction of copper from simulated ammoniacal spent etchant with 1-(4'-dodecyl)-phenyl-3-tertiary butyl-1,3-octadione(HR) was studied,and a model of extraction isotherm was proposed and verified with...The solvent extraction of copper from simulated ammoniacal spent etchant with 1-(4'-dodecyl)-phenyl-3-tertiary butyl-1,3-octadione(HR) was studied,and a model of extraction isotherm was proposed and verified with equilibrium extraction constant.The influence of equilibration time,extractant concentration and phase ratio on the extraction of copper was studied at(298±0.5) K.For the spent etching solutions containing 112.98 g/L Cu,6 mol/L NH3 and 1 mol/L NH4+,the optimal solvent extraction condition of copper was obtained in one-stage solvent extraction at phase ratio of 5:4 with 40% HR in sulphonated kerosene for 5 min.The copper concentration in the raffinate decreased to 63.24 g/L and raffinate can be favorably recycled to the etching solution.The stripping studies were carried out with the simulated copper spent electrolyte containing 30 g/L Cu and 180 g/L H2SO4.The stripping ratio is 98.27% from the loaded organic phase after one-stage stripping at phase ratio of 1:2 at(298±0.5) K.展开更多
In order to investigate the effect of magnetic field on the liquid-liquid extraction, the extraction in the acetone-water-trichloroethane system was studied under magnetic field with different magnetic induction inten...In order to investigate the effect of magnetic field on the liquid-liquid extraction, the extraction in the acetone-water-trichloroethane system was studied under magnetic field with different magnetic induction intensity.The results showed that the effect of magnetic field was positive in the extraction process, and the partition coeffi-cient and the yield of acetone increased-with the increasing magnetic induction intensity by 5.16%-8.35% and 1.85%-5.70% respectively. The effect of magnetic field on the extraction was intensified when the temperature became, higher. The experimental data of the partition coefficient of acetone were correlated by the method of least square in terms of a power-law correlation.展开更多
For the determination of salicylaldoxime in environmental water samples,a stable and rapid method with low detection was proposed and established,based on the liquid-liquid extraction-high performance liquid chromatog...For the determination of salicylaldoxime in environmental water samples,a stable and rapid method with low detection was proposed and established,based on the liquid-liquid extraction-high performance liquid chromatography with ultraviolet detector.Parameters including extraction solvent,ionic strength,solution pH,and extraction pattern were discussed for the optimal quantification of salicylaldoxime-spiked water.When the described method was applied to four spiked water samples,the obtained average extraction recovery rate was found between 87%–107%and relative standard deviation was below 6%.At the same time,good linear relationships were observed for spiked water samples from 0.01 to 10μg/mL(R2=0.9993).In addition,the detection limit of salicylaldoxime was revealed between 0.003–0.008μg/mL,which is two orders of magnitude lower than previously reported results.Thus,the presented method may be advantageous for the high-efficiency determination of salicylaldoxime in water samples.展开更多
Teicoplanin is one of the macrocyclic glycopeptide antibiotics, which is active against Gram-positive bacteria, and has attracted a lot of attention in the field of chiral separation recently. In this work, the partit...Teicoplanin is one of the macrocyclic glycopeptide antibiotics, which is active against Gram-positive bacteria, and has attracted a lot of attention in the field of chiral separation recently. In this work, the partition coefficients and extraction ratio of teicoplanin in three different solvent systems were studied: conventional extraction, reactive extraction and reverse micelle extraction. With conventional solvent extraction, n-butanol demonstrated high partition coefficient for teicoplanin, but low extraction ratio because of its high solubility in water. Reactive extraction of teicoplanin showed the highest partition coefficient with almost 100% recovery in organic phase when tri-n-octylmethyl ammonium chloride (TOMAC) was used as extractant and pH value was above 5.0. A reverse micelle system, consisted of isooctane +10mmol-L-1 TOMAC +1% n-octanol, also offered high separation factor for teicoplanin. The results are beneficial for the design of teicoplanin separation and purification process.展开更多
The use of the guanidine extractant LIX 7950 extracting copper and cyanide from alkaline cyanide solution was investigated.The extraction of copper and cyanide under different initial copper and extractant concentrati...The use of the guanidine extractant LIX 7950 extracting copper and cyanide from alkaline cyanide solution was investigated.The extraction of copper and cyanide under different initial copper and extractant concentrations was examined and the stoichiometric extraction constant of Cu(CN)32- with LIX 7950 was calculated.Both the distribution coefficient and the stoichiometric extraction constant of Cu(CN)3 2-with LIX 7950 decrease when the temperature is varied from 25℃to 45℃, indicating the extraction process is exothermic.The calculated enthalpy change of the reaction(-HΘ)is about-190 kJ/mol.The copper extraction isotherms under different molar ratios of cyanide to copper are established.The preferential extraction of Cu(CN)32- over Cu(CN)4 3-and CN -has been confirmed and a high cyanide-to-copper molar ratio tends to suppress copper loading. The loaded copper and cyanide can be stripped efficiently by the moderately strong NaOH solutions(0.5-1.0 mol/L)and the presence of NaCN in the stripping solution facilitates copper stripping.展开更多
A highly sensitive SPE-liquid/liquid extraction RPLC method has been developed for the analysis of 6β-hydroxycortisol and cortisol in the urine of cancer patients. Methods: After SPE column purification and liquid-l...A highly sensitive SPE-liquid/liquid extraction RPLC method has been developed for the analysis of 6β-hydroxycortisol and cortisol in the urine of cancer patients. Methods: After SPE column purification and liquid-liquid extraction, the sample test solutions were analyzed with RPLC using a C18 analytical column. This improved analytical method has been validated for linearity, accuracy (recovery from urine), repeatability (within-day and between-day precision), specificity, sensitivity, and stability. This SPE-liquid/liquid extraction-RPLC is rapid, simple, accurate and reproducible. The technique is particularly useful for monitoring the CYP3A activity of cancer patients in clinical settings. The results are expressed as the ratio of 6β-hydroxycortisol to cortisol. Results: The CYP3A activity from a total of 153 samples was measured using this improved method. Considerable variation in the CYP3A activity of different cancer patients has been documented. Thus, personalized medical treatment based on the individual metabolic enzyme activity level is necessary. Conclusion: This new analytical method facilitates such individualized medical treatments.展开更多
Liquid-liquid equilibrium (LLE) data for the ternary systemwater-ethanol-dimethyl succinate have been determined experimentallyat temperatures ranging from 298.15 to 318.15 K at 5 K intervals.Complete phase diagrams w...Liquid-liquid equilibrium (LLE) data for the ternary systemwater-ethanol-dimethyl succinate have been determined experimentallyat temperatures ranging from 298.15 to 318.15 K at 5 K intervals.Complete phase diagrams were obtained by determining solubility andthe tie-line data. Tie-line compositions were correlated byOthmer-Tobias method. The universal quasichemical functional groupactivity coefficient (UNIFAC) and modified UNIFAC methods were usedto predict the phase equilibrium in the system using the interactionparameters deter- Mined from experimental data between groups CH_3,CH_2, OH, CH_3 COO and H_2O.展开更多
In this work, mass transfer mechanism was studied for 50%TBP (in kerosene)-phenol-water as the working system in different hydrophobic microporous hollow fiber modules. The effect of different operating conditions on ...In this work, mass transfer mechanism was studied for 50%TBP (in kerosene)-phenol-water as the working system in different hydrophobic microporous hollow fiber modules. The effect of different operating conditions on the removal of phenol was analyzed. Solvent entrainment in this process was detected with MALVERN-2600 laser pellet diameter analytical equipment. Experimental results indicate the mass transfer coefficient is increased while the two phase flow rates are increased. With increases in the flow rate of the water phase, the removal ratio of phenol will be decreased. Highly effective removal of phenol could be reached by changing the experimental conditions and the module configuration. The solvent entrainment in the water phase in the membrane extraction process was found to be 5%—8% of that in conventional liquid-liquid extraction process. Thus, solvent pollution could be better controlled.展开更多
Liquid phase oxidation of toluene is an environmental benign route for the production of benzoic acid.In a φ48mm bubble column reactor,the commercial process of toluene liquid phase oxidation was conducted with Co(CH...Liquid phase oxidation of toluene is an environmental benign route for the production of benzoic acid.In a φ48mm bubble column reactor,the commercial process of toluene liquid phase oxidation was conducted with Co(CH3COO)2.4H2O as catalyst.The Co2+ concentration [Co2+] was determined by extraction spectrophotometry and hereby the Co3+ concentration [Co3+] was obtained by mass balance.The results showed that [Co3+] reached the maximum at about 25-30min.[Co3+] increased with increasing Co catalyst amount at total Co concentration<150 mg.L-1 of toluene.The conversion of toluene,yield and selectivity of benzoic acid increased with the increasing [Co3+/Co2+] max.A high [Co3+] and a high [Co3+]/[Co2+] ratio are beneficial to the reaction.展开更多
In the past ^68Ge (Germanium-68) was purified with toxic organic solvents in liquid-liquid extractions making the product unacceptable by the FDA (food and drug Administration) for human use. The authors report in...In the past ^68Ge (Germanium-68) was purified with toxic organic solvents in liquid-liquid extractions making the product unacceptable by the FDA (food and drug Administration) for human use. The authors report initial studies utilizing three or four columns consisting of sequences of AG 1, AG50, Chelex 100 and/or Sephadex G25 resins. Five purification methods were examined and a separation consisting of the sequence: AG 1-Chelex100-Sephedex G25 provided 87% recovery of germanium. Fractionation of the elution resulted in high germanium concentrations.展开更多
When evaluating ionic liquids (ILs) for extractive desulfurization (EDS) of fuel oils, the inevitable presence of water in the system may have a significant and in many cases strongly negative effect. However, few...When evaluating ionic liquids (ILs) for extractive desulfurization (EDS) of fuel oils, the inevitable presence of water in the system may have a significant and in many cases strongly negative effect. However, few studies have considered this particular issue and a promoted water effect on EDS is scarcely reported. In this work, COSMO-RS was firstly employed to calculate the capacity and selectivity for EDS of various IL/H20 mixtures, which cover different IL characters and a wide water concentration range. Experiments were then conducted with a representative IL [C4MIM]IH2P04], whose stable and even promoted extraction performance with a small amount of water was suggested by COSMO-RS. Through analyses of the desulfurization ratio, the cross- solubility and the water content in the desulfurized fuel, the promoted effect of water within a certain range (〈 10 wt%) was experimentally demonstrated. Moreover, such effect of water was explained combining the viscosity, the solvent-solute interactions and the COSMO-RS based analysis.展开更多
In this work, the COSMO-RS (conductor like screening model for real solvent) model algorithm was derived from the modified Rachford rice method. It could be more helpful to investigate the phase behavior of binary s...In this work, the COSMO-RS (conductor like screening model for real solvent) model algorithm was derived from the modified Rachford rice method. It could be more helpful to investigate the phase behavior of binary systems with the help of quantum chemical calculation at 6-31G* basis set. COSMO-RS was used to predict solubility of binary mixture involving non-ILs (ionic liquids), and ILs systems are: benzyl ethylamine + glycerol system (Type-Ⅰ), nitro methane + cyclohexane system (Type-Ⅱ), dipropylamine + water system (Type-Ⅲ), 1,2-ethanediol + thiophene system (Type-Ⅳ), [1,2-DMIM] [salicylate] + thiophene (Type-Ⅳ), and [EMIM] [NO3] + thiophene (Type-Ⅳ). Totally 15 cations with 27 anions were used for generating 405 binary LLE (liquid liquid equilibrium) systems involving thiophene. However, the predicted COSMO-RS values are consisting with the reported experimental values. Furthermore, the immiscibility gap at 298.15 K was determined and compared for various ILs. It was found that l-butylpyrrolidinium, l-octylquinolinium, 1-octylpyridinium and 1-octyl-3-methylimidazolium based cations are most suitable for thiophene extraction from any liquid mixture.展开更多
A number of synergistic solvent extraction (SSX) systems have been developed to recover nickel, cobalt, zinc and copper from sulphuric and chloride leach solutions by the solvent extraction team of CSIRO, Australia....A number of synergistic solvent extraction (SSX) systems have been developed to recover nickel, cobalt, zinc and copper from sulphuric and chloride leach solutions by the solvent extraction team of CSIRO, Australia. These in- clude (1) Versatic 10/CLXS0 system for the separation of Ni from Ca in sulphate solutions, (2) Versatic 10/4PC system for the separation of Ni and Co from Mn/Mg/Ca in sulphate solutions, (3) Cyanex 471X/HRJ-4277 system for the separation of Zn from Cd in sulphate solutions, (4) Versatic 10/LIX63 system for the separation of Co from Mn/Mg/Ca in sulphate solutions, (5) Versatic 10/LIX63/TBP system for separation of Ni and Co from Mn/Mg/Ca in sulphate solutions, (6) Versatic 10/LIX63 system for the separation of cobalt from nickel in sulphate solutions by difference in kinetics, (7) Cyanex 272/LIX84 system for the separation of Cu/Fe/Zn from Ni/Co in sulphate solutions, (8) Versatic 10/LIX63fFBP system to recover Cu/Ni from strong chloride solutions, and [9) Versatic 10/LIX63 system to separate Cu from Fe in strong chloride solutions. The synergistic effect on metal separation and efficiency is presented and possible industrial applications are demonstrated. The chemical stability of selected SSX systems is also reported.展开更多
Based on the interfacial ligand exchange model and the law of conservation of mass, the multi-stage enantioselective liquid-liquid extraction model has been established to analyze and discuss on multi-stage centrifuga...Based on the interfacial ligand exchange model and the law of conservation of mass, the multi-stage enantioselective liquid-liquid extraction model has been established to analyze and discuss on multi-stage centrifugal fractional extraction process of4-nitrobenzene glycine (PGL) enantiomers. The influence of phase ratio, extractant concentra- tion, and PFff concentration on the concentrations of enantiomers in the extract and raffinate was investigated by experiment and simulation. A good agreement between model and experiment was obtained. On this basis, the influence of many parameters such as location of stage, concentration levels, extractant excess, and number of stages on the symmetric separation performance was simulated. The optimal location of feed stage is the middle of fractional extraction equipment. The feed flow must satisfy a restricted relationship on flow ratios and the liquid throughout of centrifugal device. For desired purity specification, the required flow ratios decrease with extractant concentration and increase with PFff concentration. When the number of stages is 18 stages at extractant excess of 1.0 or 14 stages at extractant excess of 2.0, the eeeo (equal enantiomeric excess) can reach to 99%展开更多
The ternary phase diagrams of musk ketone, musk xylene and various solvent were obtained by calcu- lations. Moreover, the double saturated lines were found to be curve for the first time. The methods to separate eutec...The ternary phase diagrams of musk ketone, musk xylene and various solvent were obtained by calcu- lations. Moreover, the double saturated lines were found to be curve for the first time. The methods to separate eutectic mixtures of musks by solution crystallization were suggested on the basis of these phase diagrams. A new process was proposed to get musk ketone and musk xylene from the eutectics by adding acetonitrile and heptane in turn, which was verified by experiments. Musk xylene with purity of 97.50% and musk ketone with purity of 98.10% were obtained.展开更多
A new HPLC-UV method was developed and validated for the quantitative determination of epidermal growth factor receptor inhibitor erlotinib in the plasma of tumor bearing BALB/c nude mice.Erlotinib and its internal st...A new HPLC-UV method was developed and validated for the quantitative determination of epidermal growth factor receptor inhibitor erlotinib in the plasma of tumor bearing BALB/c nude mice.Erlotinib and its internal standard l-(3-((6,7-bis(2- methoxyethoxy)quinazolin-4-yl)amino)phenyl)ethanone were extracted from mice plasma samples using liquid-liquid extraction with a mixed solvent of methyl t-butyl ether and ethyl acetate(9:1,v/v).Chromatographic separation was performed on a Luna C|_(18)column(4.6 mm×250 mm,5μm)with acetonitrile:5 mM potassium phosphate buffer pH=5.2(41:59,v/v)as the mobile phase.UV detector was set at the wavelength of 345 nm,and the flow rate was 1.0 mL/min.The calibration curve was linear over the range of 20-10 000 ng/mL with acceptable intra-and inter-day precision and accuracy.The intra-day and inter-day precisions were within the range of 1.69%—5.66%,and the accuracies of intra-and inter-day assays were within the range of 105%—113%. The mean recoveries were 85.2%and 96.1%for erlotinib and IS,respectively.This method was successfully applied to a pharmacokinetic study in tumor bearing BALB/c nude mice following single oral administration at the dose of 12.5 mg/kg. The main pharmacokinetic parameters were as follows:C_(max)was 4.67μg/mL,T_(max)was 1.0 h,T_(1/2)was 2.78 h,and AUC_(0-24h)was 18.0μg/mL·h.展开更多
A simple and rapid method of ionic liquid based dispersive liquid-liquid microextraction (DLLME) combining with high performance liquid chromatography (HPLC) was developed for the analysis of four toxic anilines i...A simple and rapid method of ionic liquid based dispersive liquid-liquid microextraction (DLLME) combining with high performance liquid chromatography (HPLC) was developed for the analysis of four toxic anilines in flour steamed bread and maize steamed bread. Several possible influential factors such as the type of ionic liquid and disperser solvent, extraction time, sample pH, ionic strength and the volume of ionic liquid and disperser solvent were optimized using single factor experiments and orthogonal array design (OAD) with OA25(54) matrix. Analysis of variance (ANOVA) and percent contribution (PC) were used to investigate the significance of the factors of OAD. Sample pH and ionic strength are statistically demonstrated two chief factors. Under the optimum condition, the method exhibits a good linearity (r2 〉 0.99) over the studied range (50-1000 ng g-l) for anilines. The extraction factors and recoveries for the anilines in two kinds of steamed breads ranged between 34.1%-73.3% and 44.3%-95.3%, respectively. The limit of detections (LODs) and limit of quantitations (LOQs) ranged be- tween 10-15 ng g-1 and 30--45 ng g-1.展开更多
基金Scientific Research Foundation for the Returned Overseas Chinese Scholars by Ministry of Education of China (Grant No.[2004]527).
文摘To develop a simple and rapid purification method of rohitukine from the stem bark of Dysoxylum binectariferum. A L9 (34) orthogonal test was designed to optimize the extraction condition. Rohitukine in the plant extract was purified by using solvent-solvent partition and cation exchange resion (CER). Five different types of packing materials, including XAD-2 resin, polyamide, Sephadex LH-20, ODS and CER, were compared and CER showed the best capacity for rohitukine separation. The purification procedure was optimized as follows: the plant material powder was extracted with 70% ethanol (v/m = 60) by ultrasonic agitation for 60 min, then the 70% ethanol extract was dissolved in aqueous solution (pH 1, adjusted with 0.5 mol/L HCl) and extracted with equal volume of n-butanol. The aqueous layer was retained and the pH was adjusted to 10 with 25% aqueous ammonia and a solventsolvent partition was performed with equal volume of n-butanol. The obtained n-butanol extract was dissolved in aqueous solution (pH 1, adjusted with 0.5 mol/L HCl), and purified by a CER column eluting with H2O and 70% ethanol (pH 10, adjusted with 25% aqueous ammonia), successively. Rohitukine existed in 70% ethanol eluate, with a purity up to 53.3%. The method developed in this study provides a simple and rapid approach for the preparation of rohitukine from the stem bark ofD. binectariferum.
基金Project (2007CB613601) supported by the National Basic Research Program of China
文摘The solvent extraction of copper from simulated ammoniacal spent etchant with 1-(4'-dodecyl)-phenyl-3-tertiary butyl-1,3-octadione(HR) was studied,and a model of extraction isotherm was proposed and verified with equilibrium extraction constant.The influence of equilibration time,extractant concentration and phase ratio on the extraction of copper was studied at(298±0.5) K.For the spent etching solutions containing 112.98 g/L Cu,6 mol/L NH3 and 1 mol/L NH4+,the optimal solvent extraction condition of copper was obtained in one-stage solvent extraction at phase ratio of 5:4 with 40% HR in sulphonated kerosene for 5 min.The copper concentration in the raffinate decreased to 63.24 g/L and raffinate can be favorably recycled to the etching solution.The stripping studies were carried out with the simulated copper spent electrolyte containing 30 g/L Cu and 180 g/L H2SO4.The stripping ratio is 98.27% from the loaded organic phase after one-stage stripping at phase ratio of 1:2 at(298±0.5) K.
基金Supported by the Program on Technological Development Plan of Tianjin (No.033180611).
文摘In order to investigate the effect of magnetic field on the liquid-liquid extraction, the extraction in the acetone-water-trichloroethane system was studied under magnetic field with different magnetic induction intensity.The results showed that the effect of magnetic field was positive in the extraction process, and the partition coeffi-cient and the yield of acetone increased-with the increasing magnetic induction intensity by 5.16%-8.35% and 1.85%-5.70% respectively. The effect of magnetic field on the extraction was intensified when the temperature became, higher. The experimental data of the partition coefficient of acetone were correlated by the method of least square in terms of a power-law correlation.
基金Project(201309052)supported by the National Special Fund for Scientific Research in the Public InterestProject(2013FJ2003)supported by the Science and Technology Planning Project of Hunan Province of China
文摘For the determination of salicylaldoxime in environmental water samples,a stable and rapid method with low detection was proposed and established,based on the liquid-liquid extraction-high performance liquid chromatography with ultraviolet detector.Parameters including extraction solvent,ionic strength,solution pH,and extraction pattern were discussed for the optimal quantification of salicylaldoxime-spiked water.When the described method was applied to four spiked water samples,the obtained average extraction recovery rate was found between 87%–107%and relative standard deviation was below 6%.At the same time,good linear relationships were observed for spiked water samples from 0.01 to 10μg/mL(R2=0.9993).In addition,the detection limit of salicylaldoxime was revealed between 0.003–0.008μg/mL,which is two orders of magnitude lower than previously reported results.Thus,the presented method may be advantageous for the high-efficiency determination of salicylaldoxime in water samples.
文摘Teicoplanin is one of the macrocyclic glycopeptide antibiotics, which is active against Gram-positive bacteria, and has attracted a lot of attention in the field of chiral separation recently. In this work, the partition coefficients and extraction ratio of teicoplanin in three different solvent systems were studied: conventional extraction, reactive extraction and reverse micelle extraction. With conventional solvent extraction, n-butanol demonstrated high partition coefficient for teicoplanin, but low extraction ratio because of its high solubility in water. Reactive extraction of teicoplanin showed the highest partition coefficient with almost 100% recovery in organic phase when tri-n-octylmethyl ammonium chloride (TOMAC) was used as extractant and pH value was above 5.0. A reverse micelle system, consisted of isooctane +10mmol-L-1 TOMAC +1% n-octanol, also offered high separation factor for teicoplanin. The results are beneficial for the design of teicoplanin separation and purification process.
文摘The use of the guanidine extractant LIX 7950 extracting copper and cyanide from alkaline cyanide solution was investigated.The extraction of copper and cyanide under different initial copper and extractant concentrations was examined and the stoichiometric extraction constant of Cu(CN)32- with LIX 7950 was calculated.Both the distribution coefficient and the stoichiometric extraction constant of Cu(CN)3 2-with LIX 7950 decrease when the temperature is varied from 25℃to 45℃, indicating the extraction process is exothermic.The calculated enthalpy change of the reaction(-HΘ)is about-190 kJ/mol.The copper extraction isotherms under different molar ratios of cyanide to copper are established.The preferential extraction of Cu(CN)32- over Cu(CN)4 3-and CN -has been confirmed and a high cyanide-to-copper molar ratio tends to suppress copper loading. The loaded copper and cyanide can be stripped efficiently by the moderately strong NaOH solutions(0.5-1.0 mol/L)and the presence of NaCN in the stripping solution facilitates copper stripping.
基金supported by the Shanghai Pharmaceutical Association
文摘A highly sensitive SPE-liquid/liquid extraction RPLC method has been developed for the analysis of 6β-hydroxycortisol and cortisol in the urine of cancer patients. Methods: After SPE column purification and liquid-liquid extraction, the sample test solutions were analyzed with RPLC using a C18 analytical column. This improved analytical method has been validated for linearity, accuracy (recovery from urine), repeatability (within-day and between-day precision), specificity, sensitivity, and stability. This SPE-liquid/liquid extraction-RPLC is rapid, simple, accurate and reproducible. The technique is particularly useful for monitoring the CYP3A activity of cancer patients in clinical settings. The results are expressed as the ratio of 6β-hydroxycortisol to cortisol. Results: The CYP3A activity from a total of 153 samples was measured using this improved method. Considerable variation in the CYP3A activity of different cancer patients has been documented. Thus, personalized medical treatment based on the individual metabolic enzyme activity level is necessary. Conclusion: This new analytical method facilitates such individualized medical treatments.
文摘Liquid-liquid equilibrium (LLE) data for the ternary systemwater-ethanol-dimethyl succinate have been determined experimentallyat temperatures ranging from 298.15 to 318.15 K at 5 K intervals.Complete phase diagrams were obtained by determining solubility andthe tie-line data. Tie-line compositions were correlated byOthmer-Tobias method. The universal quasichemical functional groupactivity coefficient (UNIFAC) and modified UNIFAC methods were usedto predict the phase equilibrium in the system using the interactionparameters deter- Mined from experimental data between groups CH_3,CH_2, OH, CH_3 COO and H_2O.
基金Supported by the National Natural Science Foundation of China.
文摘In this work, mass transfer mechanism was studied for 50%TBP (in kerosene)-phenol-water as the working system in different hydrophobic microporous hollow fiber modules. The effect of different operating conditions on the removal of phenol was analyzed. Solvent entrainment in this process was detected with MALVERN-2600 laser pellet diameter analytical equipment. Experimental results indicate the mass transfer coefficient is increased while the two phase flow rates are increased. With increases in the flow rate of the water phase, the removal ratio of phenol will be decreased. Highly effective removal of phenol could be reached by changing the experimental conditions and the module configuration. The solvent entrainment in the water phase in the membrane extraction process was found to be 5%—8% of that in conventional liquid-liquid extraction process. Thus, solvent pollution could be better controlled.
基金Supported by the National Natural Science Foundation of China (20576081, 20736009) and the Ph.D. Programs Foundation of Ministry of Education of China (20070610128).
文摘Liquid phase oxidation of toluene is an environmental benign route for the production of benzoic acid.In a φ48mm bubble column reactor,the commercial process of toluene liquid phase oxidation was conducted with Co(CH3COO)2.4H2O as catalyst.The Co2+ concentration [Co2+] was determined by extraction spectrophotometry and hereby the Co3+ concentration [Co3+] was obtained by mass balance.The results showed that [Co3+] reached the maximum at about 25-30min.[Co3+] increased with increasing Co catalyst amount at total Co concentration<150 mg.L-1 of toluene.The conversion of toluene,yield and selectivity of benzoic acid increased with the increasing [Co3+/Co2+] max.A high [Co3+] and a high [Co3+]/[Co2+] ratio are beneficial to the reaction.
文摘In the past ^68Ge (Germanium-68) was purified with toxic organic solvents in liquid-liquid extractions making the product unacceptable by the FDA (food and drug Administration) for human use. The authors report initial studies utilizing three or four columns consisting of sequences of AG 1, AG50, Chelex 100 and/or Sephadex G25 resins. Five purification methods were examined and a separation consisting of the sequence: AG 1-Chelex100-Sephedex G25 provided 87% recovery of germanium. Fractionation of the elution resulted in high germanium concentrations.
基金Supported by the National Natural Science Foundation of China(NSFC U1462123)PetroChina Innovation FoundationFundamental Research Funds for the Central Universities of China(22201313007)
文摘When evaluating ionic liquids (ILs) for extractive desulfurization (EDS) of fuel oils, the inevitable presence of water in the system may have a significant and in many cases strongly negative effect. However, few studies have considered this particular issue and a promoted water effect on EDS is scarcely reported. In this work, COSMO-RS was firstly employed to calculate the capacity and selectivity for EDS of various IL/H20 mixtures, which cover different IL characters and a wide water concentration range. Experiments were then conducted with a representative IL [C4MIM]IH2P04], whose stable and even promoted extraction performance with a small amount of water was suggested by COSMO-RS. Through analyses of the desulfurization ratio, the cross- solubility and the water content in the desulfurized fuel, the promoted effect of water within a certain range (〈 10 wt%) was experimentally demonstrated. Moreover, such effect of water was explained combining the viscosity, the solvent-solute interactions and the COSMO-RS based analysis.
文摘In this work, the COSMO-RS (conductor like screening model for real solvent) model algorithm was derived from the modified Rachford rice method. It could be more helpful to investigate the phase behavior of binary systems with the help of quantum chemical calculation at 6-31G* basis set. COSMO-RS was used to predict solubility of binary mixture involving non-ILs (ionic liquids), and ILs systems are: benzyl ethylamine + glycerol system (Type-Ⅰ), nitro methane + cyclohexane system (Type-Ⅱ), dipropylamine + water system (Type-Ⅲ), 1,2-ethanediol + thiophene system (Type-Ⅳ), [1,2-DMIM] [salicylate] + thiophene (Type-Ⅳ), and [EMIM] [NO3] + thiophene (Type-Ⅳ). Totally 15 cations with 27 anions were used for generating 405 binary LLE (liquid liquid equilibrium) systems involving thiophene. However, the predicted COSMO-RS values are consisting with the reported experimental values. Furthermore, the immiscibility gap at 298.15 K was determined and compared for various ILs. It was found that l-butylpyrrolidinium, l-octylquinolinium, 1-octylpyridinium and 1-octyl-3-methylimidazolium based cations are most suitable for thiophene extraction from any liquid mixture.
文摘A number of synergistic solvent extraction (SSX) systems have been developed to recover nickel, cobalt, zinc and copper from sulphuric and chloride leach solutions by the solvent extraction team of CSIRO, Australia. These in- clude (1) Versatic 10/CLXS0 system for the separation of Ni from Ca in sulphate solutions, (2) Versatic 10/4PC system for the separation of Ni and Co from Mn/Mg/Ca in sulphate solutions, (3) Cyanex 471X/HRJ-4277 system for the separation of Zn from Cd in sulphate solutions, (4) Versatic 10/LIX63 system for the separation of Co from Mn/Mg/Ca in sulphate solutions, (5) Versatic 10/LIX63/TBP system for separation of Ni and Co from Mn/Mg/Ca in sulphate solutions, (6) Versatic 10/LIX63 system for the separation of cobalt from nickel in sulphate solutions by difference in kinetics, (7) Cyanex 272/LIX84 system for the separation of Cu/Fe/Zn from Ni/Co in sulphate solutions, (8) Versatic 10/LIX63fFBP system to recover Cu/Ni from strong chloride solutions, and [9) Versatic 10/LIX63 system to separate Cu from Fe in strong chloride solutions. The synergistic effect on metal separation and efficiency is presented and possible industrial applications are demonstrated. The chemical stability of selected SSX systems is also reported.
基金Supported by the National Natural Science Foundation of China(21176062)the Natural Science Foundation of Hunan Province(12JJ2007)+2 种基金Scientific Research Fund of Hunan Provincial Education Department(12B053)Science and Technology Planning Project of Hunan Province(2012GK3107)Aid Program for Science and Technology Innovative Research Team in Higher Educational Institutions of Hunan Province
文摘Based on the interfacial ligand exchange model and the law of conservation of mass, the multi-stage enantioselective liquid-liquid extraction model has been established to analyze and discuss on multi-stage centrifugal fractional extraction process of4-nitrobenzene glycine (PGL) enantiomers. The influence of phase ratio, extractant concentra- tion, and PFff concentration on the concentrations of enantiomers in the extract and raffinate was investigated by experiment and simulation. A good agreement between model and experiment was obtained. On this basis, the influence of many parameters such as location of stage, concentration levels, extractant excess, and number of stages on the symmetric separation performance was simulated. The optimal location of feed stage is the middle of fractional extraction equipment. The feed flow must satisfy a restricted relationship on flow ratios and the liquid throughout of centrifugal device. For desired purity specification, the required flow ratios decrease with extractant concentration and increase with PFff concentration. When the number of stages is 18 stages at extractant excess of 1.0 or 14 stages at extractant excess of 2.0, the eeeo (equal enantiomeric excess) can reach to 99%
文摘The ternary phase diagrams of musk ketone, musk xylene and various solvent were obtained by calcu- lations. Moreover, the double saturated lines were found to be curve for the first time. The methods to separate eutectic mixtures of musks by solution crystallization were suggested on the basis of these phase diagrams. A new process was proposed to get musk ketone and musk xylene from the eutectics by adding acetonitrile and heptane in turn, which was verified by experiments. Musk xylene with purity of 97.50% and musk ketone with purity of 98.10% were obtained.
基金National Integrity Innovational Technology Platform of New Drug and Development(Grant No.2009ZX09301- 010).
文摘A new HPLC-UV method was developed and validated for the quantitative determination of epidermal growth factor receptor inhibitor erlotinib in the plasma of tumor bearing BALB/c nude mice.Erlotinib and its internal standard l-(3-((6,7-bis(2- methoxyethoxy)quinazolin-4-yl)amino)phenyl)ethanone were extracted from mice plasma samples using liquid-liquid extraction with a mixed solvent of methyl t-butyl ether and ethyl acetate(9:1,v/v).Chromatographic separation was performed on a Luna C|_(18)column(4.6 mm×250 mm,5μm)with acetonitrile:5 mM potassium phosphate buffer pH=5.2(41:59,v/v)as the mobile phase.UV detector was set at the wavelength of 345 nm,and the flow rate was 1.0 mL/min.The calibration curve was linear over the range of 20-10 000 ng/mL with acceptable intra-and inter-day precision and accuracy.The intra-day and inter-day precisions were within the range of 1.69%—5.66%,and the accuracies of intra-and inter-day assays were within the range of 105%—113%. The mean recoveries were 85.2%and 96.1%for erlotinib and IS,respectively.This method was successfully applied to a pharmacokinetic study in tumor bearing BALB/c nude mice following single oral administration at the dose of 12.5 mg/kg. The main pharmacokinetic parameters were as follows:C_(max)was 4.67μg/mL,T_(max)was 1.0 h,T_(1/2)was 2.78 h,and AUC_(0-24h)was 18.0μg/mL·h.
基金supported by the National Natural Science Foundation of China (20905073 & 20975105)
文摘A simple and rapid method of ionic liquid based dispersive liquid-liquid microextraction (DLLME) combining with high performance liquid chromatography (HPLC) was developed for the analysis of four toxic anilines in flour steamed bread and maize steamed bread. Several possible influential factors such as the type of ionic liquid and disperser solvent, extraction time, sample pH, ionic strength and the volume of ionic liquid and disperser solvent were optimized using single factor experiments and orthogonal array design (OAD) with OA25(54) matrix. Analysis of variance (ANOVA) and percent contribution (PC) were used to investigate the significance of the factors of OAD. Sample pH and ionic strength are statistically demonstrated two chief factors. Under the optimum condition, the method exhibits a good linearity (r2 〉 0.99) over the studied range (50-1000 ng g-l) for anilines. The extraction factors and recoveries for the anilines in two kinds of steamed breads ranged between 34.1%-73.3% and 44.3%-95.3%, respectively. The limit of detections (LODs) and limit of quantitations (LOQs) ranged be- tween 10-15 ng g-1 and 30--45 ng g-1.