Gold(Au)and palladium(Pd)play an increasing role in the production and human life;Therefore,it is of great significance to study their recovery.A 5,11,17,23-tetra-ethylthio-25,26,27,28-tetra-hydroxyl thiacalix[4]arene...Gold(Au)and palladium(Pd)play an increasing role in the production and human life;Therefore,it is of great significance to study their recovery.A 5,11,17,23-tetra-ethylthio-25,26,27,28-tetra-hydroxyl thiacalix[4]arene(TCAET)was synthesized specifically for the capture of Au(Ⅲ)and Pd(Ⅱ)from HCl medium by liquid-liquid extraction.In a 0.1 mol·L^(-1)HCl medium,the transfer of Au(Ⅲ)and Pd(Ⅱ)from the aqueous phase to the organic phase was highly efficient,with a transfer ratio of 100%for Au(Ⅲ)and 98%for Pd(Ⅱ).Furthermore,the extraction equilibrium time for Au(Ⅲ)was just 5 min.Job's method data demonstrated that TCAET formed complexes with Au(Ⅲ)and Pd(Ⅱ)in a ratio of 2:3 and 1:1,respectively,during the extraction process.TCAET showed high selectivity toward Pd(Ⅱ)and Au(Ⅲ)over other competing metal ions.Moreover,both Au(Ⅲ)and Pd(Ⅱ)could be successfully stripped from the loaded organic phases with a 1.0 mol·L^(-1)thiourea in 0.5 mol·L^(-1)HCl and 0.5 mol·L^(-1)thiourea in 0.5 mol·L^(-1)HCl,respectively.Results obtained from five consecutive extraction-stripping cycles showed good reusability of TCAET toward Au(Ⅲ)and Pd(Ⅱ)recovery.The conclusion can provide a certain reference for thiacalixarene in the recovery of precious metal species.展开更多
In the petrochemical industry process, the relative volatility between the components to be separated is close to one or the azeotrope that systems are difficult to separate. Liquid-liquid extraction is a common and e...In the petrochemical industry process, the relative volatility between the components to be separated is close to one or the azeotrope that systems are difficult to separate. Liquid-liquid extraction is a common and effective separation method, and selecting an extraction agent is the key to extraction technology research. In this paper, a design method of extractants based on elements and chemical bonds was proposed. A knowledge-based molecular design method was adopted to pre-select elements and chemical bond groups. The molecules were automatically synthesized according to specific combination rules to avoid the problem of “combination explosion” of molecules. The target properties of the extractant were set, and the extractant meeting the requirements was selected by predicting the correlation physical properties of the generated molecules. Based on the separation performance of the extractant in liquid-liquid extraction and the relative importance of each index, the fuzzy comprehensive evaluation membership function was established, the analytic hierarchy process determined the mass ratio of each index, and the consistency test results were passed. The results of case study based on quantum chemical analysis demonstrated that effective determination of extractants for the analysis of benzene-cyclohexane systems. The results unanimously prove that the method has important theoretical significance and application value.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
A sensitive solvent extraction method for the determination of nonamolar concentrations of silicate in natural waters is developed. According to the traditional aqueous silicate method, silicomolybdenum blue formed by...A sensitive solvent extraction method for the determination of nonamolar concentrations of silicate in natural waters is developed. According to the traditional aqueous silicate method, silicomolybdenum blue formed by the reaction between silicate and ammoni- um molydate and reduced by metol-sulfite reagent is extracted by methyl isobutyl ketone. The absorbance can be enhanced substantially up to 10-folds. The detection limit of silicate is 8 nmol/dm^3 , which is one tenth smaller than the traditional method, with the precision of 4.0% at a silicate level of 50 nmol/dm^3 and 3.2% at a silicate level of 6 μmol/dm^3. Comparing the calibration curves in the distilled water and seawater, it can be seen that the salt effect also exists in the extraction method. However, the salt effect is a linear function of the salinity and can be corrected by simple calibration. The proposed method is successfully applied to the determination of silicate in natural waters. Natural concentrations of arsenate, arsenite and phosphate cause negligible interference.展开更多
In this research gasoil desalting was investigated from mass transfer point of view in an eductor liquid–liquid extraction column(eductor-LLE device).Mass transfer characteristics of the eductor-LLE device were evalu...In this research gasoil desalting was investigated from mass transfer point of view in an eductor liquid–liquid extraction column(eductor-LLE device).Mass transfer characteristics of the eductor-LLE device were evaluated and an empirical correlation was obtained by dimensional analysis of the dispersed phase Sherwood number.The Results showed that the overall mass transfer coefficient of the dispersed phase and extraction efficiency have been increased by increasing Sauter mean diameter(SMD)and decreasing the nozzle diameter from 2 to 1 mm,respectively.The effects of Reynolds number(R_(e)),projection ratio(ratio of the distance between venturi throat and nozzle tip to venturi throat diameter,Rpr),venturi throat area to nozzle area ratio(R_(th-n))and two phases flow rates ratio(R_(Q))on the mass transfer coefficient(K)were determined.According to the results,K increase with increasing Re and RQ and also with decreasing Rpr and R_(th-n).Semi-empirical models of drop formation,rising and coalescence were compared with our proposed empirical model.It was revealed that the present model provided a relatively good fitting for the mass transfer model of drop coalescence.Moreover,experimental data were in better agreement with calculated data with AARE value of 0.085.展开更多
Liquid-liquid extraction-thin layer chromatography （LLE-TLC） has been a common and routine combined method for detection of drugs in biological materials. Solid-phase extraction （SPE） is gradually replacing the tr...Liquid-liquid extraction-thin layer chromatography （LLE-TLC） has been a common and routine combined method for detection of drugs in biological materials. Solid-phase extraction （SPE） is gradually replacing the tra- ditional LLE method. High performance thin layer chromatography （HPTLC） has several advantages over TLC. The present work studied the higher efficiency of a new SPE-HPTLC method over that of a routine LLE-TLC method, in extraction and detection of urinary morphine. Fifty-eight urine samples, primarily identified as mor- phine-positive samples by a strip test, ＇were re-screened by LLE-TLC and SPE-HPTLC. The results of LLE-TLC and SPE-HPTLC were then compared with each other. The results showed that the SPE-HPTLC detected 74% of total samples as morphine-positive samples whereas the LLE-TLC detected 48% of the same samples. We further discussed the effect of codeine abuse on TLC analysis of urinary morphine. Regarding the importance of morphine detection in urine, the present combined SPE-HPTLC method is suggested as a replacement method for detection of urinary morphine by many reference laboratories.展开更多
[Objective] The research aimed to study the determination of 16 kinds of OCPs in water by liquid-liquid extraction -GC. [Method] The new method for determining 16 kinds of OCPs in water by liquid-liquid extraction -GC...[Objective] The research aimed to study the determination of 16 kinds of OCPs in water by liquid-liquid extraction -GC. [Method] The new method for determining 16 kinds of OCPs in water by liquid-liquid extraction -GC was established, and the influencing factors such as nitrogen pressure and water bath temperature were discussed. [ Result] Detection limit of the method was from 3.2 to 14.1 ng/L, the relative standard deviation was between 4.0% and 9.6%, and the average recovery ranged from 80.8% to 106.0%. By optimizing nitrogen pressure and water bath temperature in the sample pretreatment process, when nitrogen pressure was ＋0.087 kPa, and water bath temperature was ±36 ℃, recovery effect of this method was better. [ Conclusion] The determination method had accurate qualitative and quantitative results, and met detection requirement of 16 kinds of OCPs in water.展开更多
This paper shows some generalities about the glycerin byproduct obtained from biodiesel production process, presents an analysis of the ternary equilibrium between methanol, water and glycerol, and shows the influence...This paper shows some generalities about the glycerin byproduct obtained from biodiesel production process, presents an analysis of the ternary equilibrium between methanol, water and glycerol, and shows the influence that temperature has on the balance. This phase diagram illustrates ternary equilibrium at 10, 20 and 50 ℃, keeping the pressure constant at 1 atm （atmosphere） to standardize the analysis. The purpose of it is to establish the best temperature for the purification of glycerol by liquid-liquid extraction method under the ＂extraction in several stages cross flow＂ taking an initial mixture of glycerol with composition 15 wt.% water, 25 wt.% methanol and 60 wt.% glycerol. Water was used as liquid-liquid extraction solvent in order to remove as much methanol as possible from the initial solution due to the existence of a zone of insolubility between the glycerol and water in the ternary equilibrium. By this reason, two solutions are obtained, one consisting of water and methanol containing a trace of glycerin and the other consisting of water, glycerine and traces of methanol, which contain only 4.62% of the total methanol which enter in the process of liquid-liquid extraction, with 60.62% of the total glycerol, which is sent to a fractional distillation process to purify glycerin up to 98% by weight.展开更多
On the basis of homogeneous liquid-liquid extraction (HoLLE) with Zonyl FSA to plating water containing 1 mg palladium, 96.6% of the palladium was extracted into the sedimented liquid phase. After phase separation, th...On the basis of homogeneous liquid-liquid extraction (HoLLE) with Zonyl FSA to plating water containing 1 mg palladium, 96.6% of the palladium was extracted into the sedimented liquid phase. After phase separation, the volume ratio (Va/Vs) of the aqueous phase (Va) and the sedimented liquid phase (Vs) was 556 (50 mL → 0.09 mL). The assessment of the potential implementation of this procedure to wastewater treatment showed that HoLLE was satisfactorily achieved when the volume was scaled up to 1000 mL. Moreover, HoLLE was conducted to real palladium plating wastewater generated in the plating industry. 94.5% of the palladium was extracted into the sedimented liquid phase. After phase separation, the volume ratio (Va/Vs) of the aqueous phase (Va) and the sedimented liquid phase (Vs) was 500 (50 mL → 0.1 mL). In addition, HoLLE could separate palladium from coexisting metals in real plating wastewater. This knowledge is expected to lead to the development of new separation and concentration technologies of rare metals from real plating wastewater.展开更多
Continuous manufacturing is considered as one of the future trends of pharmaceutical engineering. In this work, continuous liquid-liquid extraction for sinomenine purification was realized with the usage of centrifuga...Continuous manufacturing is considered as one of the future trends of pharmaceutical engineering. In this work, continuous liquid-liquid extraction for sinomenine purification was realized with the usage of centrifugal extractors. Chloroform was used as the extractant because of the high distribution coefficient (>100). Higher extraction ratio can be obtained when using the centrifugal extractor of Model CWL50-N. The extraction ratio of the second-stage extraction was higher than that of the first-stage extraction. The extraction ratio of the second-stage countercurrent extraction was higher than that of second-stage cross-flow extraction. When chloroform phase was recycled for liquid-liquid extraction, the extraction ratio was also higher than 95%. This work can also be an example of continuous liquid-liquid extraction for the separation of other Chinese medicine components.展开更多
In this study, salting-out assisted liquid-liquid extraction combined with high performance liquid chromatography diode array detector (SALLE-HPLC-DAD) method was developed and validated for simultaneous analysis of c...In this study, salting-out assisted liquid-liquid extraction combined with high performance liquid chromatography diode array detector (SALLE-HPLC-DAD) method was developed and validated for simultaneous analysis of carbaryl, atrazine, propazine, chlorothalonil, dimethametryn and terbutryn in environmental water samples. Parameters affecting the extraction efficiency such as type and volume of extraction solvent, sample volume, salt type and amount, centrifugation speed and time, and sample pH were optimized. Under the optimum extraction conditions the method was linear over the range of 10 - 100 μg/L (carbaryl), 8 - 100 μg/L (atarzine), 7 - 100 μg/L (propazine) and 9 - 100 μg/L (chlorothalonil, terbutryn and dimethametryn) with correlation coefficients (R2) between 0.99 and 0.999. Limits of detection and quantification ranged from 2.0 to 2.8 μg/L and 6.7 to 9.5 μg/L, respectively. The extraction recoveries obtained for ground, lake and river waters were in a range of 75.5% to 106.6%, with the intra-day and inter-day relative standard deviation lower than 3.4% for all the target analytes. All of the target analytes were not detected in these samples. Therefore, the proposed SALLE-HPLC-DAD method is simple, rapid, cheap and environmentally friendly for the determination of the aforementioned herbicides, insecticide and fungicide residues in environmental water samples.展开更多
Extraction behavior of chlorpromazine hydrochloride (CPZ) and procaine hydro- chloride (PCN) in the system described in the title was studied. Research shows that the extraction efficiency of CPZ can amount to 96% by...Extraction behavior of chlorpromazine hydrochloride (CPZ) and procaine hydro- chloride (PCN) in the system described in the title was studied. Research shows that the extraction efficiency of CPZ can amount to 96% by twice extraction, while that of PCN is 77%. This system produces the distribution coefficients (KD) of 12.3 and 2.6 respectively for CPZ and PCN. Extraction mechanism is deduced according to ultraviolet and molecular fluorescence spectra variation of the drugs in the system studied.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
In this paper,a method of extracting phenols from coal tar by amines aqueous solution was proposed.The effects of various amines on the extraction properties of phenols in coal tar were researched from the views of mo...In this paper,a method of extracting phenols from coal tar by amines aqueous solution was proposed.The effects of various amines on the extraction properties of phenols in coal tar were researched from the views of molecular structure.The parameters such as molar ratio,concentration,extraction time and temperature for the extraction of coal tar by the monoethanolamine and ethylenediamine aqueous solution were examined.The results show that the organic amine with more amino groups,hydroxyl structure and strong electronegativity exhibited better extraction performance.Under the optimal conditions,the extraction yields of phenols in coal tar by the monoethanolamine or ethylenediamine aqueous solution are above 80%,and the recovery yields of amines reach 99%.Furthermore,the probable geometries of complexes formed by the combination of phenols and organic amines were calculated by density function theory.In addition,several thermodynamic models were evaluated through comparing the relative deviation of simulation results by ASPEN PLUS to the experimental ones,which provide feasibility thermodynamic models for the simulation of extraction process.The present work affords a mild,efficient and green approach for the extraction of phenols from coal tar by an aqueous solution of amines in industry application.展开更多
In this work,a novel rotating microchannel extractor(RME)is designed and further used for the extraction of chromium(Ⅲ)from water.Unexpectedly,the micro-extraction had the same effect as carrying out 2.9-stage cross-...In this work,a novel rotating microchannel extractor(RME)is designed and further used for the extraction of chromium(Ⅲ)from water.Unexpectedly,the micro-extraction had the same effect as carrying out 2.9-stage cross-flow extractions.Various factors,including the gas intake methods,gas intake quantity(Qg),distance between inner rotor and outer wall(D),rotational inner rotor speed(R)and volumetric flow rate(Qa,Qo),were selected to investigate their effect on the extraction efficiency(η)thoroughly.The relation map ofηwith Weaand We(o-g)for RME provides a comprehension for the gas–liquid–liquid extraction process in this RME system.展开更多
The utilization of liquid–liquid extraction for the separation of 2-phenylbutyric acid（2-PBA） enantiomers was proposed. Factors affecting the extract process were investigated, including organic solvents, β-cyclod...The utilization of liquid–liquid extraction for the separation of 2-phenylbutyric acid（2-PBA） enantiomers was proposed. Factors affecting the extract process were investigated, including organic solvents, β-cyclodextrin derivatives, cyclodextrin concentration, p H and temperature. A model was proposed to describe the separation process based on the homogeneous phase reaction mechanism. Important parameters of this model were determined experimentally. The physical distribution coefficients for molecular and ionic 2-PBA were0.129 and 7.455, respectively. The equilibrium constants of the complexation reactions were 89.36 and36.78 L·mol^-1 for（＋）-and（-）-2-PBA, respectively. The model was verified by experiments and proved to be an excellent means to optimize the separation system. Through modeling prediction and experiment, the best conditions（e.g., pH value of 3.00, extractant concentration of 0.1 mol·L^-1, temperature of 5.0 ℃） were acquired. Under this condition, the maximum enantioselectivity（2.096） was obtained.展开更多
1 INTRODUCTIONIn biotechnology there is a need for new protein recovery process,which combines a highselectivity for the desired product with substantial concentration increased and easy to scale-up.In this context,li...1 INTRODUCTIONIn biotechnology there is a need for new protein recovery process,which combines a highselectivity for the desired product with substantial concentration increased and easy to scale-up.In this context,liquid-liquid extraction with reversed micellar phase might serve this purpose.Reversed micelles are aggregates of surfactant molecules containing an inner core of water mole-cules,dispersed in a continuous organic solvent medium.These systems are opticallytransparent and thermodynamically stable.It has beendemonstrated [1,2]that under certainconditions proteins can be transferred from an aqueous phase towards a reversed micellarphase or vice versa(Fig.1)展开更多
A simple and high-throughput method to simultaneously determine selected benzodiazepines (i.e., diazepam, lorazepam, clonazepam, and bromazepam) in urine was developed and validated. The entire methodology consisted o...A simple and high-throughput method to simultaneously determine selected benzodiazepines (i.e., diazepam, lorazepam, clonazepam, and bromazepam) in urine was developed and validated. The entire methodology consisted of the application of an innovative extraction/cleanup procedure, namely liquid-liquid extraction with low-temperature partitioning (LLE-LTP), and analysis by liquid chromatography combined with high-resolution mass spectrometry (LC-HRMS). The LLE-LTP procedure was optimized via factorial design and by evaluating crucial variables, specifically the freezing mode (either slow or fast), the urine/acetonitrile volume ratio, and the sample ionic strength. The benzodiazepines were quantified using matrix-matched calibration curves where the following parameters were assessed by validation protocol: in general, linearity range of 17 - 200 μg?L–1 (r > 0.9957);limits of detection lower than 5 μg?L–1;relative standard deviations (RSD) lower than 12.5%;and accuracy ranging from 72.3 to 117%. To test this procedure’s performance, the method was applied to determine the content of diazepam in actual urine samples. The validation results obtained for the method demonstrated that the present methodology could be potentially applied in proficient laboratories as a routine approach for determining benzodiazepines compounds content in urine.展开更多
Objective An efficient extraction and separation method of resveratrol from a Chinese herb giant knotweed was developed and the protective effect of resveratrol on myocardium injury was investigated.Methods An orthogo...Objective An efficient extraction and separation method of resveratrol from a Chinese herb giant knotweed was developed and the protective effect of resveratrol on myocardium injury was investigated.Methods An orthogonal experiment was utilized to optimize the extraction conditions and the pure white crystal obtained utilizing the proposed method was used for the investigation of myocardium ischemic injury.Results Resveratrol was found to have many beneficial activities including the protective effect on the heart and the scavenging of free radical.Conclusion The protective effect of resveratrol on myocardium injury is related to the quenching of lipid peroxidation.展开更多
Objective:Pretreatment of biological samples is the most critical step in pharmacokinetic studies,especially pre-treatment of plasma samples.The pretreatment of biological samples in pharmacokinetic study of Tradition...Objective:Pretreatment of biological samples is the most critical step in pharmacokinetic studies,especially pre-treatment of plasma samples.The pretreatment of biological samples in pharmacokinetic study of Traditional Chinese Medicines (TCM) is difficult due to the complexity of the ingredients.An organic solvent system ethyl acetate:acetone (10:1) solution used for liquid-liquid extraction has been developed in this study and compared with the commonly used protein precipitation method.Methods:Rats,Beagle dogs and humans plasma samples were adopted in this study in order to demonstrate the universality of the pretreatment method.Feasibility of this pretreatment method was also verified through its application to the pharmacokinetics of rhubarb in rats.Results:According to the results of extraction recovery matrix effect,it was indicated that the liquid-liquid extraction methods with new organic solvent might be suitable for variety of structures of compounds and various types of plasma samples.The pharmacokinetic study result showed that the developed pretreatment method could successfully be used for simultaneous determination of three active compounds modin,emodin-8-O-β-D-glucopyranoside (EDG) and rhein in rat plasma with high sensitivity,accuracy,and recovery by liquid chromatography tandem mass spectrometry (LC-MS/MS).Conclusion:The pretreatment method of liquid-liquid extraction methods with new organic solvent could be successfully applied for multi-component pharmacokinetics of TCM.展开更多
基金supported by the National Natural Science Foundation of China(U20A20268)Natural Science Foundation of Hunan Province(2020JJ1004)Hunan Provincial Innovation Foundation for Postgraduate(CX20211190)。
文摘Gold(Au)and palladium(Pd)play an increasing role in the production and human life;Therefore,it is of great significance to study their recovery.A 5,11,17,23-tetra-ethylthio-25,26,27,28-tetra-hydroxyl thiacalix[4]arene(TCAET)was synthesized specifically for the capture of Au(Ⅲ)and Pd(Ⅱ)from HCl medium by liquid-liquid extraction.In a 0.1 mol·L^(-1)HCl medium,the transfer of Au(Ⅲ)and Pd(Ⅱ)from the aqueous phase to the organic phase was highly efficient,with a transfer ratio of 100%for Au(Ⅲ)and 98%for Pd(Ⅱ).Furthermore,the extraction equilibrium time for Au(Ⅲ)was just 5 min.Job's method data demonstrated that TCAET formed complexes with Au(Ⅲ)and Pd(Ⅱ)in a ratio of 2:3 and 1:1,respectively,during the extraction process.TCAET showed high selectivity toward Pd(Ⅱ)and Au(Ⅲ)over other competing metal ions.Moreover,both Au(Ⅲ)and Pd(Ⅱ)could be successfully stripped from the loaded organic phases with a 1.0 mol·L^(-1)thiourea in 0.5 mol·L^(-1)HCl and 0.5 mol·L^(-1)thiourea in 0.5 mol·L^(-1)HCl,respectively.Results obtained from five consecutive extraction-stripping cycles showed good reusability of TCAET toward Au(Ⅲ)and Pd(Ⅱ)recovery.The conclusion can provide a certain reference for thiacalixarene in the recovery of precious metal species.
基金supported by the National Natural Science Foundation of China(22178190).
文摘In the petrochemical industry process, the relative volatility between the components to be separated is close to one or the azeotrope that systems are difficult to separate. Liquid-liquid extraction is a common and effective separation method, and selecting an extraction agent is the key to extraction technology research. In this paper, a design method of extractants based on elements and chemical bonds was proposed. A knowledge-based molecular design method was adopted to pre-select elements and chemical bond groups. The molecules were automatically synthesized according to specific combination rules to avoid the problem of “combination explosion” of molecules. The target properties of the extractant were set, and the extractant meeting the requirements was selected by predicting the correlation physical properties of the generated molecules. Based on the separation performance of the extractant in liquid-liquid extraction and the relative importance of each index, the fuzzy comprehensive evaluation membership function was established, the analytic hierarchy process determined the mass ratio of each index, and the consistency test results were passed. The results of case study based on quantum chemical analysis demonstrated that effective determination of extractants for the analysis of benzene-cyclohexane systems. The results unanimously prove that the method has important theoretical significance and application value.
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.
基金The National Science Foundation of China under contract No.40606028the Special Fund from the National Key Basic Research Program of China under contract No.2006CB400601.
文摘A sensitive solvent extraction method for the determination of nonamolar concentrations of silicate in natural waters is developed. According to the traditional aqueous silicate method, silicomolybdenum blue formed by the reaction between silicate and ammoni- um molydate and reduced by metol-sulfite reagent is extracted by methyl isobutyl ketone. The absorbance can be enhanced substantially up to 10-folds. The detection limit of silicate is 8 nmol/dm^3 , which is one tenth smaller than the traditional method, with the precision of 4.0% at a silicate level of 50 nmol/dm^3 and 3.2% at a silicate level of 6 μmol/dm^3. Comparing the calibration curves in the distilled water and seawater, it can be seen that the salt effect also exists in the extraction method. However, the salt effect is a linear function of the salinity and can be corrected by simple calibration. The proposed method is successfully applied to the determination of silicate in natural waters. Natural concentrations of arsenate, arsenite and phosphate cause negligible interference.
文摘In this research gasoil desalting was investigated from mass transfer point of view in an eductor liquid–liquid extraction column(eductor-LLE device).Mass transfer characteristics of the eductor-LLE device were evaluated and an empirical correlation was obtained by dimensional analysis of the dispersed phase Sherwood number.The Results showed that the overall mass transfer coefficient of the dispersed phase and extraction efficiency have been increased by increasing Sauter mean diameter(SMD)and decreasing the nozzle diameter from 2 to 1 mm,respectively.The effects of Reynolds number(R_(e)),projection ratio(ratio of the distance between venturi throat and nozzle tip to venturi throat diameter,Rpr),venturi throat area to nozzle area ratio(R_(th-n))and two phases flow rates ratio(R_(Q))on the mass transfer coefficient(K)were determined.According to the results,K increase with increasing Re and RQ and also with decreasing Rpr and R_(th-n).Semi-empirical models of drop formation,rising and coalescence were compared with our proposed empirical model.It was revealed that the present model provided a relatively good fitting for the mass transfer model of drop coalescence.Moreover,experimental data were in better agreement with calculated data with AARE value of 0.085.
文摘Liquid-liquid extraction-thin layer chromatography （LLE-TLC） has been a common and routine combined method for detection of drugs in biological materials. Solid-phase extraction （SPE） is gradually replacing the tra- ditional LLE method. High performance thin layer chromatography （HPTLC） has several advantages over TLC. The present work studied the higher efficiency of a new SPE-HPTLC method over that of a routine LLE-TLC method, in extraction and detection of urinary morphine. Fifty-eight urine samples, primarily identified as mor- phine-positive samples by a strip test, ＇were re-screened by LLE-TLC and SPE-HPTLC. The results of LLE-TLC and SPE-HPTLC were then compared with each other. The results showed that the SPE-HPTLC detected 74% of total samples as morphine-positive samples whereas the LLE-TLC detected 48% of the same samples. We further discussed the effect of codeine abuse on TLC analysis of urinary morphine. Regarding the importance of morphine detection in urine, the present combined SPE-HPTLC method is suggested as a replacement method for detection of urinary morphine by many reference laboratories.
文摘[Objective] The research aimed to study the determination of 16 kinds of OCPs in water by liquid-liquid extraction -GC. [Method] The new method for determining 16 kinds of OCPs in water by liquid-liquid extraction -GC was established, and the influencing factors such as nitrogen pressure and water bath temperature were discussed. [ Result] Detection limit of the method was from 3.2 to 14.1 ng/L, the relative standard deviation was between 4.0% and 9.6%, and the average recovery ranged from 80.8% to 106.0%. By optimizing nitrogen pressure and water bath temperature in the sample pretreatment process, when nitrogen pressure was ＋0.087 kPa, and water bath temperature was ±36 ℃, recovery effect of this method was better. [ Conclusion] The determination method had accurate qualitative and quantitative results, and met detection requirement of 16 kinds of OCPs in water.
文摘This paper shows some generalities about the glycerin byproduct obtained from biodiesel production process, presents an analysis of the ternary equilibrium between methanol, water and glycerol, and shows the influence that temperature has on the balance. This phase diagram illustrates ternary equilibrium at 10, 20 and 50 ℃, keeping the pressure constant at 1 atm （atmosphere） to standardize the analysis. The purpose of it is to establish the best temperature for the purification of glycerol by liquid-liquid extraction method under the ＂extraction in several stages cross flow＂ taking an initial mixture of glycerol with composition 15 wt.% water, 25 wt.% methanol and 60 wt.% glycerol. Water was used as liquid-liquid extraction solvent in order to remove as much methanol as possible from the initial solution due to the existence of a zone of insolubility between the glycerol and water in the ternary equilibrium. By this reason, two solutions are obtained, one consisting of water and methanol containing a trace of glycerin and the other consisting of water, glycerine and traces of methanol, which contain only 4.62% of the total methanol which enter in the process of liquid-liquid extraction, with 60.62% of the total glycerol, which is sent to a fractional distillation process to purify glycerin up to 98% by weight.
文摘On the basis of homogeneous liquid-liquid extraction (HoLLE) with Zonyl FSA to plating water containing 1 mg palladium, 96.6% of the palladium was extracted into the sedimented liquid phase. After phase separation, the volume ratio (Va/Vs) of the aqueous phase (Va) and the sedimented liquid phase (Vs) was 556 (50 mL → 0.09 mL). The assessment of the potential implementation of this procedure to wastewater treatment showed that HoLLE was satisfactorily achieved when the volume was scaled up to 1000 mL. Moreover, HoLLE was conducted to real palladium plating wastewater generated in the plating industry. 94.5% of the palladium was extracted into the sedimented liquid phase. After phase separation, the volume ratio (Va/Vs) of the aqueous phase (Va) and the sedimented liquid phase (Vs) was 500 (50 mL → 0.1 mL). In addition, HoLLE could separate palladium from coexisting metals in real plating wastewater. This knowledge is expected to lead to the development of new separation and concentration technologies of rare metals from real plating wastewater.
文摘Continuous manufacturing is considered as one of the future trends of pharmaceutical engineering. In this work, continuous liquid-liquid extraction for sinomenine purification was realized with the usage of centrifugal extractors. Chloroform was used as the extractant because of the high distribution coefficient (>100). Higher extraction ratio can be obtained when using the centrifugal extractor of Model CWL50-N. The extraction ratio of the second-stage extraction was higher than that of the first-stage extraction. The extraction ratio of the second-stage countercurrent extraction was higher than that of second-stage cross-flow extraction. When chloroform phase was recycled for liquid-liquid extraction, the extraction ratio was also higher than 95%. This work can also be an example of continuous liquid-liquid extraction for the separation of other Chinese medicine components.
文摘In this study, salting-out assisted liquid-liquid extraction combined with high performance liquid chromatography diode array detector (SALLE-HPLC-DAD) method was developed and validated for simultaneous analysis of carbaryl, atrazine, propazine, chlorothalonil, dimethametryn and terbutryn in environmental water samples. Parameters affecting the extraction efficiency such as type and volume of extraction solvent, sample volume, salt type and amount, centrifugation speed and time, and sample pH were optimized. Under the optimum extraction conditions the method was linear over the range of 10 - 100 μg/L (carbaryl), 8 - 100 μg/L (atarzine), 7 - 100 μg/L (propazine) and 9 - 100 μg/L (chlorothalonil, terbutryn and dimethametryn) with correlation coefficients (R2) between 0.99 and 0.999. Limits of detection and quantification ranged from 2.0 to 2.8 μg/L and 6.7 to 9.5 μg/L, respectively. The extraction recoveries obtained for ground, lake and river waters were in a range of 75.5% to 106.6%, with the intra-day and inter-day relative standard deviation lower than 3.4% for all the target analytes. All of the target analytes were not detected in these samples. Therefore, the proposed SALLE-HPLC-DAD method is simple, rapid, cheap and environmentally friendly for the determination of the aforementioned herbicides, insecticide and fungicide residues in environmental water samples.
文摘Extraction behavior of chlorpromazine hydrochloride (CPZ) and procaine hydro- chloride (PCN) in the system described in the title was studied. Research shows that the extraction efficiency of CPZ can amount to 96% by twice extraction, while that of PCN is 77%. This system produces the distribution coefficients (KD) of 12.3 and 2.6 respectively for CPZ and PCN. Extraction mechanism is deduced according to ultraviolet and molecular fluorescence spectra variation of the drugs in the system studied.
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.
基金financial support by the National Natural Science Foundation of China(21676226,21606186)the Natural Science Foundation for Distinguished Young Scholars in Hunan Province(2018JJ1023)+1 种基金Key Research and Development Program in Hunan Province(2019GK2041)Collaborative Innovation Center of New Chemical Technologies for Environmental Benignity and Efficient Resource Utilization。
文摘In this paper,a method of extracting phenols from coal tar by amines aqueous solution was proposed.The effects of various amines on the extraction properties of phenols in coal tar were researched from the views of molecular structure.The parameters such as molar ratio,concentration,extraction time and temperature for the extraction of coal tar by the monoethanolamine and ethylenediamine aqueous solution were examined.The results show that the organic amine with more amino groups,hydroxyl structure and strong electronegativity exhibited better extraction performance.Under the optimal conditions,the extraction yields of phenols in coal tar by the monoethanolamine or ethylenediamine aqueous solution are above 80%,and the recovery yields of amines reach 99%.Furthermore,the probable geometries of complexes formed by the combination of phenols and organic amines were calculated by density function theory.In addition,several thermodynamic models were evaluated through comparing the relative deviation of simulation results by ASPEN PLUS to the experimental ones,which provide feasibility thermodynamic models for the simulation of extraction process.The present work affords a mild,efficient and green approach for the extraction of phenols from coal tar by an aqueous solution of amines in industry application.
基金financial support from the National Natural Science Foundation of China(21776181)Sichuan University innovation spark project(2018SCUH0012)+1 种基金Chinese National Key Research and Development Plan(2018YFC1900203-03)Special Project of Building World-class Universities(2030704401004)。
文摘In this work,a novel rotating microchannel extractor(RME)is designed and further used for the extraction of chromium(Ⅲ)from water.Unexpectedly,the micro-extraction had the same effect as carrying out 2.9-stage cross-flow extractions.Various factors,including the gas intake methods,gas intake quantity(Qg),distance between inner rotor and outer wall(D),rotational inner rotor speed(R)and volumetric flow rate(Qa,Qo),were selected to investigate their effect on the extraction efficiency(η)thoroughly.The relation map ofηwith Weaand We(o-g)for RME provides a comprehension for the gas–liquid–liquid extraction process in this RME system.
基金Supported by the National Basic Research Program of China(2014CB260407)
文摘The utilization of liquid–liquid extraction for the separation of 2-phenylbutyric acid（2-PBA） enantiomers was proposed. Factors affecting the extract process were investigated, including organic solvents, β-cyclodextrin derivatives, cyclodextrin concentration, p H and temperature. A model was proposed to describe the separation process based on the homogeneous phase reaction mechanism. Important parameters of this model were determined experimentally. The physical distribution coefficients for molecular and ionic 2-PBA were0.129 and 7.455, respectively. The equilibrium constants of the complexation reactions were 89.36 and36.78 L·mol^-1 for（＋）-and（-）-2-PBA, respectively. The model was verified by experiments and proved to be an excellent means to optimize the separation system. Through modeling prediction and experiment, the best conditions（e.g., pH value of 3.00, extractant concentration of 0.1 mol·L^-1, temperature of 5.0 ℃） were acquired. Under this condition, the maximum enantioselectivity（2.096） was obtained.
文摘1 INTRODUCTIONIn biotechnology there is a need for new protein recovery process,which combines a highselectivity for the desired product with substantial concentration increased and easy to scale-up.In this context,liquid-liquid extraction with reversed micellar phase might serve this purpose.Reversed micelles are aggregates of surfactant molecules containing an inner core of water mole-cules,dispersed in a continuous organic solvent medium.These systems are opticallytransparent and thermodynamically stable.It has beendemonstrated [1,2]that under certainconditions proteins can be transferred from an aqueous phase towards a reversed micellarphase or vice versa(Fig.1)
基金Conselho Nacional de Desenvolvimento Cientifico e Tecnologico(CNPq)and Fundacao de Amparo a Pesquisa do Estado de Minas Gerais(FAPEMIG)for financial support and research fellowships.
文摘A simple and high-throughput method to simultaneously determine selected benzodiazepines (i.e., diazepam, lorazepam, clonazepam, and bromazepam) in urine was developed and validated. The entire methodology consisted of the application of an innovative extraction/cleanup procedure, namely liquid-liquid extraction with low-temperature partitioning (LLE-LTP), and analysis by liquid chromatography combined with high-resolution mass spectrometry (LC-HRMS). The LLE-LTP procedure was optimized via factorial design and by evaluating crucial variables, specifically the freezing mode (either slow or fast), the urine/acetonitrile volume ratio, and the sample ionic strength. The benzodiazepines were quantified using matrix-matched calibration curves where the following parameters were assessed by validation protocol: in general, linearity range of 17 - 200 μg?L–1 (r > 0.9957);limits of detection lower than 5 μg?L–1;relative standard deviations (RSD) lower than 12.5%;and accuracy ranging from 72.3 to 117%. To test this procedure’s performance, the method was applied to determine the content of diazepam in actual urine samples. The validation results obtained for the method demonstrated that the present methodology could be potentially applied in proficient laboratories as a routine approach for determining benzodiazepines compounds content in urine.
文摘Objective An efficient extraction and separation method of resveratrol from a Chinese herb giant knotweed was developed and the protective effect of resveratrol on myocardium injury was investigated.Methods An orthogonal experiment was utilized to optimize the extraction conditions and the pure white crystal obtained utilizing the proposed method was used for the investigation of myocardium ischemic injury.Results Resveratrol was found to have many beneficial activities including the protective effect on the heart and the scavenging of free radical.Conclusion The protective effect of resveratrol on myocardium injury is related to the quenching of lipid peroxidation.
文摘Objective:Pretreatment of biological samples is the most critical step in pharmacokinetic studies,especially pre-treatment of plasma samples.The pretreatment of biological samples in pharmacokinetic study of Traditional Chinese Medicines (TCM) is difficult due to the complexity of the ingredients.An organic solvent system ethyl acetate:acetone (10:1) solution used for liquid-liquid extraction has been developed in this study and compared with the commonly used protein precipitation method.Methods:Rats,Beagle dogs and humans plasma samples were adopted in this study in order to demonstrate the universality of the pretreatment method.Feasibility of this pretreatment method was also verified through its application to the pharmacokinetics of rhubarb in rats.Results:According to the results of extraction recovery matrix effect,it was indicated that the liquid-liquid extraction methods with new organic solvent might be suitable for variety of structures of compounds and various types of plasma samples.The pharmacokinetic study result showed that the developed pretreatment method could successfully be used for simultaneous determination of three active compounds modin,emodin-8-O-β-D-glucopyranoside (EDG) and rhein in rat plasma with high sensitivity,accuracy,and recovery by liquid chromatography tandem mass spectrometry (LC-MS/MS).Conclusion:The pretreatment method of liquid-liquid extraction methods with new organic solvent could be successfully applied for multi-component pharmacokinetics of TCM.
