This study describes the development and validation of a sensitive and reliable method for determination of polybrominated diphenyl ethers（PBDEs）in atmospheric particulate matter using selective pressurized liquid e...This study describes the development and validation of a sensitive and reliable method for determination of polybrominated diphenyl ethers（PBDEs）in atmospheric particulate matter using selective pressurized liquid extraction（SPLE）and gas chromatography–mass spectrometry with a negative chemical ionization（GC-NCI-MS）.Extraction and clean-up were performed using PLE with 2 g florisil and 3 g silica placed in the extraction cells.Under optimal conditions,14 PBDEs were extracted at 70℃ using hexane/dichloromethane（50：50,v/v）as solvent.Validation of SPLE returned excellent recoveries for most analytes,with relative standard deviations mostly below20%.Method detection limits ranged from 0.13 to15.38 ng·mL^-1 for the GC-MS analyses.The method was successfully applied to atmospheric particulate matter of Beijing,where analytes were detected in the range of182.79 to 468.99 pg·m^-3.展开更多
A novel process for separation of red （Y2O3：Eu^3＋）, blue（BaMgAl10O17：Eu^2＋） and green （CeMgAl10O17：Tb^3） rare earth fluorescent powders was proposed. At first, the blue powder can be extracted selectively f...A novel process for separation of red （Y2O3：Eu^3＋）, blue（BaMgAl10O17：Eu^2＋） and green （CeMgAl10O17：Tb^3） rare earth fluorescent powders was proposed. At first, the blue powder can be extracted selectively from an aqueous solution using a chelating collector 2-thenoyltrifluoroacetone （TTA） dissolved in heptane at alkaline pH condition, then, chloroform was used for extracting the green powder into organic phase. The red phosphor remains in aqueous phase with potassium sodium tartrate depressant （PST）. Therefore, three phosphors can be separated successfully from their artificial mixtures by liquid/liquid extraction, and grades and recovery of separated products reach respectively as follows： red is 96.9% and 95.2%, blue is 82.7% and 98.8%, green is 94.6% and 82.6%.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
diketone type chelating ligands have high coordinative activity and selectivity, and are widely applied in analytical chemistry. In order to obtain profounder understanding to the properties of bis(4 acylpyrazolone ...diketone type chelating ligands have high coordinative activity and selectivity, and are widely applied in analytical chemistry. In order to obtain profounder understanding to the properties of bis(4 acylpyrazolone 5), A new 4 acylpyrazol 5 one derivative (H 2BPMPP) was syntheszed, which contains a heterocyclic ring between two 1 phenyl 3 methyl 4 acylpyrazol 5 one rings. The new compound was characterized by element analyses, UV, IR and 1H NMR spectra. The equilibrium of the keto enol tautomerism was studied. The results show that a lower dielectric constant of solvent favors the enol form which has a higher λ max . Due to special merits of paraffin wax, the solid liquid extraction behavior of Ce(Ⅲ) with molten paraffin wax as a diluent was also investigated at higher temperature. The value of the pH 1/2 was 3.19 and the value of log K ex was 3.467. The chemical composition of the complex was obtained by the slope analysis method.展开更多
Three extraction methods were compared for their efficiency to analyze sitagliptin and simvastatin in rat plasma by LC-MS/MS, including （1） liquid-liquid extraction （LLE）, （2） solid phase extraction （SPE） and ...Three extraction methods were compared for their efficiency to analyze sitagliptin and simvastatin in rat plasma by LC-MS/MS, including （1） liquid-liquid extraction （LLE）, （2） solid phase extraction （SPE） and （3） supported liquid extraction （SLE）. Comparison of recoveries of analytes with different extraction methods revealed that SLE was the best extraction method. The detection was facilitated with ion trap-mass spectrometer by multiple reactions monitoring （MRM） in a positive ion mode with ESI. The transitions monitored were m./z 441.1→325.2 for simvastatin, 408.2→235.1 for sitagliptin and 278.1→260.1 for the IS. The lower limit of quantification （LLOQ） was 0.2 ng/mL for sitagliptin and 0.1 ng/mL for simvastatin. The effective SLE offers enhanced chromatographic selectivity, thus facilitating the potential utility of the method for routine analysis of biological samples along with pharmacokinetic studies.展开更多
A novel bioanalytical method was developed and validated for the quantitative determination of darunavir（DRV） in rat plasma by employing hydrophilic interaction chromatography and tandem mass spectrometry（HILIC-MS...A novel bioanalytical method was developed and validated for the quantitative determination of darunavir（DRV） in rat plasma by employing hydrophilic interaction chromatography and tandem mass spectrometry（HILIC-MS/MS） with supported liquid extraction（SLE）.lrbesartan（IRB） was used as an internal standard（IS）.The analyte in rat plasma（200 μL） was isolated through SLE using ethyl acetate as the eluting solvent.The chromatographic separation was achieved on Luna-HILIC（250 mm × 4.6 mm,5 μm）column with a mobile phase of 0.1% of formic acid in water：acetonitrile（5：95,v/v）,at a constant flow rate of 1.0mL/min.The MS/MS ion transitions for DRV（548.1→392.0） and IS（429.2→207.1） were monitored on an ion trap mass spectrometer,operating in the multiple reaction monitoring（MRM） mode.The lower limit of quantitation（LLOQ） was 0.2 ng/mL and quantitation range was 0.2-5000 ng/mL.The method was validated for its selectivity,sensitivity,carryover,linearity,precision,accuracy,recovery,matrix effect and stability.The method was successfully applied to pharmacokinetic study in rats.展开更多
Recovery of rare earth(RE)elements from Nd-Fe-B waste is one of the ways to solve the problem of socalled RE-crisis,An alternative approach of extracting RE elements from Nd-Fe-B waste by molten Cu extraction based on...Recovery of rare earth(RE)elements from Nd-Fe-B waste is one of the ways to solve the problem of socalled RE-crisis,An alternative approach of extracting RE elements from Nd-Fe-B waste by molten Cu extraction based on liquid-solid diffusion and reaction is reported in this paper.The extraction process,product microstructure and extraction efficiency were systematically studied.The results show that the extraction rate of RE at 1200℃is about 20%higher than that at 1100℃.The enhanced extraction efficiency at 1200℃results from the fact that the liquid Fe and Fe2 B are not co-soluble with Cu,Reducing the mass ratio of Cu to waste and the size of the waste scraps is also beneficial to enhancing the separation of RE and Fe elements.In addition,the extraction time should be well controlled,for example,less than 2 h at 1100℃,in order to avoid the increased Fe content in the extracted product.Based on optimized process,the RE elements ca n be almost fully extracted from the waste.This work thus provides an effective method to recover the RE elements.展开更多
Pressurized liquid extraction using green solvents(ethanol and water)was applied to extract photosynthetic pigments from the microalgae Chlamydomonas sp.An experimental design is employed to determine the effect of th...Pressurized liquid extraction using green solvents(ethanol and water)was applied to extract photosynthetic pigments from the microalgae Chlamydomonas sp.An experimental design is employed to determine the effect of the extraction conditions on the extraction yield and the antioxidant capacity of the different extracts determined using 1,1-diphenyl-2-picryl-hydrazyl and TEAC tests.All the extracts show significant antioxidant activity in all assays.Besides,in this work,the carotenoid and chlorophyll composition of the Chlamydomonas extracts was analyzed by HPLC–DAD–APCI–MS/MS for the first time,being the main compounds lutein and pheophythin a′.展开更多
A novel silver-based dihydric alcohol extractant was substituted for ionic liquids to enrich methyl linolenate(C18-3)from tallow seed oil methyl ester in this study.The interactions among dihydric alcohol,Ag(I)and C18...A novel silver-based dihydric alcohol extractant was substituted for ionic liquids to enrich methyl linolenate(C18-3)from tallow seed oil methyl ester in this study.The interactions among dihydric alcohol,Ag(I)and C18-3 were explored by FT-IR spectroscopy.The effects of dihydric alcohol structure,carrier Ag(I)concentration,temperature and initial feed concentration on extraction yield and selectivity were reported.The good extraction performance was achieved by 1,4-butanediol containing AgBF4.The complexation of Ag(I)with C18-3 was dominant in extraction operation rather than physical partition.Furthermore,a multi-step reverse extraction method was proposed to obtain C18-3 product and regenerate the extractant.1-Hexene as the stripping phase can facilitate C18-3 reverse extraction.The content of C18-3 in the product was up to 93.36%,and the yield was 73.76%.This work opened a new route for the utilization of the dihydric alcohol properties to manipulate the carrier efficiency for extracting unsaturated fatty acid methyl esters at a lower cost.展开更多
The extraction behavior of several lanthanides（La^3＋, Eu^3＋, Lu^3＋） from nitric acid（HNO3） solution was studied using a novel extraction system based on 2,6-bis（5,6-dihexyl-1,2,4-triazin-3-yl） pyridine（isohe...The extraction behavior of several lanthanides（La^3＋, Eu^3＋, Lu^3＋） from nitric acid（HNO3） solution was studied using a novel extraction system based on 2,6-bis（5,6-dihexyl-1,2,4-triazin-3-yl） pyridine（isohexyl-BTP） as extractant in 1-alkyl-3-methylimidazolium bis（trifluoromethylsufonyl）imide（[Cnmim][NTf2]） ionic liquid. Isohexyl-BTP in ionic liquids exhibited remarkably better extraction performance for lanthanides than that in octanol-dodecane（3：7 v/v） system. Lower HNO3 concentration and short alkyl chain length of [Cnmim]^＋ were more favourable for removal of lanthanides. Besides, it was confirmed that isohexyl-BTP in ILs formed a 1：3 complex [Ln（BTP）3（NO3）n]^（3–n）＋（n=0, 1） by slope analysis. In addition, [C2mim][NTf2] preferred to extract lanthanides via a cation exchange mechanism at lower acidity, which was proved via UV-Vis measurement. It was speculated that extraction mechanism shifted from cation exchange to neutral species extraction with increase in HNO3 concentration and alkyl chain length of [Cnmim]^＋ due to the H^＋ completion, NO3^- inhibition and hydrophobicity of IL.展开更多
To establish an analytical method for determination of four bisphenols （BPA, BPB, BPF, and BPS） and two alkylphenols （4-n-OP, 4-n-NP） in water by ultra performance liquid chromatography- tandem mass spectrometry ...To establish an analytical method for determination of four bisphenols （BPA, BPB, BPF, and BPS） and two alkylphenols （4-n-OP, 4-n-NP） in water by ultra performance liquid chromatography- tandem mass spectrometry （UPLC/MS/MS）. The water samples were extracted and condensed with solid-phase extraction （SPE） using C18 cartridges and eluted by acetonitrile. Separation was carried out with Acquity BEH C8 column and detection were performed by UPLC/MS/MS. Quantification was calculated by using the internal standard BPA-d16 and 4-n-NP-d8. The linear correlation coefficients of these compounds in the range of 1.0-100.0μg/L were all over 0.999. The minimum detectable concentrations were 0.75-1.0 ng/L, and the recoveries ranged from 87.0% to 106.9%.展开更多
An improved method for trace level quantification of dicyandiamide in stream water has been developed. This method includes sample pretreatment using solid phase extraction.The extraction procedure（including loading,...An improved method for trace level quantification of dicyandiamide in stream water has been developed. This method includes sample pretreatment using solid phase extraction.The extraction procedure（including loading, washing, and eluting） used a flow rate of1.0 m L/min, and dicyandiamide was eluted with 20 m L of a methanol/acetonitrile mixture（V/V = 2：3）, followed by pre-concentration using nitrogen evaporation and analysis with high performance liquid chromatography–ultraviolet spectroscopy（HPLC–UV）. Sample extraction was carried out using a Waters Sep-Pak AC-2 Cartridge（with activated carbon）.Separation was achieved on a ZIC-Hydrophilic Interaction Liquid Chromatography（ZIC-HILIC）（50 mm × 2.1 mm, 3.5 μm） chromatography column and quantification was accomplished based on UV absorbance. A reliable linear relationship was obtained for the calibration curve using standard solutions（R^2〉 0.999）. Recoveries for dicyandiamide ranged from 84.6% to 96.8%, and the relative standard deviations（RSDs, n = 3） were below 6.1% with a detection limit of 5.0 ng/m L for stream water samples.展开更多
This paper suggested a modified model of SLM which could improve its stability.In the model, an organic solution was sandwiched between two layers of supported film,which we called sandwich supported liquid membrane(S...This paper suggested a modified model of SLM which could improve its stability.In the model, an organic solution was sandwiched between two layers of supported film,which we called sandwich supported liquid membrane(SSLM).The transport experiments of La3+ were performed with SSLM containing HEH(EHP)as a carrier. The permeability coefficient (p) of La3+ were measured and some factors affecting the p were investigated. The results showed that if the pH of the feed was below 4.0,the p was increased with increasing in pH. The p was also increased when the strip acidity increases.Inspite of not enough satisfactory reproducibility on test result, the stability of the model was improved.展开更多
The extraction of La￣(3+) with hollow fiber sandwich liquid membrane was described in present paper. The theoretical equations of mass transport for this system were deduced. The permeability coefficient p of mass tr...The extraction of La￣(3+) with hollow fiber sandwich liquid membrane was described in present paper. The theoretical equations of mass transport for this system were deduced. The permeability coefficient p of mass transport and its related factors were observed experimentally. The p value was increased with increase of pH in the feed and became constant under the condition of pH over 4. The p value was the highest when the flow rate was at 30 ml/min. The value of the coefficient was lower than that of single hollow fiber supported liquid membrane under the same conditions, but the stability and concentrated capacity of the sandwich membrane was better.展开更多
The procedures of ultrasonic extraction and clean-up were optimized for the determination of polycyclic aromatic hydrocarbons (PAHs) in marine sediments. Samples were ultrasonically extracted, and the extracts were pu...The procedures of ultrasonic extraction and clean-up were optimized for the determination of polycyclic aromatic hydrocarbons (PAHs) in marine sediments. Samples were ultrasonically extracted, and the extracts were purified with a miniaturized silica gel chromatographic column and analyzed with high performance liquid chromatography (HPLC) with a fluorescence detector. Ultrasonication with methanol-dichloromethane (2:1, v/v) mixture gave higher extraction efficiency than that with dichloromethane. Among the three elution solvents used in clean-up step, dichloromethane-hexane (2:3, v/v) mixture was the most satisfactory. Under the optimized conditions, the recoveries in the range of 54.82% to 94.70% with RSDs of 3.02% to 23.22% for a spiked blank, and in the range of 61.20% to 127.08% with RSDs of 7.61% to 26.93% for a spiked matrix, were obtained for the 15 PAHs studied, while the recoveries for a NIST standard reference SRM 1941b were in the range of 50.79% to 83.78% with RSDs of 5.24% to 21.38%. The detection limits were between 0.75 ng L-1 and 10.99 ng L-1for different PAHs. A sample from the Jiaozhou Bay area was examined to test the established methods.展开更多
A novel idea of transport of yttrium(Ⅲ) metal ions through fibers supported liquid membrane in two stage processes namely source to membrane and membrane to receiving phase has been proposed.The fibers supported liqu...A novel idea of transport of yttrium(Ⅲ) metal ions through fibers supported liquid membrane in two stage processes namely source to membrane and membrane to receiving phase has been proposed.The fibers supported liquid membrane was impregnated with different concentrations carrier.The experimental variables explored were concentration of yttrium(Ⅲ) ions,pH of source phase,PC-88A concentration in membrane phase,acid concentration in receiving phase and stirring speed.The pre-concentration of yttrium(Ⅲ) ions ...展开更多
Sequential and single extraction procedures were applied to both fresh and dried Sedum Plumbizincicola leaves and stems.The extractants, different from those of soil, sediment or sewage sludge metal fractions, were wa...Sequential and single extraction procedures were applied to both fresh and dried Sedum Plumbizincicola leaves and stems.The extractants, different from those of soil, sediment or sewage sludge metal fractions, were water, 80%(v/v) ethanol, 1 mol/L Na Cl,2% HAc and 0.6 mol/L HCl. Zn, Cd and Cu in the extracts and samples were measured by flame atomic adsorption spectrometry. In sequential extraction procedures, water soluble form and ethanol soluble form are the main fractions for Zn, while water soluble form and Na Cl soluble form for Cd, and comparatively uniform distribution for Cu with the residue form most and HCl soluble form second. Single extraction procedures are used to compare the extraction efficiencies of the five reagents to screen appropriate extractants and operating conditions for liquid extraction to deal with large amount of harvested metal-contained biomass, which will pose a threat to the environment if treated improperly. The sequences of extraction efficiencies are HCl>Na Cl≈HAc>Water≈Ethanol for Zn and HCl≈Na Cl≈HAc>Water>Ethanol for Cd. As for Cu, all the five extractants cannot effectively extract Cu, but HCl achieves a higher efficiency(>70% in fresh samples, and 45%-60% in dried samples). Besides, extraction efficiencies for most extractants in fresh samples are higher than those in dried samples, and extraction efficiencies of stems and leaves for the five extractants are close. The two extraction procedures can obtain high degree of accuracy with the relative standard deviation(RSD)lower than 10%, and metal recoveries are controlled between 80%-120% with most of 90%-110%.展开更多
Using experimental data from a number of pulsed disc and doughnut solvent extraction columns, a unified correla- tion for the prediction of dispersed phase holdup that considers the effects of mass transfer is present...Using experimental data from a number of pulsed disc and doughnut solvent extraction columns, a unified correla- tion for the prediction of dispersed phase holdup that considers the effects of mass transfer is presented. Pulsed disc and doughnut solvent extraction columns （PDDC） have been used for a range of important applications such as ura- nium extraction and nuclear fuel recycling. Although the dispersed phase holdup in a PDDC has been presented by some researchers, there is still the need to develop a robust correlation that can predict the experimental dispersed phase holdup over a range of operating conditions including the effects of mass transfer direction. In this study, dis- persed phase holdup data from different literature sources for a PDDC were used to refit constants for the correlation presented by Kumar and Hartland lind. Eng. Chem. Res.,27 （1988）,131-138] which did not consider the effect of col- umn geometry. In order to incorporate the characteristic length of the PDDC （i.e. the plate spacing）, the unified cor- relation for holdup proposed by Kumar and Hartland based on data from eight different types of columns [Ind. Eng. Chem. Res.,34 （1995） 3925-3940] was refitted to the PDDC data. New constants have been presented for each hold- up correlation for a PDDC based on regression analysis using published holdup data from PDDCs that cover a range of onerating conditions and nhwical nronerties and consider the direction of mass transfer.展开更多
Enantioselective liquid–liquid extraction has attracted considerable attention for its potential use in largescale production. Kinetic data are needed for the reliable scale-up of the process. This paper reports the ...Enantioselective liquid–liquid extraction has attracted considerable attention for its potential use in largescale production. Kinetic data are needed for the reliable scale-up of the process. This paper reports the kinetic study of reactive extraction of phenylalanine(Phe) enantiomers with BINAP–copper complex(BINAP–Cu) as a chiral selector. The theory of extraction accompanied by a chemical reaction was applied.The effects of agitation speed, interfacial area, p H value of aqueous phase, initial concentration of Phe enantiomers and initial concentration of BINAP–Cu on the specific rate of extraction were investigated. The forward rate constants of the reactions in the reactive extraction process are 7.93 × 10-5m5/2·mol-1/2·s-1for D-Phe and 1.29 × 10-4m5/2·mol-1/2·s-1for L-Phe.展开更多
In this work, the liquid-liquid two-phase mass transfer characteristics in the microchannel with deformed insert were studied. The experiment used di-(2-ethylhexyl) phosphoric acid/kerosene-Cu^(2+)as the mass transfer...In this work, the liquid-liquid two-phase mass transfer characteristics in the microchannel with deformed insert were studied. The experiment used di-(2-ethylhexyl) phosphoric acid/kerosene-Cu^(2+)as the mass transfer evaluation system. The effects of some key factors such as the total flow velocity,channel inner diameter, channel length, insert diameter, extractant concentration on the extraction efficiency and mass transfer coefficient were systematically investigated. Compared with a simple microreactor, the liquid-liquid mass transfer enhancement effect of the insert was quantitatively analyzed. The study found that the regular deformation of the insert could cause fluid interface deformation and promote flow state chaos, effectively increasing the mass transfer rate. And the enhancement effect of the insert was more significant at high flow velocities. The highest mass transfer coefficient in the microchannel with deformed insert was 7.886 s^(-1), the enhancement factor could reach 4.17. And only needed 0.095 s to approach the extraction equilibrium. The deformed center insert exhibited an effective liquid-liquid mass transfer enhancement effect, which can be used as a micro-chemical process enhancement method to be applied in the fields of higher throughput mass transfer and chemical synthesis,and at the same time provide ideas for development and structural optimization of microreactors.展开更多
基金supported by the National Natural Science Foundation of China(41325010)
文摘This study describes the development and validation of a sensitive and reliable method for determination of polybrominated diphenyl ethers（PBDEs）in atmospheric particulate matter using selective pressurized liquid extraction（SPLE）and gas chromatography–mass spectrometry with a negative chemical ionization（GC-NCI-MS）.Extraction and clean-up were performed using PLE with 2 g florisil and 3 g silica placed in the extraction cells.Under optimal conditions,14 PBDEs were extracted at 70℃ using hexane/dichloromethane（50：50,v/v）as solvent.Validation of SPLE returned excellent recoveries for most analytes,with relative standard deviations mostly below20%.Method detection limits ranged from 0.13 to15.38 ng·mL^-1 for the GC-MS analyses.The method was successfully applied to atmospheric particulate matter of Beijing,where analytes were detected in the range of182.79 to 468.99 pg·m^-3.
基金Funded by the Scientific Research Foundation for the Returned Overseas Chinese Scholars, State Education Ministry (ROCS, SEM [2005] No. 383)
文摘A novel process for separation of red （Y2O3：Eu^3＋）, blue（BaMgAl10O17：Eu^2＋） and green （CeMgAl10O17：Tb^3） rare earth fluorescent powders was proposed. At first, the blue powder can be extracted selectively from an aqueous solution using a chelating collector 2-thenoyltrifluoroacetone （TTA） dissolved in heptane at alkaline pH condition, then, chloroform was used for extracting the green powder into organic phase. The red phosphor remains in aqueous phase with potassium sodium tartrate depressant （PST）. Therefore, three phosphors can be separated successfully from their artificial mixtures by liquid/liquid extraction, and grades and recovery of separated products reach respectively as follows： red is 96.9% and 95.2%, blue is 82.7% and 98.8%, green is 94.6% and 82.6%.
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diketone type chelating ligands have high coordinative activity and selectivity, and are widely applied in analytical chemistry. In order to obtain profounder understanding to the properties of bis(4 acylpyrazolone 5), A new 4 acylpyrazol 5 one derivative (H 2BPMPP) was syntheszed, which contains a heterocyclic ring between two 1 phenyl 3 methyl 4 acylpyrazol 5 one rings. The new compound was characterized by element analyses, UV, IR and 1H NMR spectra. The equilibrium of the keto enol tautomerism was studied. The results show that a lower dielectric constant of solvent favors the enol form which has a higher λ max . Due to special merits of paraffin wax, the solid liquid extraction behavior of Ce(Ⅲ) with molten paraffin wax as a diluent was also investigated at higher temperature. The value of the pH 1/2 was 3.19 and the value of log K ex was 3.467. The chemical composition of the complex was obtained by the slope analysis method.
文摘Three extraction methods were compared for their efficiency to analyze sitagliptin and simvastatin in rat plasma by LC-MS/MS, including （1） liquid-liquid extraction （LLE）, （2） solid phase extraction （SPE） and （3） supported liquid extraction （SLE）. Comparison of recoveries of analytes with different extraction methods revealed that SLE was the best extraction method. The detection was facilitated with ion trap-mass spectrometer by multiple reactions monitoring （MRM） in a positive ion mode with ESI. The transitions monitored were m./z 441.1→325.2 for simvastatin, 408.2→235.1 for sitagliptin and 278.1→260.1 for the IS. The lower limit of quantification （LLOQ） was 0.2 ng/mL for sitagliptin and 0.1 ng/mL for simvastatin. The effective SLE offers enhanced chromatographic selectivity, thus facilitating the potential utility of the method for routine analysis of biological samples along with pharmacokinetic studies.
文摘A novel bioanalytical method was developed and validated for the quantitative determination of darunavir（DRV） in rat plasma by employing hydrophilic interaction chromatography and tandem mass spectrometry（HILIC-MS/MS） with supported liquid extraction（SLE）.lrbesartan（IRB） was used as an internal standard（IS）.The analyte in rat plasma（200 μL） was isolated through SLE using ethyl acetate as the eluting solvent.The chromatographic separation was achieved on Luna-HILIC（250 mm × 4.6 mm,5 μm）column with a mobile phase of 0.1% of formic acid in water：acetonitrile（5：95,v/v）,at a constant flow rate of 1.0mL/min.The MS/MS ion transitions for DRV（548.1→392.0） and IS（429.2→207.1） were monitored on an ion trap mass spectrometer,operating in the multiple reaction monitoring（MRM） mode.The lower limit of quantitation（LLOQ） was 0.2 ng/mL and quantitation range was 0.2-5000 ng/mL.The method was validated for its selectivity,sensitivity,carryover,linearity,precision,accuracy,recovery,matrix effect and stability.The method was successfully applied to pharmacokinetic study in rats.
基金Project supported by Guangdong Provincial Science and Technology Program(2015B010105008)the Dongguan Innovative Research Team Program(201536000200027)。
文摘Recovery of rare earth(RE)elements from Nd-Fe-B waste is one of the ways to solve the problem of socalled RE-crisis,An alternative approach of extracting RE elements from Nd-Fe-B waste by molten Cu extraction based on liquid-solid diffusion and reaction is reported in this paper.The extraction process,product microstructure and extraction efficiency were systematically studied.The results show that the extraction rate of RE at 1200℃is about 20%higher than that at 1100℃.The enhanced extraction efficiency at 1200℃results from the fact that the liquid Fe and Fe2 B are not co-soluble with Cu,Reducing the mass ratio of Cu to waste and the size of the waste scraps is also beneficial to enhancing the separation of RE and Fe elements.In addition,the extraction time should be well controlled,for example,less than 2 h at 1100℃,in order to avoid the increased Fe content in the extracted product.Based on optimized process,the RE elements ca n be almost fully extracted from the waste.This work thus provides an effective method to recover the RE elements.
基金EU MIRACLES project(Seventh Framework Programme KBBE-Grant Agreement No.613588,Multi-product Integrated bioRefinery of Algae:from Carbon dioxide and Light Energy to high-value Specialties).
文摘Pressurized liquid extraction using green solvents(ethanol and water)was applied to extract photosynthetic pigments from the microalgae Chlamydomonas sp.An experimental design is employed to determine the effect of the extraction conditions on the extraction yield and the antioxidant capacity of the different extracts determined using 1,1-diphenyl-2-picryl-hydrazyl and TEAC tests.All the extracts show significant antioxidant activity in all assays.Besides,in this work,the carotenoid and chlorophyll composition of the Chlamydomonas extracts was analyzed by HPLC–DAD–APCI–MS/MS for the first time,being the main compounds lutein and pheophythin a′.
基金supported by the National Natural Science Foundation of China(2014AA022103)the Zhejiang Province Public Welfare Technology Application Research Project(LGG20B060003)。
文摘A novel silver-based dihydric alcohol extractant was substituted for ionic liquids to enrich methyl linolenate(C18-3)from tallow seed oil methyl ester in this study.The interactions among dihydric alcohol,Ag(I)and C18-3 were explored by FT-IR spectroscopy.The effects of dihydric alcohol structure,carrier Ag(I)concentration,temperature and initial feed concentration on extraction yield and selectivity were reported.The good extraction performance was achieved by 1,4-butanediol containing AgBF4.The complexation of Ag(I)with C18-3 was dominant in extraction operation rather than physical partition.Furthermore,a multi-step reverse extraction method was proposed to obtain C18-3 product and regenerate the extractant.1-Hexene as the stripping phase can facilitate C18-3 reverse extraction.The content of C18-3 in the product was up to 93.36%,and the yield was 73.76%.This work opened a new route for the utilization of the dihydric alcohol properties to manipulate the carrier efficiency for extracting unsaturated fatty acid methyl esters at a lower cost.
基金supported by the National Natural Science Foundation of China(11475112)the Ph.D.Programs of Foundation of Ministry of Education of China(20130073120051)
文摘The extraction behavior of several lanthanides（La^3＋, Eu^3＋, Lu^3＋） from nitric acid（HNO3） solution was studied using a novel extraction system based on 2,6-bis（5,6-dihexyl-1,2,4-triazin-3-yl） pyridine（isohexyl-BTP） as extractant in 1-alkyl-3-methylimidazolium bis（trifluoromethylsufonyl）imide（[Cnmim][NTf2]） ionic liquid. Isohexyl-BTP in ionic liquids exhibited remarkably better extraction performance for lanthanides than that in octanol-dodecane（3：7 v/v） system. Lower HNO3 concentration and short alkyl chain length of [Cnmim]^＋ were more favourable for removal of lanthanides. Besides, it was confirmed that isohexyl-BTP in ILs formed a 1：3 complex [Ln（BTP）3（NO3）n]^（3–n）＋（n=0, 1） by slope analysis. In addition, [C2mim][NTf2] preferred to extract lanthanides via a cation exchange mechanism at lower acidity, which was proved via UV-Vis measurement. It was speculated that extraction mechanism shifted from cation exchange to neutral species extraction with increase in HNO3 concentration and alkyl chain length of [Cnmim]^＋ due to the H^＋ completion, NO3^- inhibition and hydrophobicity of IL.
基金supported by the Preventive medicine and public health research project of Anhui,China(No.2011Y0103)the Natural Science Foundation of Anhui,China(No.11040606M216)
文摘To establish an analytical method for determination of four bisphenols （BPA, BPB, BPF, and BPS） and two alkylphenols （4-n-OP, 4-n-NP） in water by ultra performance liquid chromatography- tandem mass spectrometry （UPLC/MS/MS）. The water samples were extracted and condensed with solid-phase extraction （SPE） using C18 cartridges and eluted by acetonitrile. Separation was carried out with Acquity BEH C8 column and detection were performed by UPLC/MS/MS. Quantification was calculated by using the internal standard BPA-d16 and 4-n-NP-d8. The linear correlation coefficients of these compounds in the range of 1.0-100.0μg/L were all over 0.999. The minimum detectable concentrations were 0.75-1.0 ng/L, and the recoveries ranged from 87.0% to 106.9%.
基金Department of Chemistry at Mississippi State University for financial support for this project
文摘An improved method for trace level quantification of dicyandiamide in stream water has been developed. This method includes sample pretreatment using solid phase extraction.The extraction procedure（including loading, washing, and eluting） used a flow rate of1.0 m L/min, and dicyandiamide was eluted with 20 m L of a methanol/acetonitrile mixture（V/V = 2：3）, followed by pre-concentration using nitrogen evaporation and analysis with high performance liquid chromatography–ultraviolet spectroscopy（HPLC–UV）. Sample extraction was carried out using a Waters Sep-Pak AC-2 Cartridge（with activated carbon）.Separation was achieved on a ZIC-Hydrophilic Interaction Liquid Chromatography（ZIC-HILIC）（50 mm × 2.1 mm, 3.5 μm） chromatography column and quantification was accomplished based on UV absorbance. A reliable linear relationship was obtained for the calibration curve using standard solutions（R^2〉 0.999）. Recoveries for dicyandiamide ranged from 84.6% to 96.8%, and the relative standard deviations（RSDs, n = 3） were below 6.1% with a detection limit of 5.0 ng/m L for stream water samples.
文摘This paper suggested a modified model of SLM which could improve its stability.In the model, an organic solution was sandwiched between two layers of supported film,which we called sandwich supported liquid membrane(SSLM).The transport experiments of La3+ were performed with SSLM containing HEH(EHP)as a carrier. The permeability coefficient (p) of La3+ were measured and some factors affecting the p were investigated. The results showed that if the pH of the feed was below 4.0,the p was increased with increasing in pH. The p was also increased when the strip acidity increases.Inspite of not enough satisfactory reproducibility on test result, the stability of the model was improved.
文摘The extraction of La￣(3+) with hollow fiber sandwich liquid membrane was described in present paper. The theoretical equations of mass transport for this system were deduced. The permeability coefficient p of mass transport and its related factors were observed experimentally. The p value was increased with increase of pH in the feed and became constant under the condition of pH over 4. The p value was the highest when the flow rate was at 30 ml/min. The value of the coefficient was lower than that of single hollow fiber supported liquid membrane under the same conditions, but the stability and concentrated capacity of the sandwich membrane was better.
基金supported by the National Natural Science Foundation of China (Grant No.20775074)
文摘The procedures of ultrasonic extraction and clean-up were optimized for the determination of polycyclic aromatic hydrocarbons (PAHs) in marine sediments. Samples were ultrasonically extracted, and the extracts were purified with a miniaturized silica gel chromatographic column and analyzed with high performance liquid chromatography (HPLC) with a fluorescence detector. Ultrasonication with methanol-dichloromethane (2:1, v/v) mixture gave higher extraction efficiency than that with dichloromethane. Among the three elution solvents used in clean-up step, dichloromethane-hexane (2:3, v/v) mixture was the most satisfactory. Under the optimized conditions, the recoveries in the range of 54.82% to 94.70% with RSDs of 3.02% to 23.22% for a spiked blank, and in the range of 61.20% to 127.08% with RSDs of 7.61% to 26.93% for a spiked matrix, were obtained for the 15 PAHs studied, while the recoveries for a NIST standard reference SRM 1941b were in the range of 50.79% to 83.78% with RSDs of 5.24% to 21.38%. The detection limits were between 0.75 ng L-1 and 10.99 ng L-1for different PAHs. A sample from the Jiaozhou Bay area was examined to test the established methods.
基金supported by Department of Science and Technology,Government of India (GAP 271526)
文摘A novel idea of transport of yttrium(Ⅲ) metal ions through fibers supported liquid membrane in two stage processes namely source to membrane and membrane to receiving phase has been proposed.The fibers supported liquid membrane was impregnated with different concentrations carrier.The experimental variables explored were concentration of yttrium(Ⅲ) ions,pH of source phase,PC-88A concentration in membrane phase,acid concentration in receiving phase and stirring speed.The pre-concentration of yttrium(Ⅲ) ions ...
基金Project(2013CB228106)supported by the National Key Basic Research Program of ChinaProject(2012AA06A204)supported by the National High Technology Research and Development Program of China
文摘Sequential and single extraction procedures were applied to both fresh and dried Sedum Plumbizincicola leaves and stems.The extractants, different from those of soil, sediment or sewage sludge metal fractions, were water, 80%(v/v) ethanol, 1 mol/L Na Cl,2% HAc and 0.6 mol/L HCl. Zn, Cd and Cu in the extracts and samples were measured by flame atomic adsorption spectrometry. In sequential extraction procedures, water soluble form and ethanol soluble form are the main fractions for Zn, while water soluble form and Na Cl soluble form for Cd, and comparatively uniform distribution for Cu with the residue form most and HCl soluble form second. Single extraction procedures are used to compare the extraction efficiencies of the five reagents to screen appropriate extractants and operating conditions for liquid extraction to deal with large amount of harvested metal-contained biomass, which will pose a threat to the environment if treated improperly. The sequences of extraction efficiencies are HCl>Na Cl≈HAc>Water≈Ethanol for Zn and HCl≈Na Cl≈HAc>Water>Ethanol for Cd. As for Cu, all the five extractants cannot effectively extract Cu, but HCl achieves a higher efficiency(>70% in fresh samples, and 45%-60% in dried samples). Besides, extraction efficiencies for most extractants in fresh samples are higher than those in dried samples, and extraction efficiencies of stems and leaves for the five extractants are close. The two extraction procedures can obtain high degree of accuracy with the relative standard deviation(RSD)lower than 10%, and metal recoveries are controlled between 80%-120% with most of 90%-110%.
文摘Using experimental data from a number of pulsed disc and doughnut solvent extraction columns, a unified correla- tion for the prediction of dispersed phase holdup that considers the effects of mass transfer is presented. Pulsed disc and doughnut solvent extraction columns （PDDC） have been used for a range of important applications such as ura- nium extraction and nuclear fuel recycling. Although the dispersed phase holdup in a PDDC has been presented by some researchers, there is still the need to develop a robust correlation that can predict the experimental dispersed phase holdup over a range of operating conditions including the effects of mass transfer direction. In this study, dis- persed phase holdup data from different literature sources for a PDDC were used to refit constants for the correlation presented by Kumar and Hartland lind. Eng. Chem. Res.,27 （1988）,131-138] which did not consider the effect of col- umn geometry. In order to incorporate the characteristic length of the PDDC （i.e. the plate spacing）, the unified cor- relation for holdup proposed by Kumar and Hartland based on data from eight different types of columns [Ind. Eng. Chem. Res.,34 （1995） 3925-3940] was refitted to the PDDC data. New constants have been presented for each hold- up correlation for a PDDC based on regression analysis using published holdup data from PDDCs that cover a range of onerating conditions and nhwical nronerties and consider the direction of mass transfer.
基金Supported by the National Natural Science Foundation of China(21171054)the Open Fund Project of Key Laboratory in Hunan University(11K029)the Key Laboratory of Hunan Province and Aid program for Science and Technology Innovative Research Team in Higher Educational Institutions of Hunan Province
文摘Enantioselective liquid–liquid extraction has attracted considerable attention for its potential use in largescale production. Kinetic data are needed for the reliable scale-up of the process. This paper reports the kinetic study of reactive extraction of phenylalanine(Phe) enantiomers with BINAP–copper complex(BINAP–Cu) as a chiral selector. The theory of extraction accompanied by a chemical reaction was applied.The effects of agitation speed, interfacial area, p H value of aqueous phase, initial concentration of Phe enantiomers and initial concentration of BINAP–Cu on the specific rate of extraction were investigated. The forward rate constants of the reactions in the reactive extraction process are 7.93 × 10-5m5/2·mol-1/2·s-1for D-Phe and 1.29 × 10-4m5/2·mol-1/2·s-1for L-Phe.
基金financially supported by the National Natural Science Foundation of China (21776180)the Key Research Development Project of Sichuan Province (21ZDYF4086)the National Natural Science Foundation of China (22108177)。
文摘In this work, the liquid-liquid two-phase mass transfer characteristics in the microchannel with deformed insert were studied. The experiment used di-(2-ethylhexyl) phosphoric acid/kerosene-Cu^(2+)as the mass transfer evaluation system. The effects of some key factors such as the total flow velocity,channel inner diameter, channel length, insert diameter, extractant concentration on the extraction efficiency and mass transfer coefficient were systematically investigated. Compared with a simple microreactor, the liquid-liquid mass transfer enhancement effect of the insert was quantitatively analyzed. The study found that the regular deformation of the insert could cause fluid interface deformation and promote flow state chaos, effectively increasing the mass transfer rate. And the enhancement effect of the insert was more significant at high flow velocities. The highest mass transfer coefficient in the microchannel with deformed insert was 7.886 s^(-1), the enhancement factor could reach 4.17. And only needed 0.095 s to approach the extraction equilibrium. The deformed center insert exhibited an effective liquid-liquid mass transfer enhancement effect, which can be used as a micro-chemical process enhancement method to be applied in the fields of higher throughput mass transfer and chemical synthesis,and at the same time provide ideas for development and structural optimization of microreactors.
