Separation of Red (Y_2O_3:Eu^(3+)), Blue (BaMgAl_(10)O_(17):Eu^(2+)) and Green (CeMgAl_(10)O_(17):Tb^3) Rare Earth Phosphors by Liquid/Liquid Extraction

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%.

Synthesis of 2, 6 Bis(1′-Phenyl- 3′- Methyl-5′-Oxopyrazole- 4′) Pyridinediacyl and Its Solid Liquid Extraction Behavior for Ce(Ⅲ)

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.

Comparison of conventional and supported liquid extraction methods for the determination of sitagliptin and simvastatin in rat plasma by LC-ESI-MS/MS

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.

Direct injection HILIC-MS/MS analysis of darunavir in rat plasma applying supported liquid extraction

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.

Pressurized Liquid Extraction of Pigments from Chlamydomonas sp.and Chemical Characterization by HPLC–MS/MS

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′.

Application of silver-based dihydric alcohol to the extraction of methyl linolenate with high extractability and stability replacing ionic liquids

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.

Study on liquid–liquid two-phase mass transfer characteristics in the microchannel with deformed insert

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.

Simultaneous Determination of Bisphenols and Alkylphenols in Water by Solid Phase Extraction and 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%.

Transport Behaviour of La^（3＋） with Hollow Fiber Sandwich Liquid Membrane Extraction System

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.

Transport of yttrium metal ions through fibers supported liquid membrane solvent extraction

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 ...

Transport Behaviour of La^（3＋） with Flat－Sheet－Sandwich Supported Liquid Membrane Extraction System

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.

Liquid chromatography tandem mass spectrometry method for the estimation of lamotrigine in human plasma:Application to a pharmacokinetic study

A reliable,selective and sensitive liquid chromatography tandem mass spectrometry method was developed and validated for the quantification of lamotrigine in human plasma using lamotrigine13C3,d3 as an internal standard.Analyte and internal standard were extracted from human plasma by solid-phase extraction and detected in positive ion mode by tandem mass spectrometry with electrospray ionization（ESI） interface.Chromatographic separation was performed on a Chromolith s SpeedROD;RP-18e column（50-4.6 mm i.d.） using acetonitrile：570.1 mM ammonium formate solution（90：10,v/v） as the mobile phase at a flow rate of 0.500 mL/min.The calibration curves were linear over the range of 5.02-1226.47 ng/mL with the lower limit of quantitation validated at 5.02 ng/mL.The analytes were found stable in human plasma through three freeze（-20℃）-thaw（ice-cold water bath） cycles and under storage on bench-top in ice-cold water bath for at least 6.8 h,and also in the mobile phase at 10℃ for at least 57h.The method has shown good reproducibility,as the intra-and inter-day precisions were within 3.0%,while the accuracies were within 76.0% of nominal values.The validated LC-MS/MS method was applied for the evaluation of pharmacokinetic and bioequivalence parameters of lamotrigine after an oral administration of 50mg lamotrigine tablet to thirty-two healthy adult male volunteers.

Effective rare earth extraction from Nd-Fe-B waste by liquid cuprum extraction method

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.

Enrichment of Trace Scandium with Microcrystalline Naphthalene and Subsequent ICP-AES Determination

A new method is proposed to preconcentrate and separate trace scandium from a large volume of aqueous solution by solid liquid extraction with microcrystalline naphthalene. Scandium oxinate can be adsorbed onto microcrystalline naphthalene quantitatively under certain conditions. The effects of various experimental parameters have been optimized. The influence of additive of cobalt (II) on recovery of scandium (III) is studied in detail. The proposed method has been used for determination of Sc in Certified Reference Material of “Vehicle Exhaust Particulates”.

Solution extraction of several lanthanides from nitric acid with isohexyl-BTP in [C_nmim][NTf_2] ionic liquid

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.

Determination of berberine in Phellodendron amurense from different sites of Changbai Mountain

Phellodendron amurense has been used for many years as a medical plant in traditional Chinese medicine and has shown great prospect in recent clinical trials for future applications. Berberine is an essential active compound contained in P. amurense. Our objective in this study was to quantify the content of berberine in P.amurense from sites at different elevations on Changbai Mountain. We collected samples of P. amurense from five different elevations on Changbai Mountain. Berberine in samples was extracted by ultrahigh pressure extraction（UPE）. And the quantity was measured by high performance liquid chromatography（HPLC）. First, the optimal HPLC conditions for berberine were identified with satisfactory precision（relative standard deviation, R SD／5.6 %）, good accuracy（relative error, R E／ 3.6 %） and good linear relation（R2= 0.9998） in the range of 6.576–328.8 mg L-1. Second, the combination of UPE and HPLC methods in quantitative analysis of berberine showed high repeatability（R SD= 3.28 %）, reproducibility（R SD= 4.72 %）,stability（R SD／ 1.27 %） and good recovery（99.54 %） for real plant materials. Samples from Heilongjiang Province at the lowest elevation contained the highest amount of berberine.Similarly, the lowest amount of berberine was recorded in samples from Changbai Forest Bureau of Jilin Province collected at the highest elevation in this paper. The proposed UPE–HPLC method is simple, reliable and low-cost for quantitative analysis of berberine. Content of berberine in P.amurense varied significantly by site on Changbai Mountain.

Analysis of trace dicyandiamide in stream water using solid phase extraction and liquid chromatography UV spectrometry

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.

Quantification of perfluorinated compounds in atmospheric particulate shows potential connection with environmental event

A method of quantification of perfluorinated compounds(PFCs)from atmospheric particulate matter(APM)is described.A single step pretreatment method,selective pressurized liquid extraction(SPLE),was developed to reduce the high matrix background and avoid contamination from commonly used multiple sample pretreatment steps.An effective sorbent was selected to purify the PFCs during SPLE,followed by liquid chromatography-tandem mass spectrometry(LC–MS/MS),for quantification of PFCs.Conditions affecting the SPLE efficiency,including temperature,static extraction time,and number of extraction cycles used,were studied.The optimum conditions were found to be 120℃,10 min,and 3 cycles,respectively.LC-MS/MS method was developed to obtain the optimal sensitivity specific to PFCs.The method detection limits(MDLs)were 0.006 to 0.48 ng/g for the PFCs studied and the linear response range was from 0.1 to 100 ng/g.To ensure accurate values were obtained,each step of the experiment was evaluated and controlled to prevent contamination.The optimized method was tested by performing spiking experiments in natural particulate matter matrices and good rates of recovery and reproducibility were obtained for all target compounds.Finally,the method was successfully used to measure 16 PFCs in the APM samples collected in Beijing over five years from 2015 to 2019.It is observed that some PFCs follow the trend of total PFC changes,and can be attributed to the environment influencing events and policy enforcement,while others don't seem to change as much with time of the year or from year to year.

N-Nitrosamine formation from chloramination of two common ionic liquids

Ionic liquids(ILs)are a class of solvents increasingly used as"green chemicals."Widespread applications of ILs have led to concerns about their accidental entry to the environment.ILs have been assessed for some environmental impacts;however,little has been done to characterize their potential impacts on drinking water if ILs accidentally enter surface water.IL cations are often aromatic or alkyl quaternary amines that resemble structures of previously confirmed N-nitrosamine(NA)precursors.Therefore,this study has evaluated two common ILs,1-ethyl-3-methylimidazolium bromide(EMIm Br)and 1-ethyl-1-methylpyrrolidinium bromide(EMPyr Br),for their NA formation potential.Each IL species was reacted with pre-formed monochloramine under various laboratory conditions.The reaction mixtures were extracted using liquid–liquid extraction and analyzed for NAs using high performance liquid chromatography tandem mass spectrometry.At low concentration of IL(250μmol/L),the yields of NAs(NMEA or NPyr)increased with increasing doses of monochloramine from both IL species.The total NA yield was as high as 2.5±0.3 ng/mg from EMIm Br,and as high as 8.6±0.8 ng/mg from EMPyr Br.At high concentration of IL(5 mmol/L),the NA yield reached a maximum at 2.5 mmol/L NH2Cl,and then decreased with subsequent increases in the reactant concentrations,demonstrating ILs’solvent effects.This study re-emphasizes the importance of preventing discharge of ILs to water bodies to prevent secondary impacts on drinking water.

Extractive desulfurization of fuel oil with metal-based ionic liquids

Several metal-based ionic liquids（ILs） were synthesized and used as extractants for the desulfurization of dibenzothiophene（DBT） in simulated fuel oil.The effects of several anion and metal ions,n（ILs）/n（metal） as mole ratio,V（IL）/V（oil） and extractive times on the removal ratio of DBT were investigated in detail.The results showed that[BMIM]HSO4/FeCl3（BMIM was short for l-butyl-3-methyl imidazole）was superior to the other ILs for the extractive desulfurization.A total of 100%of DBT was removed at room temperature in 5 min with V[BMIM]HSO4/Fecl3/Voil = 1：1.The extractive activity of[BMIM]HSO4/FeCl3 IL did not change almost after five runs.Extractive desulfurization of different sulfur compounds and commercial diesel fuel oil were also examined.The removal ratios of the sulfur compounds as the reaction substrates were all over 90%and the sulfur content of commercial diesel oil decreased to120 ppm from 12,400 ppm.