Aim An HPLC method for analyzing eleutheroside B (ELU B) and eleutheroside E(ELU E) , two of the main active substances of Acanthopanax preparations were studied. Methods Thesamples were analyzed on a kromasil ODS col...Aim An HPLC method for analyzing eleutheroside B (ELU B) and eleutheroside E(ELU E) , two of the main active substances of Acanthopanax preparations were studied. Methods Thesamples were analyzed on a kromasil ODS column with water-acetonitrile as a gradient mobile phase.The flow rate was 0.8 mL·min^(-1) and detecting wavelengths were 206 nm for ELU B, 220 nm for ELUE, solid phase extraction (SPE) and internal standard-salicin were selected. Results The recoveriesof Acanthopanax tablets and injection were 90.4% - 96.8% and 96.4% - 99.8% for ELU B, 87.7% -93.3%and 95.7% - 98.5% for ELU E, respectively. The linear ranges were 4.45 - 22.25 μg· mL^(-1) (r =0.999 8) and 5.11 - 25.55 μg·mL^(-1) ( r = 0.999 7) respectively. Conclusion This method can savethe time for cleaning the chromatographic system and improve sensitivity for Acanthopanaxpreparations , thus providing a way to evaluate the quality of Acanthopanax preparations.展开更多
This work describes a systematic approach to the development of a method for simultaneous determination of three classes of veterinary antibiotics in the suspended solids （SS） of swine wastewater, including five sul...This work describes a systematic approach to the development of a method for simultaneous determination of three classes of veterinary antibiotics in the suspended solids （SS） of swine wastewater, including five sulfonamides, three tetracyclines and one macrolide （tiamulin）. The entire procedures for sample pretreatment, ultrasonic extraction （USE）, solid-phase extraction （SPE）, and liquid chromatography-mass spectrometry （LC-MS） quantification were examined and optimized. The recovery efficiencies were found to be 76%-104% for sulfonamides, 81%-112% for tetracyclines, and 51%--64% for tiamulin at three spiking levels. The intra-day and inter-day precisions, as expressed by the relative standard deviation （RSD）, were below 17%. The method detection limits （MDLs） were between 0.14 and 7.14 μg/kg, depending on a specific antibiotic studied. The developed method was applied to field samples collected from three concentrated swine feeding plants located in Beijing, Shanghai and Shandong province of China. All the investigated antibiotics were detected in both SS and liquid phase of swine wastewater, with partition coefficients （logKd） ranging from 0.49 to 2.30. This study demonstrates that the SS can not be ignored when determining the concentrations of antibiotics in swine wastewater.展开更多
The study introduces eco-friendly leaching agents as alternatives to traditional rare earth element(REE)extraction solvents,addressing environmental concerns associated with ammonium sulfate.Bio-based ionic liquids(IL...The study introduces eco-friendly leaching agents as alternatives to traditional rare earth element(REE)extraction solvents,addressing environmental concerns associated with ammonium sulfate.Bio-based ionic liquids(ILs),known for their non-toxic and biodegradable properties,were screened using the COSMO-RS software.Initially,105 ILs involving 7 cations and 15 anions were computationally screened to find the best ILs for REE extraction.The chosen criteria were based on hydrogen bond formation,affinity screening,hydrophobicity,viscosity,and eco-toxicity test.Based on the COSMO-RS screening,choline oleate,choline decanoate,and choline hexanoate exhibit high solubility for REEs,with a chemical potential of 17.60,17.01,and 18.37 kcal/mol at REE oxidation state+2.Choline glycinate,choline oleate,choline decanoate,choline hexanoate,choline lysinate,and choline leucinate were selected for their strong affinity to extract REE dissociate ions.Experimental results show slightly higher REE extraction from ammonium sulfate(3.17 ppm)compared to choline glycinate(3.15 ppm).For long-term applications,choline glycinate offers a promising eco-friendly and cost-effective alternative to traditional leaching agents,promoting economic feasibility and environmental friendliness.展开更多
Rare earth elements(REEs) were extracted from phosphogypsum(PG) using an indirect leaching method that produces CaCO_(3).The carbonation process transforms PG into CaCO_(3),and a potential source of value is the(NH_(4...Rare earth elements(REEs) were extracted from phosphogypsum(PG) using an indirect leaching method that produces CaCO_(3).The carbonation process transforms PG into CaCO_(3),and a potential source of value is the(NH_(4))_(2)SO_(4) fertilizer.The calcium carbonate byproduct is rich in REEs that are originally present in PG.Calcium carbonate,a byproduct of PG carbonation and a rich source of REEs,could dissolve in nitric acid to produce a calcium nitrate leach solution that contains RE nitrate.Subsequently,the most widely used solvent extraction technique can make use of an environmentally benign nitrate ionic liquid.Cyphos IL 101(trihexyl(tetradecyl)phosphonium chloride) is transformed into trihexyl(tetradecyl)phosphonium nitrate([P_(66614)][NO_(3)]) ionic liquid by adding 2.5 mol/L potassium nitrate.The extraction examinations were tested by equilibration of 2 mL of [P_(66614)][NO_(3)] with 2 mL of a synthetic solution of 1000 mg/L of individual La,Ce,and Nd to gain the optimal extraction conditions.The high extraction efficiency of La,Ce,and Nd was gained by stirring a 1/1 aqueous/organic phase ratio and 3 mol/L NH_(4)NO_(3)(as salting out) at 800 r/min for 40 min at 50℃ to decrease the viscosity of [P_(66614)][NO_(3)].The La(Ⅲ),Ce(Ⅲ),and Nd(Ⅲ) stripping efficiencies were examined from their loaded [P_(66614)][NO_(3)] ionic liquid by 1/1 A/O ratio of acidified water,800 r/min stirring speed,and 25℃.After nine cycles,the extraction and stirring efficiency for the La,Ce,and Nd drop to about 80%.The extraction and stripping parameters are applied to the RE leachate from PG to gain the RE oxide with an assay of 92.67%.展开更多
The aim of this work was to develop an automated on-line solid phase extraction(SPE)with liquid chromatography-tandem mass spectrometry method for the detection of fifteen sulfonamides in pork and fish samples.Samples...The aim of this work was to develop an automated on-line solid phase extraction(SPE)with liquid chromatography-tandem mass spectrometry method for the detection of fifteen sulfonamides in pork and fish samples.Samples were extracted with 0.2%formic acid acetonitrile solution,purified by on-line SPE device with HLB column,then separated by XBridge C18 column,using 0.1%formic acid solution and acetonitrile as the mobile phase.Mass spectrometric data was acquired under multiple reaction monitoring(MRM)mode using positive ionization electrospray.Internal standard method was used in the quantification,good linear relationship was got in range of 0.1–100 ng/mL and correlation coefficient was higher than 0.9990.The limits of detection were in the range of 0.125–2.00g/kg and the limits of quantitation were in the range of 0.250–5.00g/kg.Recoveries of the method were in range of 78.3%–99.3%,relative standard deviation were lower than 10%.The method was simple,sensitivity,and could be used for routine supervision and analysis of fifteen sulfonamides in pork and fish.展开更多
[Objective] This study aimed to develop a method of C_18-functionalized magnetic silica nanoparticles solid phase extraction-high performance liquid chro- matography-tandem mass spectrometry for the determination of s...[Objective] This study aimed to develop a method of C_18-functionalized magnetic silica nanoparticles solid phase extraction-high performance liquid chro- matography-tandem mass spectrometry for the determination of sulfadimidine in royal jelly. [Method] The royal jelly samples were pretreated by MCX SPE column and C_18-functionalized magnetic silica nanoparticles, and the purified samples were de- tected by HPLC-MS/MS. [Result] The detection method showed a good linear rela- tionship in the range of 5-80 ugkg （r=0.993 1）. The recovery ranges were between 93%- 104% with the relative standard deviations （RSD） below 11.3%. [Conclusion] Combined with automation equipment, the method is simple, fast, time-saving, and easy to real- ize the automation of sulfadimidine in the royal jelly samples before determination.展开更多
A convenient,cost-effective and fast method using dynamic microwave-assisted extraction and liquid phase microextraction based on the solidification of a floating drop was proposed to analyze organochlorine pesticides...A convenient,cost-effective and fast method using dynamic microwave-assisted extraction and liquid phase microextraction based on the solidification of a floating drop was proposed to analyze organochlorine pesticides in grains including rice,maize and millet.Twelve samples can be processed simultaneously in the method.During the extraction process,10%acetonitrile-water solutions containing 110μL of n-hexadecane were used to extract organochlorine pesticides.Subsequently,1.0 g sodium chloride was placed in the extract,and then centrifuged and cooled.The n-hexadecane drops containing the analytes were solidifi ed and transferred for determination by gas chromatography-electron capture detector without any further filtration or cleaning process.Limits of detection for organochlorine pesticides were 0.97–1.01μg/kg and the RSDs were in the range of 2.6%–8.5%.The developed technology has succeeded in analyzing six real grains samples and the recoveries of the organochlorine pesticides were 72.2%–94.3%.Compared with the published extraction methods,the developed method was used to analyze organochlorine pesticides in grains,being more environmentally friendly,which is suitable for the daily determination of organochlorine pesticides.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
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
To assess uncertainty of determination of MC-LR in environmental samples by solid phase extraction- ultra performance liquid chromatography- tandem mass spectrometry,the sources of the uncertainty were evaluated first...To assess uncertainty of determination of MC-LR in environmental samples by solid phase extraction- ultra performance liquid chromatography- tandem mass spectrometry,the sources of the uncertainty were evaluated firstly,and the expanded uncertainty was calculated finally.The results show that when MC-LR concentration in the water samples was 0.50 μg/L,the expanded uncertainty was 0.00628 μg/L(k=2).展开更多
An efficient preparative method was successfully developed for isolation and purification of unstable components from medicinal plant extracts, using a combined method of preparative high performance liquid chro-matog...An efficient preparative method was successfully developed for isolation and purification of unstable components from medicinal plant extracts, using a combined method of preparative high performance liquid chro-matography(HPLC) and solid-phase extraction(SPE). The aim of this study was to obtain an effective method with high preparative efficiency and importantly to avoid the transformation of unstable compounds. The preparative HPLC system was based on an LC/MS controlled four-channel autopurification system. The SPE method was performed with a C18 packing material to trap the target compounds and to remove the acidic additive derived from the mobile phase. Using this method, the unstable iridoid glucosides(IGs) as model compounds were successfully isolated and purified from the extract of Hedyotis diffusa Willd. Six IGs(including one new minor IG) and one nucleotide compound were simultaneously obtained, each with a purity of 91% as determined by HPLC. The structures of the isolated compounds were identified by UPLC/Q-TOF MS, UV, 1D and/or 2D NMR. It was demonstrated that the combination of preparative HPLC with SPE is a versatile tool for preparative purification of unstable compounds from complex natural products.展开更多
An on-line solid phase extraction-high performance liquid chromatography-tandem mass spectrometry method for the analysis of perfluoroalkyl substances（PFASs） in water samples was developed.The optimal analytical con...An on-line solid phase extraction-high performance liquid chromatography-tandem mass spectrometry method for the analysis of perfluoroalkyl substances（PFASs） in water samples was developed.The optimal analytical conditions were obtained through the optimization of the extraction efficiency of online solid phase extraction column,sample loading rate and loading volume,and the concentration of ammonium acetate in mobile phase.Under the optimal condition,the analytical method displayed good linearity（r^2〉0.99） for 12 PFASs（C5-C14 perfluoroalkyl carboxylic acids and C6/C8 perfluoroalkyl sulfonic acids） over a concentration range of 0.5-100 ng/L.The limits of quantitation for samples were between 0.025 ng/L and 0.5 ng/L and the relative standard deviations（RSD） of five consecutive analyses were less than 10%for 1 ng/L standard solution.Satisfactory results were obtained using this analytical method for the analysis of perfluoroalkyl substances in Antarctic ice core samples.The recoveries of all perfluoroalkyl substances were in a range of 73%-117%when the samples were spiked with standards at the concentrations of 2.5 ng/L and 25 ng/L.展开更多
To formulate a scientific basis for a reasonable spray dose and safe interval period of 20% flubendiamide water dispersible granule (WDG) on controlling vegetable pests, degradation dynamics of flubendiamide in cabbag...To formulate a scientific basis for a reasonable spray dose and safe interval period of 20% flubendiamide water dispersible granule (WDG) on controlling vegetable pests, degradation dynamics of flubendiamide in cabbage and soil was analyzed in this study. Dissipation and residue of flubendiamide in 20% flubendiamide WDG in cabbage and soil under field conditions were investigated by liquid chromatography-tandem mass spectrometry with dispersive solid phase extraction. Results showed that the degradation dynamic equations of flubendiamide in cabbage and soil were based on the first-order reaction dynamic equations. The half-lives of the degradation of flubendiamide were 3.51 d to 3.96 d and 3.43 d to 3.87 d in the cabbage of Yangzhou and Jingzhou, respectively, and 4.42 d to 5.13 d and 4.37 d to 4.99 d in the soil of Yangzhou and Jingzhou, respectively. The terminal residues of flubendiamide in the cabbage of Yangzhou and Jingzhou were 0.0247 mg·kg-1 to 0.0393 mg·kg-1 and 0.0225 mg·kg-1 to 0.0273 mg·kg-1, respectively, when 20% flubendiamide WDG was applied at a dose of0.050g·m-2. Flubendiamide is safe to be applied in cabbage fields at the recommended dose.展开更多
A new, rapid and efficient reverse phase Liquid Chromatography (RP-LC) method was developed for determination of Gibberellin A4 (GA4) in samples of flower stalk of Dasylirion cedrosanum and vegetative tissue of Epithe...A new, rapid and efficient reverse phase Liquid Chromatography (RP-LC) method was developed for determination of Gibberellin A4 (GA4) in samples of flower stalk of Dasylirion cedrosanum and vegetative tissue of Epithelantha micromeris. Purification of GA4 was carried out by solid phase extraction (SPE), in Epithelantha micromeris. In the chromatography method was obtaining a retention time of 2.1 min, using Hypersil GOLD C-18 column (100 × 4.6 mm dim and size particle 5 μ), mobile phase 50/50 acetonitrile/water and a flow 1.0 ml/min. Detection was carried out by a UV detector set at 205 nm, and a quantization limit of 0.4 mg/L. The obtained correlation coefficient was 0.995.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
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
A fast analytical method for the simultaneous determination of 9 mycotoxins, including alfatoxins （B1, B2, G1, and G2）, fumonisins （B1, B2 and B3）, zearalenone, and deoxynivalenol in corn using dispersive solid-ph...A fast analytical method for the simultaneous determination of 9 mycotoxins, including alfatoxins （B1, B2, G1, and G2）, fumonisins （B1, B2 and B3）, zearalenone, and deoxynivalenol in corn using dispersive solid-phase extraction method and ultra-performance liquid chromatography coupled to tandem quadrupole time-of-lfight mass spectrometry （UPLC-Q-TOF-MS） was developed and validated. Samples were extracted with acetonitrile-water （84：16, v：v, containing 1% acetic acid） using ultrasonic extraction. The extracts were puriifed with a dispersive SPE method using C18 as a cleaning agent. The ifnal clear extracts were dried by nitrogen blowing and subsequently redissolved in methanol-water （5：5, v：v）. The samples were then analyzed by UPLC-Q-TOF-MS with 0.1% formic acid in ammonium acetate-methanol as mobile phase. The mean recoveries were ranged from 68.0 to 120.0%, and the relative standard deviation （RSD） ranged from 0.18 to 6.29%. Limits of detections ranged from 0.05 to 50 μg kg？1, and limits of quantiifcation ranged from 0.1 to 200 μg kg？1, which were below the legal limits set by the European Union for the legislated mycotoxins. The developed method was applied to 130 corn samples. Among the mycotoxins studied, alfatoxins B1 and fumonisins B1, B2 and B3 were the most predominant mycotoxins, and their concentrations were 0–593.12, 0–2.01×104, 0–6.94×103 and 0–3.05×103 μg kg–1, respectively.展开更多
The extraction behavior of rare earths was studied by using paraffin with ceresin as a diluent containing 1-phenyl-3-methyl-4-benzoyl-pyrazolone-5.In solid phase,the composition of complexes is REP_3.The equilib- rium...The extraction behavior of rare earths was studied by using paraffin with ceresin as a diluent containing 1-phenyl-3-methyl-4-benzoyl-pyrazolone-5.In solid phase,the composition of complexes is REP_3.The equilib- rium extraction constants and pH_(1/2) values of solid-liquid extraction are higher than those of normal liquid-liquid extraction.The extraction efficiency tends to maximum when the ratio of phases is 1:1.When the extraction temperature is higher than the melting point of paraffin and the extraction time is over 10 min,the extraction efficiency keeps constant.Moreover,the relationship among separation factor,equilibrium extrac- tion constant,pH_(1/2) value and atomic number was obtained.The mechanism of solid-liquid extraction is analogous to that of liquid-liquid extraction.展开更多
An overview of extraction of some trace metal ions using molten solvent (lowmelting substance) during last two decades is presented. The development of this technique since itsinception is briefly traced. The comparis...An overview of extraction of some trace metal ions using molten solvent (lowmelting substance) during last two decades is presented. The development of this technique since itsinception is briefly traced. The comparison of extraction efficiency, thermodynamics and kineticsmainly involving extraction of rare earth ions between molten solvent extraction at high temperatureand usual liquid-liquid extraction at room temperature are discussed in detail. The variousparameters obtained from the previous and present studies such as equilibrium extraction constantK_(ex), pH_(1/2), thermodynamic and kinetic data are displayed in tabular form. Finally, the currentdemands, disadvantages and future prospects are also evaluated.展开更多
Silver nanoparticles were synthesized in reverse micelles consisting of sucrose fatty acid esters by dissolving reactant powder in the water pool of reverse micelles through the solid-liquid extraction. Silver nanopar...Silver nanoparticles were synthesized in reverse micelles consisting of sucrose fatty acid esters by dissolving reactant powder in the water pool of reverse micelles through the solid-liquid extraction. Silver nanoparticles having various sizes and shapes were obtained at high concentration. The size of silver nanoparticles was controlled by reaction temperature. Moreover, the size of silver nanoparticles was dependent upon the average esterification degree of sucrose fatty acid esters forming reverse micelles. The wavelength in the peaks, which corresponded upon the localized surface plasmon resonance of resultant silver nanoparticles, was correlated with their sizes.展开更多
文摘Aim An HPLC method for analyzing eleutheroside B (ELU B) and eleutheroside E(ELU E) , two of the main active substances of Acanthopanax preparations were studied. Methods Thesamples were analyzed on a kromasil ODS column with water-acetonitrile as a gradient mobile phase.The flow rate was 0.8 mL·min^(-1) and detecting wavelengths were 206 nm for ELU B, 220 nm for ELUE, solid phase extraction (SPE) and internal standard-salicin were selected. Results The recoveriesof Acanthopanax tablets and injection were 90.4% - 96.8% and 96.4% - 99.8% for ELU B, 87.7% -93.3%and 95.7% - 98.5% for ELU E, respectively. The linear ranges were 4.45 - 22.25 μg· mL^(-1) (r =0.999 8) and 5.11 - 25.55 μg·mL^(-1) ( r = 0.999 7) respectively. Conclusion This method can savethe time for cleaning the chromatographic system and improve sensitivity for Acanthopanaxpreparations , thus providing a way to evaluate the quality of Acanthopanax preparations.
基金supported by the National Natural Science Foundation of China (No. 50878206, 50921064)the Ministry of Science and Technology of China (No. 2007AA06Z344,2009BAC57B02, 2009AA063901)
文摘This work describes a systematic approach to the development of a method for simultaneous determination of three classes of veterinary antibiotics in the suspended solids （SS） of swine wastewater, including five sulfonamides, three tetracyclines and one macrolide （tiamulin）. The entire procedures for sample pretreatment, ultrasonic extraction （USE）, solid-phase extraction （SPE）, and liquid chromatography-mass spectrometry （LC-MS） quantification were examined and optimized. The recovery efficiencies were found to be 76%-104% for sulfonamides, 81%-112% for tetracyclines, and 51%--64% for tiamulin at three spiking levels. The intra-day and inter-day precisions, as expressed by the relative standard deviation （RSD）, were below 17%. The method detection limits （MDLs） were between 0.14 and 7.14 μg/kg, depending on a specific antibiotic studied. The developed method was applied to field samples collected from three concentrated swine feeding plants located in Beijing, Shanghai and Shandong province of China. All the investigated antibiotics were detected in both SS and liquid phase of swine wastewater, with partition coefficients （logKd） ranging from 0.49 to 2.30. This study demonstrates that the SS can not be ignored when determining the concentrations of antibiotics in swine wastewater.
基金supported by Petronas Research Sdn Bhd(PRSB)with grant number(015M20-129)Centre of Research in Ionic Liquids(CORIL)Universiti Teknologi PETRONAS for the facilities and support provided。
文摘The study introduces eco-friendly leaching agents as alternatives to traditional rare earth element(REE)extraction solvents,addressing environmental concerns associated with ammonium sulfate.Bio-based ionic liquids(ILs),known for their non-toxic and biodegradable properties,were screened using the COSMO-RS software.Initially,105 ILs involving 7 cations and 15 anions were computationally screened to find the best ILs for REE extraction.The chosen criteria were based on hydrogen bond formation,affinity screening,hydrophobicity,viscosity,and eco-toxicity test.Based on the COSMO-RS screening,choline oleate,choline decanoate,and choline hexanoate exhibit high solubility for REEs,with a chemical potential of 17.60,17.01,and 18.37 kcal/mol at REE oxidation state+2.Choline glycinate,choline oleate,choline decanoate,choline hexanoate,choline lysinate,and choline leucinate were selected for their strong affinity to extract REE dissociate ions.Experimental results show slightly higher REE extraction from ammonium sulfate(3.17 ppm)compared to choline glycinate(3.15 ppm).For long-term applications,choline glycinate offers a promising eco-friendly and cost-effective alternative to traditional leaching agents,promoting economic feasibility and environmental friendliness.
文摘Rare earth elements(REEs) were extracted from phosphogypsum(PG) using an indirect leaching method that produces CaCO_(3).The carbonation process transforms PG into CaCO_(3),and a potential source of value is the(NH_(4))_(2)SO_(4) fertilizer.The calcium carbonate byproduct is rich in REEs that are originally present in PG.Calcium carbonate,a byproduct of PG carbonation and a rich source of REEs,could dissolve in nitric acid to produce a calcium nitrate leach solution that contains RE nitrate.Subsequently,the most widely used solvent extraction technique can make use of an environmentally benign nitrate ionic liquid.Cyphos IL 101(trihexyl(tetradecyl)phosphonium chloride) is transformed into trihexyl(tetradecyl)phosphonium nitrate([P_(66614)][NO_(3)]) ionic liquid by adding 2.5 mol/L potassium nitrate.The extraction examinations were tested by equilibration of 2 mL of [P_(66614)][NO_(3)] with 2 mL of a synthetic solution of 1000 mg/L of individual La,Ce,and Nd to gain the optimal extraction conditions.The high extraction efficiency of La,Ce,and Nd was gained by stirring a 1/1 aqueous/organic phase ratio and 3 mol/L NH_(4)NO_(3)(as salting out) at 800 r/min for 40 min at 50℃ to decrease the viscosity of [P_(66614)][NO_(3)].The La(Ⅲ),Ce(Ⅲ),and Nd(Ⅲ) stripping efficiencies were examined from their loaded [P_(66614)][NO_(3)] ionic liquid by 1/1 A/O ratio of acidified water,800 r/min stirring speed,and 25℃.After nine cycles,the extraction and stirring efficiency for the La,Ce,and Nd drop to about 80%.The extraction and stripping parameters are applied to the RE leachate from PG to gain the RE oxide with an assay of 92.67%.
基金This work was supported by“National Key Research and Development Program of China”(Project No.2018YFC1603400)Science and Technology Program of Hebei Province(Project No.19225503D).
文摘The aim of this work was to develop an automated on-line solid phase extraction(SPE)with liquid chromatography-tandem mass spectrometry method for the detection of fifteen sulfonamides in pork and fish samples.Samples were extracted with 0.2%formic acid acetonitrile solution,purified by on-line SPE device with HLB column,then separated by XBridge C18 column,using 0.1%formic acid solution and acetonitrile as the mobile phase.Mass spectrometric data was acquired under multiple reaction monitoring(MRM)mode using positive ionization electrospray.Internal standard method was used in the quantification,good linear relationship was got in range of 0.1–100 ng/mL and correlation coefficient was higher than 0.9990.The limits of detection were in the range of 0.125–2.00g/kg and the limits of quantitation were in the range of 0.250–5.00g/kg.Recoveries of the method were in range of 78.3%–99.3%,relative standard deviation were lower than 10%.The method was simple,sensitivity,and could be used for routine supervision and analysis of fifteen sulfonamides in pork and fish.
基金Supported by the Innovation Fund for Technology Based Firms of Ministry of Science and Technology(09C26214425280)the National Key Technology R&D Program during the 12th Five-Year Plan Period(2012BAK17B10)the International S&T Cooperation and Communication Program of China(2011DFA32930)~~
文摘[Objective] This study aimed to develop a method of C_18-functionalized magnetic silica nanoparticles solid phase extraction-high performance liquid chro- matography-tandem mass spectrometry for the determination of sulfadimidine in royal jelly. [Method] The royal jelly samples were pretreated by MCX SPE column and C_18-functionalized magnetic silica nanoparticles, and the purified samples were de- tected by HPLC-MS/MS. [Result] The detection method showed a good linear rela- tionship in the range of 5-80 ugkg （r=0.993 1）. The recovery ranges were between 93%- 104% with the relative standard deviations （RSD） below 11.3%. [Conclusion] Combined with automation equipment, the method is simple, fast, time-saving, and easy to real- ize the automation of sulfadimidine in the royal jelly samples before determination.
基金The study was financially supported by the National Science and Technology Support Program of China(Grant No.2013BAD16B08).
文摘A convenient,cost-effective and fast method using dynamic microwave-assisted extraction and liquid phase microextraction based on the solidification of a floating drop was proposed to analyze organochlorine pesticides in grains including rice,maize and millet.Twelve samples can be processed simultaneously in the method.During the extraction process,10%acetonitrile-water solutions containing 110μL of n-hexadecane were used to extract organochlorine pesticides.Subsequently,1.0 g sodium chloride was placed in the extract,and then centrifuged and cooled.The n-hexadecane drops containing the analytes were solidifi ed and transferred for determination by gas chromatography-electron capture detector without any further filtration or cleaning process.Limits of detection for organochlorine pesticides were 0.97–1.01μg/kg and the RSDs were in the range of 2.6%–8.5%.The developed technology has succeeded in analyzing six real grains samples and the recoveries of the organochlorine pesticides were 72.2%–94.3%.Compared with the published extraction methods,the developed method was used to analyze organochlorine pesticides in grains,being more environmentally friendly,which is suitable for the daily determination of organochlorine pesticides.
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%.
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To assess uncertainty of determination of MC-LR in environmental samples by solid phase extraction- ultra performance liquid chromatography- tandem mass spectrometry,the sources of the uncertainty were evaluated firstly,and the expanded uncertainty was calculated finally.The results show that when MC-LR concentration in the water samples was 0.50 μg/L,the expanded uncertainty was 0.00628 μg/L(k=2).
基金Supported by the Science and Technology Plan of Liaoning Province, China(No.2006226002)the Project of the Doctor Fund of Hebei University of Science and Technology, China(No.005121)
文摘An efficient preparative method was successfully developed for isolation and purification of unstable components from medicinal plant extracts, using a combined method of preparative high performance liquid chro-matography(HPLC) and solid-phase extraction(SPE). The aim of this study was to obtain an effective method with high preparative efficiency and importantly to avoid the transformation of unstable compounds. The preparative HPLC system was based on an LC/MS controlled four-channel autopurification system. The SPE method was performed with a C18 packing material to trap the target compounds and to remove the acidic additive derived from the mobile phase. Using this method, the unstable iridoid glucosides(IGs) as model compounds were successfully isolated and purified from the extract of Hedyotis diffusa Willd. Six IGs(including one new minor IG) and one nucleotide compound were simultaneously obtained, each with a purity of 91% as determined by HPLC. The structures of the isolated compounds were identified by UPLC/Q-TOF MS, UV, 1D and/or 2D NMR. It was demonstrated that the combination of preparative HPLC with SPE is a versatile tool for preparative purification of unstable compounds from complex natural products.
基金supported by the National Natural Science Foundation of China(Nos.21377145,21321004)the Strategic Priority Research Program of the Chinese Academy of Sciences(No.XDB01020300)
文摘An on-line solid phase extraction-high performance liquid chromatography-tandem mass spectrometry method for the analysis of perfluoroalkyl substances（PFASs） in water samples was developed.The optimal analytical conditions were obtained through the optimization of the extraction efficiency of online solid phase extraction column,sample loading rate and loading volume,and the concentration of ammonium acetate in mobile phase.Under the optimal condition,the analytical method displayed good linearity（r^2〉0.99） for 12 PFASs（C5-C14 perfluoroalkyl carboxylic acids and C6/C8 perfluoroalkyl sulfonic acids） over a concentration range of 0.5-100 ng/L.The limits of quantitation for samples were between 0.025 ng/L and 0.5 ng/L and the relative standard deviations（RSD） of five consecutive analyses were less than 10%for 1 ng/L standard solution.Satisfactory results were obtained using this analytical method for the analysis of perfluoroalkyl substances in Antarctic ice core samples.The recoveries of all perfluoroalkyl substances were in a range of 73%-117%when the samples were spiked with standards at the concentrations of 2.5 ng/L and 25 ng/L.
文摘To formulate a scientific basis for a reasonable spray dose and safe interval period of 20% flubendiamide water dispersible granule (WDG) on controlling vegetable pests, degradation dynamics of flubendiamide in cabbage and soil was analyzed in this study. Dissipation and residue of flubendiamide in 20% flubendiamide WDG in cabbage and soil under field conditions were investigated by liquid chromatography-tandem mass spectrometry with dispersive solid phase extraction. Results showed that the degradation dynamic equations of flubendiamide in cabbage and soil were based on the first-order reaction dynamic equations. The half-lives of the degradation of flubendiamide were 3.51 d to 3.96 d and 3.43 d to 3.87 d in the cabbage of Yangzhou and Jingzhou, respectively, and 4.42 d to 5.13 d and 4.37 d to 4.99 d in the soil of Yangzhou and Jingzhou, respectively. The terminal residues of flubendiamide in the cabbage of Yangzhou and Jingzhou were 0.0247 mg·kg-1 to 0.0393 mg·kg-1 and 0.0225 mg·kg-1 to 0.0273 mg·kg-1, respectively, when 20% flubendiamide WDG was applied at a dose of0.050g·m-2. Flubendiamide is safe to be applied in cabbage fields at the recommended dose.
文摘A new, rapid and efficient reverse phase Liquid Chromatography (RP-LC) method was developed for determination of Gibberellin A4 (GA4) in samples of flower stalk of Dasylirion cedrosanum and vegetative tissue of Epithelantha micromeris. Purification of GA4 was carried out by solid phase extraction (SPE), in Epithelantha micromeris. In the chromatography method was obtaining a retention time of 2.1 min, using Hypersil GOLD C-18 column (100 × 4.6 mm dim and size particle 5 μ), mobile phase 50/50 acetonitrile/water and a flow 1.0 ml/min. Detection was carried out by a UV detector set at 205 nm, and a quantization limit of 0.4 mg/L. The obtained correlation coefficient was 0.995.
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.
基金supported by the Key Project of Science and Technology Development Program of Shandong Province,China(2013KF03)
文摘A fast analytical method for the simultaneous determination of 9 mycotoxins, including alfatoxins （B1, B2, G1, and G2）, fumonisins （B1, B2 and B3）, zearalenone, and deoxynivalenol in corn using dispersive solid-phase extraction method and ultra-performance liquid chromatography coupled to tandem quadrupole time-of-lfight mass spectrometry （UPLC-Q-TOF-MS） was developed and validated. Samples were extracted with acetonitrile-water （84：16, v：v, containing 1% acetic acid） using ultrasonic extraction. The extracts were puriifed with a dispersive SPE method using C18 as a cleaning agent. The ifnal clear extracts were dried by nitrogen blowing and subsequently redissolved in methanol-water （5：5, v：v）. The samples were then analyzed by UPLC-Q-TOF-MS with 0.1% formic acid in ammonium acetate-methanol as mobile phase. The mean recoveries were ranged from 68.0 to 120.0%, and the relative standard deviation （RSD） ranged from 0.18 to 6.29%. Limits of detections ranged from 0.05 to 50 μg kg？1, and limits of quantiifcation ranged from 0.1 to 200 μg kg？1, which were below the legal limits set by the European Union for the legislated mycotoxins. The developed method was applied to 130 corn samples. Among the mycotoxins studied, alfatoxins B1 and fumonisins B1, B2 and B3 were the most predominant mycotoxins, and their concentrations were 0–593.12, 0–2.01×104, 0–6.94×103 and 0–3.05×103 μg kg–1, respectively.
文摘The extraction behavior of rare earths was studied by using paraffin with ceresin as a diluent containing 1-phenyl-3-methyl-4-benzoyl-pyrazolone-5.In solid phase,the composition of complexes is REP_3.The equilib- rium extraction constants and pH_(1/2) values of solid-liquid extraction are higher than those of normal liquid-liquid extraction.The extraction efficiency tends to maximum when the ratio of phases is 1:1.When the extraction temperature is higher than the melting point of paraffin and the extraction time is over 10 min,the extraction efficiency keeps constant.Moreover,the relationship among separation factor,equilibrium extrac- tion constant,pH_(1/2) value and atomic number was obtained.The mechanism of solid-liquid extraction is analogous to that of liquid-liquid extraction.
基金This work was financially supported by the Project of KJCXGC-01 of Northwest Normal University,and the Gansu Province Nature Science Foundation(ZR96016).]
文摘An overview of extraction of some trace metal ions using molten solvent (lowmelting substance) during last two decades is presented. The development of this technique since itsinception is briefly traced. The comparison of extraction efficiency, thermodynamics and kineticsmainly involving extraction of rare earth ions between molten solvent extraction at high temperatureand usual liquid-liquid extraction at room temperature are discussed in detail. The variousparameters obtained from the previous and present studies such as equilibrium extraction constantK_(ex), pH_(1/2), thermodynamic and kinetic data are displayed in tabular form. Finally, the currentdemands, disadvantages and future prospects are also evaluated.
文摘Silver nanoparticles were synthesized in reverse micelles consisting of sucrose fatty acid esters by dissolving reactant powder in the water pool of reverse micelles through the solid-liquid extraction. Silver nanoparticles having various sizes and shapes were obtained at high concentration. The size of silver nanoparticles was controlled by reaction temperature. Moreover, the size of silver nanoparticles was dependent upon the average esterification degree of sucrose fatty acid esters forming reverse micelles. The wavelength in the peaks, which corresponded upon the localized surface plasmon resonance of resultant silver nanoparticles, was correlated with their sizes.
