The demand for neodymium(NdFeB) permanent magnets for electric vehicles and eco-friendly generators is increasing.However,NdFeB magnets contain rare earth elements(REEs),which are limited in supply.In this study,we pe...The demand for neodymium(NdFeB) permanent magnets for electric vehicles and eco-friendly generators is increasing.However,NdFeB magnets contain rare earth elements(REEs),which are limited in supply.In this study,we performed an exchange reaction between magnesium halides(fluoride and chloride) and waste NdFeB scrap and then compared the characteristics of the extracted halides salts.The compositions of the ternary Mg fluoride(LiF:NaF:MgF_(2)=50:40:10 in mole ratio) and chloride(LiCl:NaCl:MgCl_(2)=10:50:40 in mole ratio) salts were thermodynamically determined for achieving low eutectic temperatures.The reactions between the NdFeB scrap powder(1-2 mm) and Mg halide salts were carried out at 1073 and 873 K for the fluoride and chloride systems,respectively,in an argon atmosphere.After the reaction,we separated Nd halide from the residual salt and evaluated the Ndextraction rate.The phase formation of the salt was analyzed using X-ray diffraction(XRD),and the extraction rate of Nd was analyzed using inductively coupled plasma optical emission spectroscopy(ICPOES).Nd was extracted in the form of Nd halide(NdF_(3) or NdCl_(3)),and the extraction rates in the fluoride and chloride systems are 98.64% and 84.59%,respectively.Thus,the fluoride system is more effective than the chloride system for Nd extraction.Our study provides a comprehensive comparative analysis of the effectiveness of fluo ride and chlo ride systems in extracting REEs from NdFeB magnet scrap.Our study findings can be used to develop an effective method for recycling magnet scraps.展开更多
In order to investigate the effect of magnetic field on the liquid-liquid extraction, the extraction in the acetone-water-trichloroethane system was studied under magnetic field with different magnetic induction inten...In order to investigate the effect of magnetic field on the liquid-liquid extraction, the extraction in the acetone-water-trichloroethane system was studied under magnetic field with different magnetic induction intensity.The results showed that the effect of magnetic field was positive in the extraction process, and the partition coeffi-cient and the yield of acetone increased-with the increasing magnetic induction intensity by 5.16%-8.35% and 1.85%-5.70% respectively. The effect of magnetic field on the extraction was intensified when the temperature became, higher. The experimental data of the partition coefficient of acetone were correlated by the method of least square in terms of a power-law correlation.展开更多
In this work, a metal-organic framework derived nanoporous carbon （MOF-5-C） was fabricated and modified with Fe3O4 magnetic nanoparticles. The resulting magnetic MOF-5-derived porous carbon （Fe304@MOF-5-C） was the...In this work, a metal-organic framework derived nanoporous carbon （MOF-5-C） was fabricated and modified with Fe3O4 magnetic nanoparticles. The resulting magnetic MOF-5-derived porous carbon （Fe304@MOF-5-C） was then used for the magnetic solid-phase extraction of chlorophenols （CPs） from mushroom samples prior to high performance liquid chromatography-ultraviolet detection. Scanning electron microscopy, transmission electron microscopy, X-ray diffraction, and N2 adsorption were used to characterize the adsorbent. After experimental optimization, the amount of the adsorbent was chosen as 8.0 mg, extraction time as 10 min, sample volume as 50 mL, desorption solvent as 0.4 mL （0.2 mL × 2） of alkaline methanol, and sample pH as 6. Under the above optimized conditions, good linearity for the analytes was obtained in the range of 0.8-100.0 ng g 1 with the correlation coefficients between 0.9923 and 0.9963. The limits of detection （SIN= 3） were in the range of 0.25-0.30 ng g-1, and the relative standard deviations were below 6.8%. The result showed that the Fe304@MOF-5-C has an excellent adsorption capacity for the analytes.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
In this paper, I introduce what are called weak gravity and magnetic anomalies and propose standards for estimating their reliability. I also introduce new techniques for processing this kind of weak anomaly. These te...In this paper, I introduce what are called weak gravity and magnetic anomalies and propose standards for estimating their reliability. I also introduce new techniques for processing this kind of weak anomaly. These techniques consist of interference elimination and weak signal extraction. Practical applications have proved their effectiveness, Weak gravity and magnetic anomalies will get more attention with the development of targeted exploration.展开更多
The analysis of endogenous glycoproteins and glycopeptides in human body fluids is of great importance for screening and discovering disease biomarkers with clinical significance.However,the presence of interfering su...The analysis of endogenous glycoproteins and glycopeptides in human body fluids is of great importance for screening and discovering disease biomarkers with clinical significance.However,the presence of interfering substances makes the direct quantitative detection of low-abundance glycoproteins and glycopeptides in human body fluids one of the great challenges in analytical chemistry.Magnetic solid phase extraction(MSPE)has the advantages of easy preparation,low cost and good magnetic responsiveness.Magnetic adsorbents are the core of MSPE technology,and magnetic adsorbents based on different functional materials are widely used in the quantitative analysis of glycoproteins and glycopeptides in human body fluids,making it possible to analyze glycoproteins and glycopeptides with low abundance as well as multiple types,which provides a technical platform for screening and evaluating glycoproteins and glycopeptides in body fluids as disease biomarkers.In this paper,we focus on the recent advances in the application of MSPE technology and magnetic adsorbents for the separation and enrichment of glycoproteins and glycopeptides in human body fluids,and the future trends and application prospects in this field are also presented.展开更多
The determination method of chlorogenic acid in traditional Chinese prescription Shuanghuanglian capsule was established by using quantitative nuclear magnetic resonance spectroscopy(q NMR) in combination with solid p...The determination method of chlorogenic acid in traditional Chinese prescription Shuanghuanglian capsule was established by using quantitative nuclear magnetic resonance spectroscopy(q NMR) in combination with solid phase extraction(SPE). As the capsule’s main active component, chlorogenic acid comes from the extraction of Chinese herb medicine Flos Lonicerae. The chlorogenic acid in capsule was ultrasonically extracted at room temperature using pure water as solvent. The extracting solution was enriched and cleaned using HC-C18 SPE cartridge. The effect of ultrasonic extraction, sample pretreatment conditions via SPE and q NMR experimental conditions were investigated. The q NMR experiment conditions were selected using deuterated DMSO as solvent, calibrated 1,4-phthalaldehyde as internal standard, and P1(pulse width) = 14.4 μs, d1(pulse delay time) = 1 s, NS(number of scan) = 512. The 1 H NMR peaks of δ 6.138–6.182(H-8’, d, 1 H) of chlorogenic acid was chosen as the quantitative peaks. Method validation was performed, including precision(the intra-day RSD = 1.2% and the inter-day RSD = 1.5%), linearity(correlation coefficient r>0.9999), LOD(0.0017 mg/g) and LOQ(0.079 mg/g). The recovery of the SPE-q NMR was within the range of 100.2%–103.2%. The result showed that the method was stable, accurate and reliabile. Determined by the method, the chlorogenic acid in a real Shuanghuanglian capsule was within the range of 9.68–10.35 mg/g.展开更多
Increasing use of silver in various fields has caused Ag^(+)pollution in water environment,taking great threats to people’s health.As a consequence,establishing rapid and reliable methods for sensitive determination ...Increasing use of silver in various fields has caused Ag^(+)pollution in water environment,taking great threats to people’s health.As a consequence,establishing rapid and reliable methods for sensitive determination of Ag^(+)is of great significance.Fluorescent(FL)sensors based on carbon dots(CDs),an excellent carbonaceous nanomaterial with strong and stable fluorescence,have absorbed extensive attentions in analysis of pollutants due to its advantages of carbon sources being readily available,low cost,easy operation and fast response.Moreover,ion-imprinting is a better way to increase the selectivity of the proposed method.Present work described an effective method for the sensitive measurement of silver ion in water samples in combination with magnetic ion-imprinted solid phase extraction and CDs based fluorescent sensor,which took full advantages of easy separation and high enrichment of magnetic solid phase extraction,high selectivity of ion-imprinting technology,and sensitivity and rapid response of fluorescent sensor from CDs.Sulfur-doped CDs derived from dithizone and magnetic ion-imprinted nanomaterial were prepared,and characterized with Fourier transform infrared spectroscopy and transmission electron microscope,etc.Magnetic Ag^(+)imprinted nanomaterial based solid phase extraction was employed for separating and enriching Ag^(+)from water samples.The significant parameters were optimized in detail.Under the optimal conditions,the proposed method provided good linearity in the range of 0.01-0.4μmol/L and low detection limit of 3 nmol/L.The reliability of the proposed method was validated with real water samples,and the results demonstrated that the proposed method was simple,robust,selective and sensitive detection tool for Ag^(+)in real water samples.展开更多
Enrichment of trace bioactive constituents and metabolites from complex biological samples is challenging.This study presented a one-pot synthesis of magnetic polydopamine nanoparticles(Fe3O4@-SiO2@PDA NPs)with multip...Enrichment of trace bioactive constituents and metabolites from complex biological samples is challenging.This study presented a one-pot synthesis of magnetic polydopamine nanoparticles(Fe3O4@-SiO2@PDA NPs)with multiple recognition sites for the magnetic dispersive solid-phase extraction(MDSPE)of ginsenosides from rat plasma treated with white ginseng.The extracted ginsenosides were characterized by combining an ultra-high-performance liquid chromatography coupled to a highresolution mass spectrometry with supplemental UNIFI libraries.Response surface methodology was statistically used to optimize the extraction procedure of the ginsenosides.The reusability of Fe3O4@-SiO2@PDA NPs was also examined and the results showed that the recovery rate exceeded 80%after recycling 6 times.Furthermore,the proposed method showed greater enrichment efficiency and could rapidly determine and characterize 23 ginsenoside prototypes and metabolites from plasma.In comparison,conventional methanol method can only detect 8 ginsenosides from the same plasma samples.The proposed approach can provide methodological reference for the trace determination and characterization of different bioactive ingredients and metabolites of traditional Chinese medicines and food.展开更多
A rapid and sensitive method for analyzing trace b-blockers in complex biological samples,which involved magnetic solid-phase extraction(MSPE)coupled with Fourier transform ion cyclotron resonance mass spectrometry(FT...A rapid and sensitive method for analyzing trace b-blockers in complex biological samples,which involved magnetic solid-phase extraction(MSPE)coupled with Fourier transform ion cyclotron resonance mass spectrometry(FTICR-MS),was developed.Novel nanosilver-functionalized magnetic nanoparticles with an interlayer of poly(3,4-dihydroxyphenylalanine)(polyDOPA@Ag-MNPs)were synthesized and used as MSPE adsorbents to extract trace b-blockers from biological samples.After extraction,the analytes loaded on the polyDOPA@Ag-MNPs were desorbed using an organic solvent and analyzed by FTICR-MS.The method was rapid and sensitive,with a total detection procedure of less than 10 min as well as limits of detection and quantification in the ranges of 3.5-6.8 pg/mL and 11.7-22.8 pg/mL,respectively.The accuracy of the method was also desirable,with recoveries ranging from 80.9%to 91.0%following the detection of analytes in human blood samples.All the experimental results demonstrated that the developed MSPE-FTICR-MS method was suitable for the rapid and sensitive analysis of trace b-blockers in complex biological samples.展开更多
This paper proposes a design and fine-tuning method for mixed electric and magnetic coupling filters.It derives the quantitative relationship between the coupling coefficients(electric and magnetic coupling,i.e.,EC an...This paper proposes a design and fine-tuning method for mixed electric and magnetic coupling filters.It derives the quantitative relationship between the coupling coefficients(electric and magnetic coupling,i.e.,EC and MC)and the linear coefficients of frequencydependent coupling for the first time.Different from the parameter extraction technique using the bandpass circuit model,the proposed approach explicitly relatesEC and MC to the coupling matrix model.This paper provides a general theoretic framework for computer-aided design and tuning of a mixed electric and magnetic coupling filter based on coupling matrices.An example of a 7th-order coaxial combline filter design is given in the paper,verifying the practical value of the approach.展开更多
As a typical bioflavonoid,diosmetin is desirable in the field of natural medicine,healthy food,and cosmetics by anti-cancer,antibacterial,antioxidant,estrogen-like and anti-inflammatory activities,and it comes from a ...As a typical bioflavonoid,diosmetin is desirable in the field of natural medicine,healthy food,and cosmetics by anti-cancer,antibacterial,antioxidant,estrogen-like and anti-inflammatory activities,and it comes from a wide range of sources in traditional Chinese medicine like spider fragrance,spearmint and chrysanthemum,as well as in Citrus fruit.However,traditional analytical methods such as silica gel column chromatography face multiple challenges in the selective extraction of diosmetin from biological materials and traditional Chinese medicinal materials.Therefore,it is urgent to develop a new type of absorbent with high efficiency,recyclability and good specificity to diosmetin.In this investigation,a magnetic surface molecularly imprinted polymer(labeled as Diosmetin/SMIPs)was synthesized employing magnetic nanoparticles as the carrier and 4-vinylpyridinyl(4-VP)as the functional monomer by surface imprinting technology.The functional monomer was screened by the binding energy(△E)between functional monomers and template molecules via computational simulation.The Diosmetin/SMIPs had a high level of specific recognition and adsorption capability towards diosmetin with a 20.25 mg g^(-1) adsorption capacity and an imprinting factor(IF)of 2.28.Additionally,it demonstrated excellent regeneration performance with 8 adsorption/desorption cycles.In addition,91.20%-94.16% of spiked diosmetin was recovered from the lemon peel samples.The strategy of constructing Diosmetin/SMIPs based on computational simulation can effectively enhance the specific adsorption performance of diosmetin.Meanwhile,Diosmetin/SMIPs synthesized by imprinting polymerization showed excellent anti-interference and reusability,and realized efficient targeted extraction of diosmetin from lemon peel samples.The results of this investigation provide a promising adsorbent for selective enrichment of diosmetin from Citrus fruit and complicated materials.展开更多
Organophosphorus pesticides(OPPs)in foods pose a serious threat to human health,motivating the development of novel analytical methods for their rapid detection and quantification.A magnetic covalent organic framework...Organophosphorus pesticides(OPPs)in foods pose a serious threat to human health,motivating the development of novel analytical methods for their rapid detection and quantification.A magnetic covalent organic framework(M-COF)adsorbent for the magnetic solid-phase extraction(MSPE)of OPPs from foods was reported.M-COF was synthesized by the Schiff base condensation reaction of 1,3,5-tris(4-aminophenyl)benzene and 4,4-biphenyldicarboxaldehyde on the surface of amino-functionalized magnetic nanoparticles.Density functional theory(DFT)calculations showed that adsorption of OPPs onto the surface of M-COF involved hydrophobic effects,van der Waals interactions,π-πinteractions,halogen-N bonding,and hydrogen bonding.Combined with gas chromatography-mass spectrometry(GC-MS)technology,the MSPE method features low limits of detection for OPPs(0.002-0.015μg/L),good reproducibility(1.45%-6.14%),wide linear detection range(0.01-1μg/L,R≥0.9935),and satisfactory recoveries(87.3%-110.4%).The method was successfully applied for the trace analysis of OPPs in spiked fruit juices.展开更多
Microporous organic networks(MONs)are attractive adsorbents for use in sample pretreatment owning to their unique structure and properties.However,methods for constructing functional MONs are still limited because the...Microporous organic networks(MONs)are attractive adsorbents for use in sample pretreatment owning to their unique structure and properties.However,methods for constructing functional MONs are still limited because the lack of monomers via direct synthesis and their complex procedures via postmodification.To address this issue,a facile one-pot in situ doping strategy was proposed herein for synthesis a novel phenylboronic acid-functionalized magnetic cyclodextrin-based microporous organic network([PBA]_(3/4)-MCD-MON-0.04).[PBA]_(3/4)MCD-MON-0.04 was used for the selective and efficient extraction of sulfonylurea herbicides(SUHs)from complex food and environmental water samples via the synergistic hydrogen bonding,host-vip,hydrophobic andπ-πinteractions and the specific B-N coordination.[PBA]_(3/4)-MCD-MON-0.04 had a large surface area,high saturation magnetism,good reusability,and remarkable stability.A rapid,sensitive,and selective method was proposed for monitoring SUHs from diverse matrices.This study provides a new strategy for synthesizing novel and multifunctional magnetic CD-MONs-based adsorbents and reveals the considerable potential of CD-MONs in sample pretreatment.展开更多
Solid phase extraction （SPE） is a widely used sample pretreatment method for separation, purification and enrichment, which has been established due to its significant advantages of time-saving, low consumption of s...Solid phase extraction （SPE） is a widely used sample pretreatment method for separation, purification and enrichment, which has been established due to its significant advantages of time-saving, low consumption of solvent, high enrichment factor, high accuracy, etc. In recent years, a variety of new SPE methods such as molecularly imprinted solid phase extraction （MISPE）, magnetic solid phase extraction （MSPE）, solid phase micro-extraction （SPME）, etc., which are superior to the conventional SPE, have been developed and been widely applied to food, drugs, and environmental monitoring. In this paper, the basic principles and methods of SPE and its new applications in different areas are reviewed.展开更多
The aim of this study is a present of a simple solvothermal synthesis approach to preparation of Cu-based magnetic metal organic framework(MMOF)and subsequently its application as sorbent for ultrasound assisted magne...The aim of this study is a present of a simple solvothermal synthesis approach to preparation of Cu-based magnetic metal organic framework(MMOF)and subsequently its application as sorbent for ultrasound assisted magnetic solid phase extraction(UAMSPE)of ampicillin(AMP)from cow milk samples prior to high performance liquid chromatography-Ultraviolet(HPLC-UV)determination.Characteristics of prepared MMOF were fully investigated by different techniques which showed the exclusive properties of proposed sorbent in terms of proper functionality,desirable magnetic property and also high specific surface area.Different influential factors on extraction recovery including sorbent dosage,ultrasonic time,washing solvent volume and eluent solvent volume were assessed using central composite design(CCD)based response surface methodology(RSM)as an operative and powerful optimization tool.This is the first report for determination of AMP using MMOF.The proposed method addressed some drawbacks of other methods and sorbents for determination of AMP.The presented method decreases the extraction time(4 min)and also enhances adsorption capacity(250 mg/g).Moreover,the magnetic property of presented sorbent(15 emu/g)accelerates the extraction process which does not need filtration,centrifuge and precipitation procedures.Under the optimized conditions,the proposed method is applicable for linear range of 1.0-5000.0 μg/L with detection limit of 0.29 μg/L,satisfactory recoveries(≥95.0%)and acceptable repeatability(RSD less than 4.0%).The present study indicates highly promising perspectives of MMOF for highly effective analysis of AMP in complicated matrices.展开更多
Coals consist of some molecules trapped within an organic matrix from which some organic compounds can be extracted by solvents. The Soxhlet technique has been widely used for extracting organic compounds. Microwave h...Coals consist of some molecules trapped within an organic matrix from which some organic compounds can be extracted by solvents. The Soxhlet technique has been widely used for extracting organic compounds. Microwave heating methods may be successfully applied in the field of coal science. Acetone extraction yields and the chemical composition of the extract were investigated using a typical Chinese coal, Shenfu coal, with microwave-assisted extraction. The acetone extract and residue were analyzed by GC/MS and carbon-13 nuclear magnetic resonance spectroscopy respectively. The carbon spectra were converted into several numerical parameters, fa, Ha, Xb, which indicate the difference in macromolecular structure between Shenfu coal and its residue. Furthermore, a hybrid genetic algorithm was employed using these parameters to approximate a coal macromolecule by assembling the structural fragments or functional groups into a large and complicated structure.展开更多
Tension-compression fatigue test was performed on 0.45% C steel specimens.Normal and tangential components of magnetic memory testing signals,Hp(y) and Hp(x) signals,with their characteristics,K of Hp(y) and Hp(x)M of...Tension-compression fatigue test was performed on 0.45% C steel specimens.Normal and tangential components of magnetic memory testing signals,Hp(y) and Hp(x) signals,with their characteristics,K of Hp(y) and Hp(x)M of Hp(x),throughout the fatigue process were presented and analyzed.Abnormal peaks of Hp(y) and peak of Hp(x) reversed after loading; Hp(y) curves rotated clockwise and Hp(x) curves elevated significantly with the increase of fatigue cycle number at the first a few fatigue cycles,both Hp(y) and Hp(x) curves were stable after that,the amplitude of abnormal peaks of Hp(y) and peak value of Hp(x) increased more quickly after fatigue crack initiation.Abnormal peaks of Hp(y) and peak of Hp(x) at the notch reversed again after failure.The characteristics were found to exhibit consistent tendency in the whole fatigue life and behave differently in different stages of fatigue.In initial and crack developing stages,the characteristics increased significantly due to dislocations increase and crack propagation,respectively.In stable stage,the characteristics remained constant as a result of dislocation blocking,K value ranged from 20 to 30 A/(m·mm)-1,and Hp(x)M ranged from 270 to 300 A/m under the test parameters in this work.After failure,both abnormal peaks of Hp(y) and peak of Hp(x) reversed,K value was 133 A/(m·mm)-1 and Hp(x)M was-640 A/m.The results indicate that the characteristics of Hp(y) and Hp(x) signals were related to the accumulation of fatigue,so it is feasible and applicable to monitor fatigue damage of ferromagnetic components using metal magnetic memory testing(MMMT).展开更多
Novel uniform-sized magnetic molecularly imprinted polymers （MMIPs） were synthe- sized for selective recognition of active antitumor ingredients of kaempferol （KMF） and protoapi- genone （PA） in Macrothelypteris ...Novel uniform-sized magnetic molecularly imprinted polymers （MMIPs） were synthe- sized for selective recognition of active antitumor ingredients of kaempferol （KMF） and protoapi- genone （PA） in Macrothelypteris torresiana （M. torresiana） by surface molecular imprinting tech- nique in this study. Super paramagnetic core-sheU nanoparticles （γ-MPS-SiO2@Fe3O4） were used as seeds, KMF as template molecule, acrylamide （AM） as functional monomer, and N, N＇-methylene bisacrylamide （BisAM） as cross-linker. The prepared MMIPs were characterized by X-ray diffraction （XRD）, Fourier transform infrared spectrum fiT/R）, transmission electron microscopy （TEM） and thermo-gravimetric analysis （TGA）, respectively. The recognition capacity of MMIPs was 2.436 times of non-imprinted polymers. The adsorption results based on kinetics and isotherm analysis were in accordance with the pseudo-second-order model （R2=0.9980） and the Langmuir adsorption model （R2=0.9944）. The value of E （6.742 kJ/mol） calculated from the Dubinin-Radushkevich isotherm model suggested that the physical adsorption via hydrogen-bonding might be predominant. The Scatchard plot showed a single line （R2=0.9172） and demonstrated the homogeneous recognition sites on MMIPs for KMF. The magnetic solid phase extraction （MSPE） based on MMIPs as sorbent was established for fast and selective enrichment of KMF and its structural analogue PA from the crude extract of M. torresiana and then KMF and PA were detected by HPLC-UV. The established method showed good performance and satisfactory results for real sample analysis. It also showed the feasi- bility of MMIPs for selective recognition of active structural analogues from complex herbal extracts.展开更多
基金supported by the Technology Innovation (20010817,Technology for the ecofriendly rare earth refining from used motors and manufacture of permanent magnet materials) funded by the Ministry of Trade,Industry & Energy (MOTIE),Korea。
文摘The demand for neodymium(NdFeB) permanent magnets for electric vehicles and eco-friendly generators is increasing.However,NdFeB magnets contain rare earth elements(REEs),which are limited in supply.In this study,we performed an exchange reaction between magnesium halides(fluoride and chloride) and waste NdFeB scrap and then compared the characteristics of the extracted halides salts.The compositions of the ternary Mg fluoride(LiF:NaF:MgF_(2)=50:40:10 in mole ratio) and chloride(LiCl:NaCl:MgCl_(2)=10:50:40 in mole ratio) salts were thermodynamically determined for achieving low eutectic temperatures.The reactions between the NdFeB scrap powder(1-2 mm) and Mg halide salts were carried out at 1073 and 873 K for the fluoride and chloride systems,respectively,in an argon atmosphere.After the reaction,we separated Nd halide from the residual salt and evaluated the Ndextraction rate.The phase formation of the salt was analyzed using X-ray diffraction(XRD),and the extraction rate of Nd was analyzed using inductively coupled plasma optical emission spectroscopy(ICPOES).Nd was extracted in the form of Nd halide(NdF_(3) or NdCl_(3)),and the extraction rates in the fluoride and chloride systems are 98.64% and 84.59%,respectively.Thus,the fluoride system is more effective than the chloride system for Nd extraction.Our study provides a comprehensive comparative analysis of the effectiveness of fluo ride and chlo ride systems in extracting REEs from NdFeB magnet scrap.Our study findings can be used to develop an effective method for recycling magnet scraps.
基金Supported by the Program on Technological Development Plan of Tianjin (No.033180611).
文摘In order to investigate the effect of magnetic field on the liquid-liquid extraction, the extraction in the acetone-water-trichloroethane system was studied under magnetic field with different magnetic induction intensity.The results showed that the effect of magnetic field was positive in the extraction process, and the partition coeffi-cient and the yield of acetone increased-with the increasing magnetic induction intensity by 5.16%-8.35% and 1.85%-5.70% respectively. The effect of magnetic field on the extraction was intensified when the temperature became, higher. The experimental data of the partition coefficient of acetone were correlated by the method of least square in terms of a power-law correlation.
基金Financial support from the National Natural Science Foundation of China (Nos. 31471643, 31571925)the Innovation Research Program of the Department of Education of Hebei for Hebei Provincial Universities (No. LJRC009)
文摘In this work, a metal-organic framework derived nanoporous carbon （MOF-5-C） was fabricated and modified with Fe3O4 magnetic nanoparticles. The resulting magnetic MOF-5-derived porous carbon （Fe304@MOF-5-C） was then used for the magnetic solid-phase extraction of chlorophenols （CPs） from mushroom samples prior to high performance liquid chromatography-ultraviolet detection. Scanning electron microscopy, transmission electron microscopy, X-ray diffraction, and N2 adsorption were used to characterize the adsorbent. After experimental optimization, the amount of the adsorbent was chosen as 8.0 mg, extraction time as 10 min, sample volume as 50 mL, desorption solvent as 0.4 mL （0.2 mL × 2） of alkaline methanol, and sample pH as 6. Under the above optimized conditions, good linearity for the analytes was obtained in the range of 0.8-100.0 ng g 1 with the correlation coefficients between 0.9923 and 0.9963. The limits of detection （SIN= 3） were in the range of 0.25-0.30 ng g-1, and the relative standard deviations were below 6.8%. The result showed that the Fe304@MOF-5-C has an excellent adsorption capacity for the analytes.
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 subject is sponsored by the National 863Project Fund (Project No.2006AA06Z201)
文摘In this paper, I introduce what are called weak gravity and magnetic anomalies and propose standards for estimating their reliability. I also introduce new techniques for processing this kind of weak anomaly. These techniques consist of interference elimination and weak signal extraction. Practical applications have proved their effectiveness, Weak gravity and magnetic anomalies will get more attention with the development of targeted exploration.
基金supported by the Natural Science Foundation of Jilin Provincial Science&Technology Department(No.20190201079JC)。
文摘The analysis of endogenous glycoproteins and glycopeptides in human body fluids is of great importance for screening and discovering disease biomarkers with clinical significance.However,the presence of interfering substances makes the direct quantitative detection of low-abundance glycoproteins and glycopeptides in human body fluids one of the great challenges in analytical chemistry.Magnetic solid phase extraction(MSPE)has the advantages of easy preparation,low cost and good magnetic responsiveness.Magnetic adsorbents are the core of MSPE technology,and magnetic adsorbents based on different functional materials are widely used in the quantitative analysis of glycoproteins and glycopeptides in human body fluids,making it possible to analyze glycoproteins and glycopeptides with low abundance as well as multiple types,which provides a technical platform for screening and evaluating glycoproteins and glycopeptides in body fluids as disease biomarkers.In this paper,we focus on the recent advances in the application of MSPE technology and magnetic adsorbents for the separation and enrichment of glycoproteins and glycopeptides in human body fluids,and the future trends and application prospects in this field are also presented.
基金National Natural Science Foundation of China(Grant No.31671928)Natural Science Foundation of Shanghai(Grant No.15ZR1440800).
文摘The determination method of chlorogenic acid in traditional Chinese prescription Shuanghuanglian capsule was established by using quantitative nuclear magnetic resonance spectroscopy(q NMR) in combination with solid phase extraction(SPE). As the capsule’s main active component, chlorogenic acid comes from the extraction of Chinese herb medicine Flos Lonicerae. The chlorogenic acid in capsule was ultrasonically extracted at room temperature using pure water as solvent. The extracting solution was enriched and cleaned using HC-C18 SPE cartridge. The effect of ultrasonic extraction, sample pretreatment conditions via SPE and q NMR experimental conditions were investigated. The q NMR experiment conditions were selected using deuterated DMSO as solvent, calibrated 1,4-phthalaldehyde as internal standard, and P1(pulse width) = 14.4 μs, d1(pulse delay time) = 1 s, NS(number of scan) = 512. The 1 H NMR peaks of δ 6.138–6.182(H-8’, d, 1 H) of chlorogenic acid was chosen as the quantitative peaks. Method validation was performed, including precision(the intra-day RSD = 1.2% and the inter-day RSD = 1.5%), linearity(correlation coefficient r>0.9999), LOD(0.0017 mg/g) and LOQ(0.079 mg/g). The recovery of the SPE-q NMR was within the range of 100.2%–103.2%. The result showed that the method was stable, accurate and reliabile. Determined by the method, the chlorogenic acid in a real Shuanghuanglian capsule was within the range of 9.68–10.35 mg/g.
基金supported by the National Natural Science Foundation of China(No.21976211).
文摘Increasing use of silver in various fields has caused Ag^(+)pollution in water environment,taking great threats to people’s health.As a consequence,establishing rapid and reliable methods for sensitive determination of Ag^(+)is of great significance.Fluorescent(FL)sensors based on carbon dots(CDs),an excellent carbonaceous nanomaterial with strong and stable fluorescence,have absorbed extensive attentions in analysis of pollutants due to its advantages of carbon sources being readily available,low cost,easy operation and fast response.Moreover,ion-imprinting is a better way to increase the selectivity of the proposed method.Present work described an effective method for the sensitive measurement of silver ion in water samples in combination with magnetic ion-imprinted solid phase extraction and CDs based fluorescent sensor,which took full advantages of easy separation and high enrichment of magnetic solid phase extraction,high selectivity of ion-imprinting technology,and sensitivity and rapid response of fluorescent sensor from CDs.Sulfur-doped CDs derived from dithizone and magnetic ion-imprinted nanomaterial were prepared,and characterized with Fourier transform infrared spectroscopy and transmission electron microscope,etc.Magnetic Ag^(+)imprinted nanomaterial based solid phase extraction was employed for separating and enriching Ag^(+)from water samples.The significant parameters were optimized in detail.Under the optimal conditions,the proposed method provided good linearity in the range of 0.01-0.4μmol/L and low detection limit of 3 nmol/L.The reliability of the proposed method was validated with real water samples,and the results demonstrated that the proposed method was simple,robust,selective and sensitive detection tool for Ag^(+)in real water samples.
基金This work was supported by grants from the National Natural Science Foundation of China Key Program(NO.81530094)General Program(NO.81573574,81873193)the Science and Technology Development Project of Jilin Province(20190201283JC).
文摘Enrichment of trace bioactive constituents and metabolites from complex biological samples is challenging.This study presented a one-pot synthesis of magnetic polydopamine nanoparticles(Fe3O4@-SiO2@PDA NPs)with multiple recognition sites for the magnetic dispersive solid-phase extraction(MDSPE)of ginsenosides from rat plasma treated with white ginseng.The extracted ginsenosides were characterized by combining an ultra-high-performance liquid chromatography coupled to a highresolution mass spectrometry with supplemental UNIFI libraries.Response surface methodology was statistically used to optimize the extraction procedure of the ginsenosides.The reusability of Fe3O4@-SiO2@PDA NPs was also examined and the results showed that the recovery rate exceeded 80%after recycling 6 times.Furthermore,the proposed method showed greater enrichment efficiency and could rapidly determine and characterize 23 ginsenoside prototypes and metabolites from plasma.In comparison,conventional methanol method can only detect 8 ginsenosides from the same plasma samples.The proposed approach can provide methodological reference for the trace determination and characterization of different bioactive ingredients and metabolites of traditional Chinese medicines and food.
基金supported by the National Natural Science Foundation of China(Grant Nos.:21976168,22127810,and 22004113)Key Research and Development Program of Guangdong Province(Grant No.:2020B1111350002)+1 种基金Guangdong Basic and Applied Basic Research Foundation(Grant No.:2019A1515110420)GDAS0 Project of Science and Technology Development(Grant No.:2021GDASYL-20210103034).
文摘A rapid and sensitive method for analyzing trace b-blockers in complex biological samples,which involved magnetic solid-phase extraction(MSPE)coupled with Fourier transform ion cyclotron resonance mass spectrometry(FTICR-MS),was developed.Novel nanosilver-functionalized magnetic nanoparticles with an interlayer of poly(3,4-dihydroxyphenylalanine)(polyDOPA@Ag-MNPs)were synthesized and used as MSPE adsorbents to extract trace b-blockers from biological samples.After extraction,the analytes loaded on the polyDOPA@Ag-MNPs were desorbed using an organic solvent and analyzed by FTICR-MS.The method was rapid and sensitive,with a total detection procedure of less than 10 min as well as limits of detection and quantification in the ranges of 3.5-6.8 pg/mL and 11.7-22.8 pg/mL,respectively.The accuracy of the method was also desirable,with recoveries ranging from 80.9%to 91.0%following the detection of analytes in human blood samples.All the experimental results demonstrated that the developed MSPE-FTICR-MS method was suitable for the rapid and sensitive analysis of trace b-blockers in complex biological samples.
基金supported by the National Natural Science Foundation of China under Grant No.62001339.
文摘This paper proposes a design and fine-tuning method for mixed electric and magnetic coupling filters.It derives the quantitative relationship between the coupling coefficients(electric and magnetic coupling,i.e.,EC and MC)and the linear coefficients of frequencydependent coupling for the first time.Different from the parameter extraction technique using the bandpass circuit model,the proposed approach explicitly relatesEC and MC to the coupling matrix model.This paper provides a general theoretic framework for computer-aided design and tuning of a mixed electric and magnetic coupling filter based on coupling matrices.An example of a 7th-order coaxial combline filter design is given in the paper,verifying the practical value of the approach.
基金supported by the National Natural Science Foundation of China(Nos.32301259,32101228,32271527 and 32371536)the“Pioneer”and“Leading Goose”R&D Program of Zhejiang(Nos.2022C02023 and 2023C02015)+1 种基金the Research Foundation of Talented Scholars of Zhejiang A&F University(No.2021LFR058)the Dean-ship of Scientific Research at Northern Border University,Arar,KSA for funding this research work through the project number“NBU-FPEJ-2024-177-01”.
文摘As a typical bioflavonoid,diosmetin is desirable in the field of natural medicine,healthy food,and cosmetics by anti-cancer,antibacterial,antioxidant,estrogen-like and anti-inflammatory activities,and it comes from a wide range of sources in traditional Chinese medicine like spider fragrance,spearmint and chrysanthemum,as well as in Citrus fruit.However,traditional analytical methods such as silica gel column chromatography face multiple challenges in the selective extraction of diosmetin from biological materials and traditional Chinese medicinal materials.Therefore,it is urgent to develop a new type of absorbent with high efficiency,recyclability and good specificity to diosmetin.In this investigation,a magnetic surface molecularly imprinted polymer(labeled as Diosmetin/SMIPs)was synthesized employing magnetic nanoparticles as the carrier and 4-vinylpyridinyl(4-VP)as the functional monomer by surface imprinting technology.The functional monomer was screened by the binding energy(△E)between functional monomers and template molecules via computational simulation.The Diosmetin/SMIPs had a high level of specific recognition and adsorption capability towards diosmetin with a 20.25 mg g^(-1) adsorption capacity and an imprinting factor(IF)of 2.28.Additionally,it demonstrated excellent regeneration performance with 8 adsorption/desorption cycles.In addition,91.20%-94.16% of spiked diosmetin was recovered from the lemon peel samples.The strategy of constructing Diosmetin/SMIPs based on computational simulation can effectively enhance the specific adsorption performance of diosmetin.Meanwhile,Diosmetin/SMIPs synthesized by imprinting polymerization showed excellent anti-interference and reusability,and realized efficient targeted extraction of diosmetin from lemon peel samples.The results of this investigation provide a promising adsorbent for selective enrichment of diosmetin from Citrus fruit and complicated materials.
基金supported by Key Research and Development Project of Shandong Province(2021ZDSYS12)National Natural Science Foundation of China(22076086,21777089)+3 种基金Taishan Scholar Program of Shandong Province(ts20190948)Shandong Province Science and Technology Small and Medium Enterprises Innovation Ability Enhancement Project(2023TSGC0689,2023TSGC0055)Natural Science Foundation of Shandong Province(ZR2021MB086,ZR2023QB035)Jinan City University and Institute Innovation Team Project(2021GXRC061,20228045,202333027)。
文摘Organophosphorus pesticides(OPPs)in foods pose a serious threat to human health,motivating the development of novel analytical methods for their rapid detection and quantification.A magnetic covalent organic framework(M-COF)adsorbent for the magnetic solid-phase extraction(MSPE)of OPPs from foods was reported.M-COF was synthesized by the Schiff base condensation reaction of 1,3,5-tris(4-aminophenyl)benzene and 4,4-biphenyldicarboxaldehyde on the surface of amino-functionalized magnetic nanoparticles.Density functional theory(DFT)calculations showed that adsorption of OPPs onto the surface of M-COF involved hydrophobic effects,van der Waals interactions,π-πinteractions,halogen-N bonding,and hydrogen bonding.Combined with gas chromatography-mass spectrometry(GC-MS)technology,the MSPE method features low limits of detection for OPPs(0.002-0.015μg/L),good reproducibility(1.45%-6.14%),wide linear detection range(0.01-1μg/L,R≥0.9935),and satisfactory recoveries(87.3%-110.4%).The method was successfully applied for the trace analysis of OPPs in spiked fruit juices.
基金supported by the National Natural Science Foundation of China(Nos.22174071 and 22206114)the Natural Science Foundation of Shandong Province(Nos.ZR2022YQ08 and ZR2022QB085)+2 种基金the Innovation Team of Shandong Higher School Youth Innovation Technology Program(No.2023KJ344)the Academic Promotion Program(No.2019LJ003)Joint Innovation Team for Clinical&Basic Research(No.202401)of Shandong First Medical University。
文摘Microporous organic networks(MONs)are attractive adsorbents for use in sample pretreatment owning to their unique structure and properties.However,methods for constructing functional MONs are still limited because the lack of monomers via direct synthesis and their complex procedures via postmodification.To address this issue,a facile one-pot in situ doping strategy was proposed herein for synthesis a novel phenylboronic acid-functionalized magnetic cyclodextrin-based microporous organic network([PBA]_(3/4)-MCD-MON-0.04).[PBA]_(3/4)MCD-MON-0.04 was used for the selective and efficient extraction of sulfonylurea herbicides(SUHs)from complex food and environmental water samples via the synergistic hydrogen bonding,host-vip,hydrophobic andπ-πinteractions and the specific B-N coordination.[PBA]_(3/4)-MCD-MON-0.04 had a large surface area,high saturation magnetism,good reusability,and remarkable stability.A rapid,sensitive,and selective method was proposed for monitoring SUHs from diverse matrices.This study provides a new strategy for synthesizing novel and multifunctional magnetic CD-MONs-based adsorbents and reveals the considerable potential of CD-MONs in sample pretreatment.
基金supported by the Key Laboratory for Rare Disease of Shandong Province
文摘Solid phase extraction （SPE） is a widely used sample pretreatment method for separation, purification and enrichment, which has been established due to its significant advantages of time-saving, low consumption of solvent, high enrichment factor, high accuracy, etc. In recent years, a variety of new SPE methods such as molecularly imprinted solid phase extraction （MISPE）, magnetic solid phase extraction （MSPE）, solid phase micro-extraction （SPME）, etc., which are superior to the conventional SPE, have been developed and been widely applied to food, drugs, and environmental monitoring. In this paper, the basic principles and methods of SPE and its new applications in different areas are reviewed.
基金This work was financially supported by Graduate School and Research Council of Yasouj University.
文摘The aim of this study is a present of a simple solvothermal synthesis approach to preparation of Cu-based magnetic metal organic framework(MMOF)and subsequently its application as sorbent for ultrasound assisted magnetic solid phase extraction(UAMSPE)of ampicillin(AMP)from cow milk samples prior to high performance liquid chromatography-Ultraviolet(HPLC-UV)determination.Characteristics of prepared MMOF were fully investigated by different techniques which showed the exclusive properties of proposed sorbent in terms of proper functionality,desirable magnetic property and also high specific surface area.Different influential factors on extraction recovery including sorbent dosage,ultrasonic time,washing solvent volume and eluent solvent volume were assessed using central composite design(CCD)based response surface methodology(RSM)as an operative and powerful optimization tool.This is the first report for determination of AMP using MMOF.The proposed method addressed some drawbacks of other methods and sorbents for determination of AMP.The presented method decreases the extraction time(4 min)and also enhances adsorption capacity(250 mg/g).Moreover,the magnetic property of presented sorbent(15 emu/g)accelerates the extraction process which does not need filtration,centrifuge and precipitation procedures.Under the optimized conditions,the proposed method is applicable for linear range of 1.0-5000.0 μg/L with detection limit of 0.29 μg/L,satisfactory recoveries(≥95.0%)and acceptable repeatability(RSD less than 4.0%).The present study indicates highly promising perspectives of MMOF for highly effective analysis of AMP in complicated matrices.
基金Project 40472082 supported by the National Natural Science Foundation of China
文摘Coals consist of some molecules trapped within an organic matrix from which some organic compounds can be extracted by solvents. The Soxhlet technique has been widely used for extracting organic compounds. Microwave heating methods may be successfully applied in the field of coal science. Acetone extraction yields and the chemical composition of the extract were investigated using a typical Chinese coal, Shenfu coal, with microwave-assisted extraction. The acetone extract and residue were analyzed by GC/MS and carbon-13 nuclear magnetic resonance spectroscopy respectively. The carbon spectra were converted into several numerical parameters, fa, Ha, Xb, which indicate the difference in macromolecular structure between Shenfu coal and its residue. Furthermore, a hybrid genetic algorithm was employed using these parameters to approximate a coal macromolecule by assembling the structural fragments or functional groups into a large and complicated structure.
基金Projects(50975283,50975287)supported by the National Natural Science Foundation of ChinaProject(2011CB013401)supported by the National Basic Research Program,China
文摘Tension-compression fatigue test was performed on 0.45% C steel specimens.Normal and tangential components of magnetic memory testing signals,Hp(y) and Hp(x) signals,with their characteristics,K of Hp(y) and Hp(x)M of Hp(x),throughout the fatigue process were presented and analyzed.Abnormal peaks of Hp(y) and peak of Hp(x) reversed after loading; Hp(y) curves rotated clockwise and Hp(x) curves elevated significantly with the increase of fatigue cycle number at the first a few fatigue cycles,both Hp(y) and Hp(x) curves were stable after that,the amplitude of abnormal peaks of Hp(y) and peak value of Hp(x) increased more quickly after fatigue crack initiation.Abnormal peaks of Hp(y) and peak of Hp(x) at the notch reversed again after failure.The characteristics were found to exhibit consistent tendency in the whole fatigue life and behave differently in different stages of fatigue.In initial and crack developing stages,the characteristics increased significantly due to dislocations increase and crack propagation,respectively.In stable stage,the characteristics remained constant as a result of dislocation blocking,K value ranged from 20 to 30 A/(m·mm)-1,and Hp(x)M ranged from 270 to 300 A/m under the test parameters in this work.After failure,both abnormal peaks of Hp(y) and peak of Hp(x) reversed,K value was 133 A/(m·mm)-1 and Hp(x)M was-640 A/m.The results indicate that the characteristics of Hp(y) and Hp(x) signals were related to the accumulation of fatigue,so it is feasible and applicable to monitor fatigue damage of ferromagnetic components using metal magnetic memory testing(MMMT).
基金supported by grants from the National Natural Science Foundation of China(No.21105032)Doctoral Program Fund of Ministry of Education of China(No.20110142120031)
文摘Novel uniform-sized magnetic molecularly imprinted polymers （MMIPs） were synthe- sized for selective recognition of active antitumor ingredients of kaempferol （KMF） and protoapi- genone （PA） in Macrothelypteris torresiana （M. torresiana） by surface molecular imprinting tech- nique in this study. Super paramagnetic core-sheU nanoparticles （γ-MPS-SiO2@Fe3O4） were used as seeds, KMF as template molecule, acrylamide （AM） as functional monomer, and N, N＇-methylene bisacrylamide （BisAM） as cross-linker. The prepared MMIPs were characterized by X-ray diffraction （XRD）, Fourier transform infrared spectrum fiT/R）, transmission electron microscopy （TEM） and thermo-gravimetric analysis （TGA）, respectively. The recognition capacity of MMIPs was 2.436 times of non-imprinted polymers. The adsorption results based on kinetics and isotherm analysis were in accordance with the pseudo-second-order model （R2=0.9980） and the Langmuir adsorption model （R2=0.9944）. The value of E （6.742 kJ/mol） calculated from the Dubinin-Radushkevich isotherm model suggested that the physical adsorption via hydrogen-bonding might be predominant. The Scatchard plot showed a single line （R2=0.9172） and demonstrated the homogeneous recognition sites on MMIPs for KMF. The magnetic solid phase extraction （MSPE） based on MMIPs as sorbent was established for fast and selective enrichment of KMF and its structural analogue PA from the crude extract of M. torresiana and then KMF and PA were detected by HPLC-UV. The established method showed good performance and satisfactory results for real sample analysis. It also showed the feasi- bility of MMIPs for selective recognition of active structural analogues from complex herbal extracts.
