Solid phase extraction is widely used in sample pretreatment,concentration and analysis processes due to high selectivity and suitability for low concentration sample system.In this review,we systematically summarized...Solid phase extraction is widely used in sample pretreatment,concentration and analysis processes due to high selectivity and suitability for low concentration sample system.In this review,we systematically summarized and discussed the development trends of solid phase extraction by bibliometrics method.By analyzing papers output scale,the research and development direction of solid phase extraction technology is prospected.We also give an overview on current strategies of novel solid phase extraction from the separation medium and separation technology.The paper aims to describe the global research profile and the development trends of solid phase extraction,to help researchers to accurately grasp the research trend and to provide support for scientific research institutions to formulate scientific policies and strategic plans.Furthermore,the prospect of the development and application of solid phase extraction is also discussed.展开更多
A sensitive flow injection chemiluminescence method has been developed for the detection of resveratrol in red wine based on the fact that resveratrol can greatly enhance chemiluminescence reaction between KMnO4 and H...A sensitive flow injection chemiluminescence method has been developed for the detection of resveratrol in red wine based on the fact that resveratrol can greatly enhance chemiluminescence reaction between KMnO4 and HCHO in sulfuric acid medium. Analytes were pre-concentrated on solid sorbents (C18 solid-phase extraction cartridges). Under the optimum conditions, the proposed method allows the measurement of resveratrol over the range of 1.32 × 10^-8 to 1.32 × 10^-5 mol/L with a detection limit of 3.30 ×10^-9 mol/L, and the relative standard deviation for 1.32 ×10^-5 mol/L resveratrol (n = 11) is 3.8%. This method has been successfully applied for the determination of the resveratrol in red wine. Furthermore, the possible reaction mechanism was also discussed.展开更多
The determination of the methamidaphos pesticide residue on vegetables with a simple solid phase extract(SPE) flow injection(FI) -chemiluminescence(CL) method is described. The method is based on the enhancing e...The determination of the methamidaphos pesticide residue on vegetables with a simple solid phase extract(SPE) flow injection(FI) -chemiluminescence(CL) method is described. The method is based on the enhancing effect of methamidaphos on the CL reaction of luminol with hydrogen peroxide in an alkaline solution. Under the optimal conditions, the CL intensity is linear to the methamidaphos mass concentration in a range of 0. 2-13μg/mL ( r= 0. 9992). The detection limit(3σ) is 0. 047μg/mL. The relative standard deviations for the analysis of three samples are 1.8%, 2.5% and 3.7% ( n = 5 ), respectively. The recovery is in a range of 90%-109% by the method. In this work, this method was successfully applied to the determination of the methamidaphos residue on some vegetable samples.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
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
A procedure for the preconcentration of copper was described in this paper using multi-walled carbon nanotubes (MWCNTs) oxidized by potassium permanganate as the adsorbent for the enrichment of trace copper in water s...A procedure for the preconcentration of copper was described in this paper using multi-walled carbon nanotubes (MWCNTs) oxidized by potassium permanganate as the adsorbent for the enrichment of trace copper in water samples. Important parameters, such as the sample pH, the concentration and volume of eluent, sample flow rate and volume, and interference of coexisting ions, were investigated. The obtained results indicated that proposed method possessed an excellent analytical performance. The linear range, the detection limit, and precison (RSD) were 1–100 ng/mL (R(2) = 0.9993), 0.32 ng/mL and 2.88%, respectively. The results showed that copper could be adsorbed quantitatively on the pretreated MWCNTs with potassium permanganate, and proposed method was very useful in the monitoring of copper in the environment.展开更多
The comparison of solid phase extraction(SPE) for the preconcentration and isolation of polyphenols in tobacco samples was carried out by ultra-high performance liquid chromatography/tandem mass spectrometry (UPLC/...The comparison of solid phase extraction(SPE) for the preconcentration and isolation of polyphenols in tobacco samples was carried out by ultra-high performance liquid chromatography/tandem mass spectrometry (UPLC/MS/MS) and multivariate analysis.Several adsorbing materials of SPE(C18,NH2,SAX and OASIS) were investigated.It was found that the C18 and OASIS cartridges can not only speed up the purification process,but also simplify the SPE operation.A UPLC/MS/MS was used for the determination of polyphenols in tobacco samples after purification.All analytes were separated and determined in 2min.The limit of detection was 0.05 ng/mL.Cluster analysis(CA) and principal component analysis(PCA) were used for the analysis of 4 varieties(flue-cured tobacco,oriental tobacco,sun-cured tobacco and burley) in order to interpret the effect of planting and machining process on the concentration of polyphenols.The different types of tobacco samples could be easily clustered by CA.PCA on the chemical composition of tobacco resulted in two principal components(PCs) that take 84.2% of the total variance.The PCA and CA indicate that the polyphenols can be used for distinguishing tobacco types.展开更多
A solid phase extraction procedure of methomyl and thiodicarb from environmental water was presented. This method utilizes a 40—60 mesh activated carbon cartridge and high performance liquid chromatography (HPLC). Th...A solid phase extraction procedure of methomyl and thiodicarb from environmental water was presented. This method utilizes a 40—60 mesh activated carbon cartridge and high performance liquid chromatography (HPLC). The 40—60 mesh activated carbon works faster and yield higher adsorption efficiency. Detection limits of methomyl and thiodicarb in environmental water are 0 1 μg/L and 0 2 μg/L, respectively. Average recoveries of fortified methomyl and thiodicarb in water are in the range of 90 7%—98 8% and 88 9%—103 6%, respectively. The relative standard deviations are lower than 7%. This method is simple, rapid, accurate and precise.展开更多
A simple, rapid, and reproducible method is described employing solid phase extraction(SPE) using dichloromethane followed by gas chromatography(GC) with flame ionization detection(FID) for determination of volatile ...A simple, rapid, and reproducible method is described employing solid phase extraction(SPE) using dichloromethane followed by gas chromatography(GC) with flame ionization detection(FID) for determination of volatile organic compound(VOC) from the Buriganga River water of Bangladesh. The method was applied to detect the benzene, toluene, ethylbenzene, xylene and cumene(BTEXC) in the sample collected from the surface or 15 cm depth of water. Two hundred ml of n hexane pretreated and filtered water samples were applied directly to a C 18 SPE column. BTEXC were extracted with dichloromethane and average concentrations were obtained as 0 104 to 0 372 μg/ml. The highest concentration of benzene was found as 0 372 μg/ml with a relative standard deviation(RSD) of 6 2%, and cumene was not detected. Factors influencing SPE e.g., adsorbent types, sample load volume, eluting solvent, headspace and temperatures, were investigated. A cartridge containing a C 18 adsorbent and using dichloromethane gave better performance for extraction of BTEXC from water. Average recoveries exceeding 90% could be achieved for cumene at 4℃ with a 2 7% RSD.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
Two sample preparation methods were introduced and compared in this paper to establish a simple,quick and exact analysis of geosmin and 2-methylisoborneol.LC-18 column was employed in solid phase extraction(SPE),1.0 m...Two sample preparation methods were introduced and compared in this paper to establish a simple,quick and exact analysis of geosmin and 2-methylisoborneol.LC-18 column was employed in solid phase extraction(SPE),1.0 mL of hexane was adopted in liquid-liquid extraction(LLE),and the extracts were analyzed by gas chromatograph mass spectrum(GCMS)in selected ion mode.Mean recoveries of SPE were low for 2-methylisoborneol(2-MIB)and geosmin(GSM)with values below 50%.For LLE,the recoveries were satisfyingly above 50%for 2-MIB and 80%for GSM.Detection limits of the LLE method were as low as 1.0 ng/L for GSM and 5.0 ng/L for 2-MIB.A year-long investigation on odor chemicals of drinking water in Shanghai demonstrated that in the summer,there was a serious odor problem induced by a high concentration of 2-MIB.The highest concentration of 152.82 ng/L appeared in July in raw water,while GSM flocculation was minimal with concentrations below odor threshold.展开更多
Octylphenols, considered as xenoestrogens, mainly exist as 4-tert-octylphenol (OP) in aquatic environments. The high stability and accumulation of OP in aquatic systems have caused endocrine disruption. The OP in su...Octylphenols, considered as xenoestrogens, mainly exist as 4-tert-octylphenol (OP) in aquatic environments. The high stability and accumulation of OP in aquatic systems have caused endocrine disruption. The OP in surface water in Jinan, China was analyzed by gas chromatography-mass spectrometry (GC-MS) coupled with solid phase extraction (SPE). Water samples were extracted by SPE on a cartridge system containing C-18 as sorbent. To increase sensitivity and selectivity, OP was derivatized to 4-tert-octyl-phenoxy silane. With the use of phenanthrene-d10 as internal standard, the detection limit based on signal-to-noise ratio (S/N = 3) was 0.06 ng/mL. The average recovery was from 84.67% to 109.7%. The precision of the method given as the relative standard deviations (RSD) was within the range 6.24%-12.96%. In the target water samples, the concentrations of OP were as follows: 15.88-71.24 ng/L for Jinxiuchuan Reservoir, 3.850-26.68 ng/L for the city moat, 6.930-41.56 ng/L for Daming Lake, 66.03-474.2 ng/L for Xiaoqing River, 14.66-17.72 ng/L for the Yellow River, and 10.60-26.43 ng/L for Queshan Reservoir. The Xiaoqing River was seriously polluted due to the discharge of wastewater from Jinan. Jinxiuchuan Reservoir had a higher concentration of OP compared with the Yellow River and Queshan Reservoir, which is ascribed to the surrounding human activities. These data are reported for the first time, providing strong support for the control of OP pollution in Jinan.展开更多
Surface molecularly imprinted polymers (SMIPs) for selective adsorption of ampicillin sodium were synthesized using surface molecular imprinting technique with silica gel as a support. The physical and morphological...Surface molecularly imprinted polymers (SMIPs) for selective adsorption of ampicillin sodium were synthesized using surface molecular imprinting technique with silica gel as a support. The physical and morphological characteristics of the polymers were investigated by scanning electron microscope (SEM), Fourier transform infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), elemental analysis and nitrogen adsorption-desorption test. The obtained results showed that the SMIPs displayed great adsorption capacity (13.5 lag/mg), high recognition ability (the imprinted factor is 3.2) and good binding kinetics for ampicillin sodium. Finally, as solid phase extraction adsorbents, the SMIPs coupled with HPLC method were validated and applied for the enrichment, purification and determination of anapicillin sodium in real milk and blood samples. The averages of spiked accuracy ranged from 92.1% to 107.6%. The relative standard deviations of intra- and inter-day precisions were less than 4.6%. This study provides a new and promising method for enriching, extracting and determining ampicillin sodium in complex biological samples.展开更多
This paper developed a fluorometric method for the sensitive determination of nonylphenol in water samples by preconcentration with zirconium doped titanium dioxide nanotubes solid phase extraction.The parameters on e...This paper developed a fluorometric method for the sensitive determination of nonylphenol in water samples by preconcentration with zirconium doped titanium dioxide nanotubes solid phase extraction.The parameters on extraction that would influence the enrichment performance such as the kind and volume of eluent,sample pH,sample flow rate,and sample volume were optimized in detail.Under the optimal conditions,the proposed method provided an excellent linear range of 1-150 mg/L and good LOD of 0.076 mg/L.The relative standard deviation(RSD,n = 6) was 2.8%.Proposed method was also used for the analysis of real water samples and the spiked recoveries were satisfied in the range of 98.7-103%.展开更多
A novel capillary electrophoresis method for simultaneous determination of Cu and Pb has been developed in this paper.Cu(Ⅱ) and Pb(Ⅱ) ions were reacted with ABEDTA to form complex to achieve an ideal sensitivity...A novel capillary electrophoresis method for simultaneous determination of Cu and Pb has been developed in this paper.Cu(Ⅱ) and Pb(Ⅱ) ions were reacted with ABEDTA to form complex to achieve an ideal sensitivity of heavy metal complexes.The digestion solution of Rhizoma coptidis drug sample was purified by neutral Al_2O_3 column chromatography and the chromatographic behavior of metal-L complexes was investigated.The calibration curve was linear in the range of 5-60μg/mL for Cu^(2+) and 5-25μg/mL for Pb^(2+) with the correlation coefficients 0.9970 and 0.9972 for each(n = 5).The average recoveries were 86.2%for Pb and 90.1%for Cu,while the relative standard deviations were 5.1%and 3.6%respectively.The method was successfully applied to determine Cu and Pb in R.coptidis drug samples.展开更多
Surface-active organic molecules(surfactants)may influence the ability of an aerosol particle to act as a cloud condensation nuclei by reducing its surface tension.One source of organic mass in aerosol particles,which...Surface-active organic molecules(surfactants)may influence the ability of an aerosol particle to act as a cloud condensation nuclei by reducing its surface tension.One source of organic mass in aerosol particles,which may also contain surfactants,is bubble bursting on the sea surface.In order to directly compare these molecules in the ocean and aerosol particles,we developed a method using multiple solid phase extractions and high resolution mass spectrometry to characterize surface active organic molecules in both.This method has extraction efficiencies greater than 85%,75%,and 60%for anionic,cationic,and nonionic surfactant standards,respectively.In this study,we demonstrate the presence of three ionic classes of surface active organics in atmospheric aerosol particles and estuarine water from Skidaway Island,GA.With this extraction method,organic molecules from both estuarine water and atmospheric aerosol particles significantly reduced surface tension of pure water(surface tension depression of~18 m N/m)and had high ratios of hydrogen to carbon(H/C)and low ratios of oxygen to carbon(O/C),indicative of surfactants.While previous work has observed a larger fraction of anionic surface active organics in seawater and marine aerosol particles,here we show cationic surface active organics may make up a large fraction of the total surface active molecules in estuarine water(43%–47%).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
A simple and selective method was developed for the preconcentration, separation, and determination of trace amounts of As(Ⅲ) in an aqueous solution by solid phase extraction combined with graphite furnace atomic a...A simple and selective method was developed for the preconcentration, separation, and determination of trace amounts of As(Ⅲ) in an aqueous solution by solid phase extraction combined with graphite furnace atomic absorption spectrometry. Activated carbon (AC) was modified by sodium diethyldithiocarbamate (NaDDTC) and then used as a new, stable and easily prepared solid sorbent in a mini column for the extraction of As(Ⅲ) in aqueous solution. Factors influencing the sorption and desorption of As(Ⅲ), such as volume and concentration of eluent, sam- ple pH, flow rate and effect of interfering ions on the recovery of As(Ⅲ) have been systemically investigated. At pH 2.0 As(Ⅲ) could be adsorbed quantitatively by NaDDTC-AC, and then eluted completely with 2 mL of 3.0 moloL 1 HNO3. The amount of eluted As(Ⅲ) was measured using graphite furnace atomic absorption spectrometry. The detection limit of As(Ⅲ) was 0.04 ng·mL-1 with enrichment factor of 100 and the relative standard deviation (RSD, n=8) was 1.58% at 10 ng·mL-1 level.展开更多
In this work, a new sample pretreatment method prior to HPLC separations was developed for the determination of auxins in plant samples, Owing to its large surface area and high adsorption capacity, multi-walled carbo...In this work, a new sample pretreatment method prior to HPLC separations was developed for the determination of auxins in plant samples, Owing to its large surface area and high adsorption capacity, multi-walled carbon nanotube (MWCNT) was chosen as the adsorbent for the extraction of auxins from plant samples. In this study, two important auxins were selected as model analytes, namely indole-3- butyric acid (IBA) and 1-naphthylacetic acid (NAA). They could be extracted and concentrated due to their π-π stacking interactions with MWCNT. Then HPLC-UV was introduced to detect IBA and NAA after sample pretreatment. Factors that may affect the enrichment efficiency were investigated and optimized. Comparative studies showed that MWCNT was superior to CI 8 for the extraction of the two analytes. Validation experiments showed that the optimized method had good linearity (0.9998 and 0.9960), high recovery (81.4%-85.4%), and low detection limits (0.0030 mg/L and 0.0012 mg/L). The results indicated that the novel method had advantages of convenience, good sensitivity, high efficiency, and it was feasible for the determination of auxins in plant samples.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
基金financial support of the Natural Science Foundation of Beijing (2194086)the National Natural Science Foundation of China (Nos. 21922814, 21676273, 21961160745, 31961133019 and 21921005)
文摘Solid phase extraction is widely used in sample pretreatment,concentration and analysis processes due to high selectivity and suitability for low concentration sample system.In this review,we systematically summarized and discussed the development trends of solid phase extraction by bibliometrics method.By analyzing papers output scale,the research and development direction of solid phase extraction technology is prospected.We also give an overview on current strategies of novel solid phase extraction from the separation medium and separation technology.The paper aims to describe the global research profile and the development trends of solid phase extraction,to help researchers to accurately grasp the research trend and to provide support for scientific research institutions to formulate scientific policies and strategic plans.Furthermore,the prospect of the development and application of solid phase extraction is also discussed.
文摘A sensitive flow injection chemiluminescence method has been developed for the detection of resveratrol in red wine based on the fact that resveratrol can greatly enhance chemiluminescence reaction between KMnO4 and HCHO in sulfuric acid medium. Analytes were pre-concentrated on solid sorbents (C18 solid-phase extraction cartridges). Under the optimum conditions, the proposed method allows the measurement of resveratrol over the range of 1.32 × 10^-8 to 1.32 × 10^-5 mol/L with a detection limit of 3.30 ×10^-9 mol/L, and the relative standard deviation for 1.32 ×10^-5 mol/L resveratrol (n = 11) is 3.8%. This method has been successfully applied for the determination of the resveratrol in red wine. Furthermore, the possible reaction mechanism was also discussed.
文摘The determination of the methamidaphos pesticide residue on vegetables with a simple solid phase extract(SPE) flow injection(FI) -chemiluminescence(CL) method is described. The method is based on the enhancing effect of methamidaphos on the CL reaction of luminol with hydrogen peroxide in an alkaline solution. Under the optimal conditions, the CL intensity is linear to the methamidaphos mass concentration in a range of 0. 2-13μg/mL ( r= 0. 9992). The detection limit(3σ) is 0. 047μg/mL. The relative standard deviations for the analysis of three samples are 1.8%, 2.5% and 3.7% ( n = 5 ), respectively. The recovery is in a range of 90%-109% by the method. In this work, this method was successfully applied to the determination of the methamidaphos residue on some vegetable samples.
基金supported by the Preventive medicine and public health research project of Anhui,China(No.2011Y0103)the Natural Science Foundation of Anhui,China(No.11040606M216)
文摘To establish an analytical method for determination of four bisphenols (BPA, BPB, BPF, and BPS) and two alkylphenols (4-n-OP, 4-n-NP) in water by ultra performance liquid chromatography- tandem mass spectrometry (UPLC/MS/MS). The water samples were extracted and condensed with solid-phase extraction (SPE) using C18 cartridges and eluted by acetonitrile. Separation was carried out with Acquity BEH C8 column and detection were performed by UPLC/MS/MS. Quantification was calculated by using the internal standard BPA-d16 and 4-n-NP-d8. The linear correlation coefficients of these compounds in the range of 1.0-100.0μg/L were all over 0.999. The minimum detectable concentrations were 0.75-1.0 ng/L, and the recoveries ranged from 87.0% to 106.9%.
基金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.
文摘A procedure for the preconcentration of copper was described in this paper using multi-walled carbon nanotubes (MWCNTs) oxidized by potassium permanganate as the adsorbent for the enrichment of trace copper in water samples. Important parameters, such as the sample pH, the concentration and volume of eluent, sample flow rate and volume, and interference of coexisting ions, were investigated. The obtained results indicated that proposed method possessed an excellent analytical performance. The linear range, the detection limit, and precison (RSD) were 1–100 ng/mL (R(2) = 0.9993), 0.32 ng/mL and 2.88%, respectively. The results showed that copper could be adsorbed quantitatively on the pretreated MWCNTs with potassium permanganate, and proposed method was very useful in the monitoring of copper in the environment.
基金Supported by the Foundation of State Tabacco Monopoly Bureau(China) in Research Project(No.110200902008)
文摘The comparison of solid phase extraction(SPE) for the preconcentration and isolation of polyphenols in tobacco samples was carried out by ultra-high performance liquid chromatography/tandem mass spectrometry (UPLC/MS/MS) and multivariate analysis.Several adsorbing materials of SPE(C18,NH2,SAX and OASIS) were investigated.It was found that the C18 and OASIS cartridges can not only speed up the purification process,but also simplify the SPE operation.A UPLC/MS/MS was used for the determination of polyphenols in tobacco samples after purification.All analytes were separated and determined in 2min.The limit of detection was 0.05 ng/mL.Cluster analysis(CA) and principal component analysis(PCA) were used for the analysis of 4 varieties(flue-cured tobacco,oriental tobacco,sun-cured tobacco and burley) in order to interpret the effect of planting and machining process on the concentration of polyphenols.The different types of tobacco samples could be easily clustered by CA.PCA on the chemical composition of tobacco resulted in two principal components(PCs) that take 84.2% of the total variance.The PCA and CA indicate that the polyphenols can be used for distinguishing tobacco types.
文摘A solid phase extraction procedure of methomyl and thiodicarb from environmental water was presented. This method utilizes a 40—60 mesh activated carbon cartridge and high performance liquid chromatography (HPLC). The 40—60 mesh activated carbon works faster and yield higher adsorption efficiency. Detection limits of methomyl and thiodicarb in environmental water are 0 1 μg/L and 0 2 μg/L, respectively. Average recoveries of fortified methomyl and thiodicarb in water are in the range of 90 7%—98 8% and 88 9%—103 6%, respectively. The relative standard deviations are lower than 7%. This method is simple, rapid, accurate and precise.
文摘A simple, rapid, and reproducible method is described employing solid phase extraction(SPE) using dichloromethane followed by gas chromatography(GC) with flame ionization detection(FID) for determination of volatile organic compound(VOC) from the Buriganga River water of Bangladesh. The method was applied to detect the benzene, toluene, ethylbenzene, xylene and cumene(BTEXC) in the sample collected from the surface or 15 cm depth of water. Two hundred ml of n hexane pretreated and filtered water samples were applied directly to a C 18 SPE column. BTEXC were extracted with dichloromethane and average concentrations were obtained as 0 104 to 0 372 μg/ml. The highest concentration of benzene was found as 0 372 μg/ml with a relative standard deviation(RSD) of 6 2%, and cumene was not detected. Factors influencing SPE e.g., adsorbent types, sample load volume, eluting solvent, headspace and temperatures, were investigated. A cartridge containing a C 18 adsorbent and using dichloromethane gave better performance for extraction of BTEXC from water. Average recoveries exceeding 90% could be achieved for cumene at 4℃ with a 2 7% RSD.
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 study was supported by the National High-Tech Research and Development(863)Program of China(Grant No.2002AA601130)the Key Technologies Research and Development Program(No.2003BA808A17)of China.
文摘Two sample preparation methods were introduced and compared in this paper to establish a simple,quick and exact analysis of geosmin and 2-methylisoborneol.LC-18 column was employed in solid phase extraction(SPE),1.0 mL of hexane was adopted in liquid-liquid extraction(LLE),and the extracts were analyzed by gas chromatograph mass spectrum(GCMS)in selected ion mode.Mean recoveries of SPE were low for 2-methylisoborneol(2-MIB)and geosmin(GSM)with values below 50%.For LLE,the recoveries were satisfyingly above 50%for 2-MIB and 80%for GSM.Detection limits of the LLE method were as low as 1.0 ng/L for GSM and 5.0 ng/L for 2-MIB.A year-long investigation on odor chemicals of drinking water in Shanghai demonstrated that in the summer,there was a serious odor problem induced by a high concentration of 2-MIB.The highest concentration of 152.82 ng/L appeared in July in raw water,while GSM flocculation was minimal with concentrations below odor threshold.
基金supported by the State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences (No. KF2009-13)the National Natural Science Foundation of China (No. 21007019, 21107030,21277059, 21277060)
文摘Octylphenols, considered as xenoestrogens, mainly exist as 4-tert-octylphenol (OP) in aquatic environments. The high stability and accumulation of OP in aquatic systems have caused endocrine disruption. The OP in surface water in Jinan, China was analyzed by gas chromatography-mass spectrometry (GC-MS) coupled with solid phase extraction (SPE). Water samples were extracted by SPE on a cartridge system containing C-18 as sorbent. To increase sensitivity and selectivity, OP was derivatized to 4-tert-octyl-phenoxy silane. With the use of phenanthrene-d10 as internal standard, the detection limit based on signal-to-noise ratio (S/N = 3) was 0.06 ng/mL. The average recovery was from 84.67% to 109.7%. The precision of the method given as the relative standard deviations (RSD) was within the range 6.24%-12.96%. In the target water samples, the concentrations of OP were as follows: 15.88-71.24 ng/L for Jinxiuchuan Reservoir, 3.850-26.68 ng/L for the city moat, 6.930-41.56 ng/L for Daming Lake, 66.03-474.2 ng/L for Xiaoqing River, 14.66-17.72 ng/L for the Yellow River, and 10.60-26.43 ng/L for Queshan Reservoir. The Xiaoqing River was seriously polluted due to the discharge of wastewater from Jinan. Jinxiuchuan Reservoir had a higher concentration of OP compared with the Yellow River and Queshan Reservoir, which is ascribed to the surrounding human activities. These data are reported for the first time, providing strong support for the control of OP pollution in Jinan.
基金financially supported by the National Natural Science Foundation of China (Nos. 81573391 and 81173024)the National Key Projects of China (No. 812277802)
文摘Surface molecularly imprinted polymers (SMIPs) for selective adsorption of ampicillin sodium were synthesized using surface molecular imprinting technique with silica gel as a support. The physical and morphological characteristics of the polymers were investigated by scanning electron microscope (SEM), Fourier transform infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), elemental analysis and nitrogen adsorption-desorption test. The obtained results showed that the SMIPs displayed great adsorption capacity (13.5 lag/mg), high recognition ability (the imprinted factor is 3.2) and good binding kinetics for ampicillin sodium. Finally, as solid phase extraction adsorbents, the SMIPs coupled with HPLC method were validated and applied for the enrichment, purification and determination of anapicillin sodium in real milk and blood samples. The averages of spiked accuracy ranged from 92.1% to 107.6%. The relative standard deviations of intra- and inter-day precisions were less than 4.6%. This study provides a new and promising method for enriching, extracting and determining ampicillin sodium in complex biological samples.
文摘This paper developed a fluorometric method for the sensitive determination of nonylphenol in water samples by preconcentration with zirconium doped titanium dioxide nanotubes solid phase extraction.The parameters on extraction that would influence the enrichment performance such as the kind and volume of eluent,sample pH,sample flow rate,and sample volume were optimized in detail.Under the optimal conditions,the proposed method provided an excellent linear range of 1-150 mg/L and good LOD of 0.076 mg/L.The relative standard deviation(RSD,n = 6) was 2.8%.Proposed method was also used for the analysis of real water samples and the spiked recoveries were satisfied in the range of 98.7-103%.
基金supported by National Natural Science Foundation of China(No30672618)Major National S&T Program of China(No2009ZX09502-026)China Postdoctoral Science Foundation funded project(No201104073)
文摘A novel capillary electrophoresis method for simultaneous determination of Cu and Pb has been developed in this paper.Cu(Ⅱ) and Pb(Ⅱ) ions were reacted with ABEDTA to form complex to achieve an ideal sensitivity of heavy metal complexes.The digestion solution of Rhizoma coptidis drug sample was purified by neutral Al_2O_3 column chromatography and the chromatographic behavior of metal-L complexes was investigated.The calibration curve was linear in the range of 5-60μg/mL for Cu^(2+) and 5-25μg/mL for Pb^(2+) with the correlation coefficients 0.9970 and 0.9972 for each(n = 5).The average recoveries were 86.2%for Pb and 90.1%for Cu,while the relative standard deviations were 5.1%and 3.6%respectively.The method was successfully applied to determine Cu and Pb in R.coptidis drug samples.
基金supported by the University of Georgia Investment in Sciences Initiative and Office of Researchthe University of Georgia Junior Faculty Seed Grant。
文摘Surface-active organic molecules(surfactants)may influence the ability of an aerosol particle to act as a cloud condensation nuclei by reducing its surface tension.One source of organic mass in aerosol particles,which may also contain surfactants,is bubble bursting on the sea surface.In order to directly compare these molecules in the ocean and aerosol particles,we developed a method using multiple solid phase extractions and high resolution mass spectrometry to characterize surface active organic molecules in both.This method has extraction efficiencies greater than 85%,75%,and 60%for anionic,cationic,and nonionic surfactant standards,respectively.In this study,we demonstrate the presence of three ionic classes of surface active organics in atmospheric aerosol particles and estuarine water from Skidaway Island,GA.With this extraction method,organic molecules from both estuarine water and atmospheric aerosol particles significantly reduced surface tension of pure water(surface tension depression of~18 m N/m)and had high ratios of hydrogen to carbon(H/C)and low ratios of oxygen to carbon(O/C),indicative of surfactants.While previous work has observed a larger fraction of anionic surface active organics in seawater and marine aerosol particles,here we show cationic surface active organics may make up a large fraction of the total surface active molecules in estuarine water(43%–47%).
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.
文摘A simple and selective method was developed for the preconcentration, separation, and determination of trace amounts of As(Ⅲ) in an aqueous solution by solid phase extraction combined with graphite furnace atomic absorption spectrometry. Activated carbon (AC) was modified by sodium diethyldithiocarbamate (NaDDTC) and then used as a new, stable and easily prepared solid sorbent in a mini column for the extraction of As(Ⅲ) in aqueous solution. Factors influencing the sorption and desorption of As(Ⅲ), such as volume and concentration of eluent, sam- ple pH, flow rate and effect of interfering ions on the recovery of As(Ⅲ) have been systemically investigated. At pH 2.0 As(Ⅲ) could be adsorbed quantitatively by NaDDTC-AC, and then eluted completely with 2 mL of 3.0 moloL 1 HNO3. The amount of eluted As(Ⅲ) was measured using graphite furnace atomic absorption spectrometry. The detection limit of As(Ⅲ) was 0.04 ng·mL-1 with enrichment factor of 100 and the relative standard deviation (RSD, n=8) was 1.58% at 10 ng·mL-1 level.
基金supported by National Natural Science Foundation of China(Nos.20975056,21275082 and 81102411)Natural Science Foundation of Shandong(Nos. ZR2011BZ004,ZR2011BQ005)+2 种基金JSPS and NSFC under the Japan-China Scientific Cooperation Program(No.21111140014)State Key Laboratory of Analytical Chemistry for Life Science(No. SKLACLS1110)the National Key Basic Research Development Program of China(973 Special Preliminary Study Plan,No. 2012CB722705)
文摘In this work, a new sample pretreatment method prior to HPLC separations was developed for the determination of auxins in plant samples, Owing to its large surface area and high adsorption capacity, multi-walled carbon nanotube (MWCNT) was chosen as the adsorbent for the extraction of auxins from plant samples. In this study, two important auxins were selected as model analytes, namely indole-3- butyric acid (IBA) and 1-naphthylacetic acid (NAA). They could be extracted and concentrated due to their π-π stacking interactions with MWCNT. Then HPLC-UV was introduced to detect IBA and NAA after sample pretreatment. Factors that may affect the enrichment efficiency were investigated and optimized. Comparative studies showed that MWCNT was superior to CI 8 for the extraction of the two analytes. Validation experiments showed that the optimized method had good linearity (0.9998 and 0.9960), high recovery (81.4%-85.4%), and low detection limits (0.0030 mg/L and 0.0012 mg/L). The results indicated that the novel method had advantages of convenience, good sensitivity, high efficiency, and it was feasible for the determination of auxins in plant samples.
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.