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
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
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
In this work,Fe3O4-Al2O3@CNFs nanocomposite was synthesised and used as a nanosorbent in the ultrasound-assisted dispersive magnetic solid phase extraction(UA-DMSPE)of 17-beta estradiol(E2)in wastewater samples.The qu...In this work,Fe3O4-Al2O3@CNFs nanocomposite was synthesised and used as a nanosorbent in the ultrasound-assisted dispersive magnetic solid phase extraction(UA-DMSPE)of 17-beta estradiol(E2)in wastewater samples.The quantification of E2 was achieved using high performance liquid chromatography coupled with diode array detector(HPLC-DAD).Various parameters affecting the efficiency of this sample preparation technique were optimised to achieve excellent sensitivity and high recoveries of E2.Response surface methodology was utilised for optimisation of these parameters.Using the optimised conditions,the linear dynamic range was achieved in the range of 0.1e1000 mgL^-1and the correlation coefficient was found to be 0.9981.The preconcentration factor,enrichment factor,limit of detection(LOD)and limit of quantification(LOQ)were 67,169,0.025 mgL^-1and 0.083 mg L1,respectively.The relative standard deviation(%RSD)for the intraday(n?10)and interday(n?5 working days)were 1.8%and 3.3%,respectively.The developed UA-DMSPE/HPLC-DAD method was applied for the preconcentration and determination of E2 in wastewater samples.The obtained results indicated that E2 was present in the wastewater 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
[Objectives]This study was conducted to explore the occurrence levels of endocrine disruptors(EDCs)in rural areas around a county landfill in Tongren City.[Methods]The water around the landfill was sampled and analyze...[Objectives]This study was conducted to explore the occurrence levels of endocrine disruptors(EDCs)in rural areas around a county landfill in Tongren City.[Methods]The water around the landfill was sampled and analyzed.A solid-phase extraction and high performance liquid chromatography-tandem mass spectrometry(SPE-UPLC-MS/MS)method was established for the determination of 27 EDCs.After the HLB solid-phase extraction column was activated,a water sample,which was adjusted with phosphoric acid to a pH of 2(±0.5)and added with 500 mg of disodium EDTA,was loaded,and 5 ml of water and 20%methanol water was added for washing.Next,10 ml of elution solution was added for elution,and the collected eluate was evaporated under reduced pressure at 40℃to near dryness,and 1 ml of reconstitution solution was added to a constant volume.An ACQUITY UPLC BEH C18(100×2.1 mm,2.6μm)chromatographic column was adopted for LC separation by gradient elution with pure water solution-acetonitrile as the mobile phase.For MS detection,the MRM mode was adopted for collection,and the positive and negative ion modes were switched for simultaneous determination,and the internal standard method was used for quantification.[Results]The correlation coefficient R2 was greater than 0.99 in the linear range of each target substance.The limits of quantitation in the method were between 0.05 and 2.00 ng/L,and the recoveries ranged from 75.3%to 105.7%.[Conclusions]The method has high sensitivity,good accuracy and strong practical value.展开更多
In this study,ecofriendly and economic carboxy-terminated plant fibers(PFs)were used as adsorbents for the effective in-syringe solid phase extraction(IS-SPE)of fluoroquinolone(FQ)residues from water.Based on the ther...In this study,ecofriendly and economic carboxy-terminated plant fibers(PFs)were used as adsorbents for the effective in-syringe solid phase extraction(IS-SPE)of fluoroquinolone(FQ)residues from water.Based on the thermal esterification and etherification reaction of cellulose hydroxy with citric acid(CA)and sodium chloroacetate in aqueous solutions,carboxy groups grafted onto cotton,cattail,and corncob fibers were fabricated.Compared with carboxy-terminated corncob and cotton,CA-modified cattail with more carboxy groups showed excellent adsorption capacity for FQs.The modified cattail fibers were reproducible and reusable with relative standard deviations of 3.2%-4.2% within 10 cycles of adsorptiondesorption.A good extraction efficiency of 71.3%-80.9% was achieved after optimizing the extraction condition.Based on carboxylated cattail,IS-SPE coupled with ultra-performance liquid chromatography with a photodiode array detector was conducted to analyze FQs in environmental water samples.High sensitivity with limit of detections of 0.08-0.25 mg/L and good accuracy with recoveries of 83.8%-111.7% were obtained.Overall,the simple and environment-friendly modified waste PFs have potential applications in the effective extraction and detection of FQs in natural waters.展开更多
In this study,a hydrophilic resin named GCHM was fabricated based on poly(N-vinyl pyrrolidone-codivinylbenzene),characterized,and applied as a solid-phase extraction(SPE)material.Up to 44 pharmaceuticals and personal ...In this study,a hydrophilic resin named GCHM was fabricated based on poly(N-vinyl pyrrolidone-codivinylbenzene),characterized,and applied as a solid-phase extraction(SPE)material.Up to 44 pharmaceuticals and personal care products(PPCPs)belonging to 10 classes were recovered in environmental water samples.Different variables affecting extraction,such as adsorbent amount,sample pH,and loading speed,were optimized.Under optimal conditions,the average absolute recovgy of 44 PPCPs was 75.6%using GCHM,indicating a better performance than the commercial Oasis^HLB.SPE with home-made hydrophilic polymeric sorbent followed by ultra-performance liquid chromatography and tandem mass spectrometry was validated,and the method achieved good linearity(r2>0.991,for all analytes).In addition,the method detection limits of target compounds ranged from 0.03 to 0.6 ng/L.The developed method was applied to determine PPCPs in 10 environmental water samples taken from the Yangtze River,Huaihe River,and Taihu Lake,1 groundwater sample from Changzhou in Jiangsu Province,1 wastewater sample from Xiamen and 2 seawater samples from the Jiulong River in Fujian Province,China.In these samples,22 compounds were determined at levels ranging from 0.5 to 1590 ng/L.展开更多
In order to optimize the solid phase extraction(SPE)conditions of perfluorooctanoic acid(PFOA)in the raw leachate and treated leachate,the effects of activator properties,SPE cartridge,p H value,ionic strength,and elu...In order to optimize the solid phase extraction(SPE)conditions of perfluorooctanoic acid(PFOA)in the raw leachate and treated leachate,the effects of activator properties,SPE cartridge,p H value,ionic strength,and eluent properties were studied through single factor experiments.The optimal results of each single factor were obtained.Considering that the concentration of PFOA in the treated leachate is lower than that of the raw leachate,the SPE conditions of the treated leachate have been further optimized.Based on the above single-factor experiment,the main influencing factors were screened out as the volume of activator,ionic strength,and volume of eluent,and the three-factor threelevel response surface methodology(RSM)was optimized.The optimum SPE conditions of PFOA from treated landfill leachate were as follows:Activation of weak anion exchange(WAX)cartridge with 10 mL methanol,dosage of 600 mg KCl,6 m L 1%ammonia methanol eluted PFOA,the theory recovery rate is over95.67%.It has been verified that the error between the predicted value and the actual extraction recovery is small and has good repeatability.展开更多
In this study,we developed a novel on-line solid phase extraction(SPE)-ultra-high-performance liquid chromatography tandem mass spectrometry(UHPLC-MS/MS)-based analytical method for simultaneously quantifying 12 illic...In this study,we developed a novel on-line solid phase extraction(SPE)-ultra-high-performance liquid chromatography tandem mass spectrometry(UHPLC-MS/MS)-based analytical method for simultaneously quantifying 12 illicit drugs and metabolites(methamphetamine,amphetamine,morphine,codeine,6-monoacetylmorphine,benzoylecgonine,3,4-methylenedioxymethamphetamine,3,4-methylenedioxyamphetamine,cocaine,ketamine,norketamine,and methcathinone)and cotinine(COT)in wastewater samples.The analysis was performed by loading 2 m L of the sample onto an Oasis hydrophilic-lipophilic balance cartridge and using a cleanup step(5%methanol)to eliminate interference with a total run time of 13 min.The isotope-labeled internal standard method was used to quantify the target substances and correct for unavoidable losses and matrix effects during the on-line SPE process.Typical analytical characteristics used for method validation were sensitivity,linearity,precision,repeatability,recovery,and matrix effects.The limit of detection(LOD)and limit of quantification(LOQ)of each target were set at 0.20 ng/L and 0.50 ng/L,respectively.The linearity was between 0.5 ng/L and250 ng/L,except for that of COT.The intra-and inter-day precisions were<10.45%and 25.64%,respectively,and the relative recovery ranged from 83.74%to 162.26%.The method was used to analyze various wastewater samples from 33 cities in China,and the results were compared with the experimental results of identical samples analyzed using off-line SPE.The difference rate was between 19.91%and-20.44%,and the error range could be considered acceptable.These findings showed that on-line SPE is a suitable alternative to off-line SPE for the analysis of illicit drugs in samples.展开更多
Didanosine is an effective antiviral drug in untreated and antiretroviral therapy-experienced patients with Human Immunodeficiency Virus (HIV). An automated system using on-line solid extraction and High Performance L...Didanosine is an effective antiviral drug in untreated and antiretroviral therapy-experienced patients with Human Immunodeficiency Virus (HIV). An automated system using on-line solid extraction and High Performance Liquid Chromatography (HPLC) with ultraviolet (UV) detection was developed and validated for pharmacokinetic analysis of didanosine in dog plasma. Modifications were introduced on a previous methodology for simultaneous analysis of antiretroviral drugs in human plasma. Extraction was carried out on C18 cartridges, with high extraction yield as stationary phase, whereas mobile phase consisted of a mixture of 0.02 M potassium phosphate buffer, acetonitrile (KH2PO4: acetonitrile: 96:4, v/v) and 0.5% (w/v) of heptane sulphonic acid. The pH was adjusted to 6.5 with triethylamine. All samples and standard solutions were chromatographed at 28 1C. For an isocratic run, the fiux was 1.0 mL/min, detection was at 250 nm and injected volume was 20 mL. The method was selective and linear for concentrations between 50 and 5000 ng/mL. Drug stability data ranged from 96% to 98%, and limit of quantification was 25 ng/mL. Extraction yield was up to 95%. Drug stability in dog plasma was kept frozen at 20 1C for one month after three freeze-thaw cycles, and for 24 h after processing in the auto sampler. Assay was successfully applied to measure didanosine concentrations in plasma dogs.展开更多
A rapid,accurate,and sensitive analytical method,ultrasonication-assisted spraying based fine droplet formationeliquid phase microextractionegas chromatographyemass spectrometry(UA-SFDF-LPME-GCMS),was proposed for the...A rapid,accurate,and sensitive analytical method,ultrasonication-assisted spraying based fine droplet formationeliquid phase microextractionegas chromatographyemass spectrometry(UA-SFDF-LPME-GCMS),was proposed for the determination of trace amounts of hydroxychloroquine sulfate in human serum,urine,and saliva samples.To determine the best extraction strategy,several liquid and solid phase extraction methods were investigated for their efficiencies in isolation and preconcentration of hydroxychloroquine sulfate from biological matrices.The UA-SFDF-LPME method was determined to be the best extraction method as it was operationally simple and provided accurate results.Variables such as the extraction solvent,spraying number,sodium hydroxide concentration and volume,sample volume,mixing method,and mixing period were optimized for the proposed method using the onevariable-at-a-time approach.In addition,Tukey’s method based on a post hoc comparison test was employed to evaluate the significant difference between the parameters inspected.After the optimization studies,the limit of detection(LOD)and limit of quantification(LOQ)were determined to be 0.7 and 2.4 mg/kg,respectively.The sensitivity of the GC-MS system based on the LOD was enhanced approximately 440-fold when the UA-SFDF-LPME method was employed.Spiking experiments were also conducted for the human serum,urine,and saliva samples to determine the applicability and accuracy of the proposed method.Recoveries for the human serum,urine,and saliva samples were found to be in the ranges of 93.9%-101.7%,95.2%-105.0%,and 93.1%-102.3%,respectively.These results were satisfactory and indicated that the hydroxychloroquine sulfate level in the above biological samples could be analyzed using the proposed method.展开更多
Solid-phase extraction method has proven efficient and amenable to microchips.A novel DNA purification microchip was demonstrated using porous silicon dioxide as the solid phase matrix.Porous SiO_2 was coated on the w...Solid-phase extraction method has proven efficient and amenable to microchips.A novel DNA purification microchip was demonstrated using porous silicon dioxide as the solid phase matrix.Porous SiO_2 was coated on the wall of the channel of the microchip to provide a surface-enlarging matrix.The porous silicon was achieved by anodisation of the silicon reactor in a HF/ethanol mixture and then was oxidized thermally at a lower increasing/decreasing rate to form porous SiO_2.Through optimization of the preparing conditions a more stable microchip was established.Compared with the microchip without the porous layer,the microchip with the porous SiO_2 layer achieved higher extracted efficiency of DNA.Genomic DNA from rat whole blood could be extracted and purified in 35 minutes.展开更多
A simple,rapid and robust high-throughput assay for the quantitative analysis of irbesartan in plasma from two species using liquid chromatography tandem mass spectrometric method was developed and validated.Solid p...A simple,rapid and robust high-throughput assay for the quantitative analysis of irbesartan in plasma from two species using liquid chromatography tandem mass spectrometric method was developed and validated.Solid phase extraction was used and quantification was achieved using a positive electrospray ionization interface under multiple reactions monitoring condition.Complete validation(as per recent regulatory requirements)was done using human plasma.The same method was validated using dog plasma and the validation parameters met respective acceptance criteria.The method has shorter run time of 3 min.This will help in high throughput.The low aliquot volume in the method helped us to take enough sampling time points for better pharmacokinetic profiles.The calibration curve was shown to be linear from 12.1 to 6018.7 ng/ml in human plasma and 12.1 to 5987.2 ng/ml in dog plasma.This method was successfully applied to samples collected during bioavailability studies of irbesartan in humans and dogs.展开更多
Piperacillin/tazobactam and ciprofloxacin are often used in combination as initial empiric anti-biotic therapy in critical ill patients. Especially in patients undergoing continuous renal replacement therapy (CRRT) th...Piperacillin/tazobactam and ciprofloxacin are often used in combination as initial empiric anti-biotic therapy in critical ill patients. Especially in patients undergoing continuous renal replacement therapy (CRRT) the pharmacokinetics of antimicrobial agents can be highly variable. In order to avoid under- or overdosage of antibiotics therapeutic drug monitoring (TDM) is highly re-commendable. Based on two known HPLC assays for piperacillin a new method in combination with solid phase extraction (SPE) for the simultaneous determination of piperacillin and ciprofloxacin was developed. Method validation was performed according to the EMA guideline on validation of bioanalytical methods. The HPLC column used was a Perfect Bond ODS-HD C18 analytical column (100 mm × 4.6 mm i.d., particle size 5 μm), equipped with a guard column (10 mm × 4.6 mm, particle size 5 μm) containing the same packing material. Detection wavelength was set at 228 nm for piperacillin and benzylpenicillin was used as internal standard (IS). Ciprofloxacin was determined at two wavelengths (280 nm, 315 nm). This newly developed HPLC method in combination with SPE-extraction allows an accurate, precise, specific and efficient determination of piperacillin and ciprofloxacin in biological matrices. Results allow the calculation of all relevant pharmacokinetic data for critically ill patients undergoing CRRT and the optimization of dosing and TDM.展开更多
A solid phase extraction procedure(SPE)is described for the quantitative analysis of polycyclic aromatic hydrocarbons(PAHs)in atmospheric particulate matter(PM),as ubiquitous environmental pollutants routinely measure...A solid phase extraction procedure(SPE)is described for the quantitative analysis of polycyclic aromatic hydrocarbons(PAHs)in atmospheric particulate matter(PM),as ubiquitous environmental pollutants routinely measured in air qualitymonitoring.A SPE cartridge was used based on a molecular imprinted polymer(MIP-SPE)properly tailored for selective retention of PAHs with 4 and more benzene fused rings.The performance of the clean-up procedure was evaluated with the specific concern of selective purification towards saturated hydrocarbons,which are the PM components mostly interfering GC analysis of target PAHs.Under optimized operative conditions,the MIP-SPE provided analyte recovery close to 95%for heavier PAHs,from benzo(α)pyrene to benzo(ghi)perylene,and close to 90%for four benzene rings PAHs,with good reproducibility(RSDs:2.5%-5.9%).Otherwise,C_(17)-C_(32) n-alkanes were nearly completely removed.The proposed method was critically compared with Solid Phase Micro Extraction(SPME)using a polyacrylate fiber.Both methods were successfully applied to the analysis of ambient PM2.5 samples collected at an urban polluted site.Between the two procedures,the MIP-SPE provided the highest recovery(R%≥93%)for PAHs with 5 and more benzene rings,but lower for lighter PAHs.In contrast,SPME showed a mean acceptable R%value(∼80%)for all the investigated PAHs,except for the heaviest PAHs in the most polluted samples(R%:110%-138%),suggesting an incomplete purification from the interfering n-hydrocarbons.展开更多
In this study for the first time, a novel copper Solid Phase Microextraction (SPME) fiber has been introduced for removal of naphthalene, phenanthrene and anthracene from aqueous solution. Copper was used as a solid s...In this study for the first time, a novel copper Solid Phase Microextraction (SPME) fiber has been introduced for removal of naphthalene, phenanthrene and anthracene from aqueous solution. Copper was used as a solid support, which was at first coated by 3-mercaptopropyltrimethoxysi- lane. A stationary phase of oxidized multi walled carbon nanotube (MWCNTs)) was bonded to the surface of the copper wire. The developed SPME was characterized by IR and Scanning Electron Microscopy (SEM) and coupled to gas chromatography for separation of the analytes. Stability of the fiber, the effect of coating thickness and recovery time were optimized. The MWCNTs film thickness was about 5 μm which was perfect for a rapid mass transfer. The detection limits were at the range of 0.005 to 0.1 μg·L<sup>-1</sup>. The calibration curves were linear R<sup>2</sup> > 0.9813 in the range of 0.01 to 5 μg·L<sup>-1</sup>. The method has been successfully applied for real samples with standard addition of 5 μL<sup>-1</sup> of each sample. Stability study of the fiber to acid and alkali shows that it can be used for more than 50 times.展开更多
Promethazine(PHZ)is used as a sedative in veterinary medicine,and its residue can threaten the health of human.The electrochemical detection of PHZ is suitable method for application in the field.However,the tradition...Promethazine(PHZ)is used as a sedative in veterinary medicine,and its residue can threaten the health of human.The electrochemical detection of PHZ is suitable method for application in the field.However,the traditional electroanalysis is difficult to perform directly in meat samples due to matrix interference.This work integrates magnetic solid-phase extraction and differential pulse voltammetry for highly sensitive and selective determination of PHZ in beef and beef liver for the first time.CoFe_(2)O_(4)/graphene coated with C_(18)-functionalized mesoporous silica(MG@mSiO_(2)-C_(18))is synthesized as dispersed magnetic adsorbent to extract PHZ.Magnetic glassy carbon electrode modified with nitrogen-doped hollow carbon microspheres(HCM)attracts the MG@mSiO_(2)-C_(18)with PHZ,and directly detects the PHZ without elution procedure.MG@mSiO_(2)-C_(18)can separate PHZ to avoid the interference of impurities on following detection,and also concentrate PHZ on magnetic electrode.Additionally,the electrode modification with HCM can amplify the electrochemical signal of PHZ.Finally,the integrated PHZ determination method exhibits a wide linear range from 0.08μmol/L to 300μmol/L with a low limit of detection of 9.8 nmol/L.The beef sample analysis presents excellent recovery,demonstrating that this protocol is promising for the rapid and onsite detection of PHZ in real meat samples。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.
基金This work was supported by“National Key Research and Development Program of China”(Project No.2018YFC1603400)Science and Technology Program of Hebei Province(Project No.19225503D).
文摘The aim of this work was to develop an automated on-line solid phase extraction(SPE)with liquid chromatography-tandem mass spectrometry method for the detection of fifteen sulfonamides in pork and fish samples.Samples were extracted with 0.2%formic acid acetonitrile solution,purified by on-line SPE device with HLB column,then separated by XBridge C18 column,using 0.1%formic acid solution and acetonitrile as the mobile phase.Mass spectrometric data was acquired under multiple reaction monitoring(MRM)mode using positive ionization electrospray.Internal standard method was used in the quantification,good linear relationship was got in range of 0.1–100 ng/mL and correlation coefficient was higher than 0.9990.The limits of detection were in the range of 0.125–2.00g/kg and the limits of quantitation were in the range of 0.250–5.00g/kg.Recoveries of the method were in range of 78.3%–99.3%,relative standard deviation were lower than 10%.The method was simple,sensitivity,and could be used for routine supervision and analysis of fifteen sulfonamides in pork and fish.
基金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the Department of Science and Technology(DST,South Africa)/National Nanoscience Postgraduate Teaching and Training Programme(NNPTTP)and National Research Foundation(NRF,South Africa,grant no.99270&91230).
文摘In this work,Fe3O4-Al2O3@CNFs nanocomposite was synthesised and used as a nanosorbent in the ultrasound-assisted dispersive magnetic solid phase extraction(UA-DMSPE)of 17-beta estradiol(E2)in wastewater samples.The quantification of E2 was achieved using high performance liquid chromatography coupled with diode array detector(HPLC-DAD).Various parameters affecting the efficiency of this sample preparation technique were optimised to achieve excellent sensitivity and high recoveries of E2.Response surface methodology was utilised for optimisation of these parameters.Using the optimised conditions,the linear dynamic range was achieved in the range of 0.1e1000 mgL^-1and the correlation coefficient was found to be 0.9981.The preconcentration factor,enrichment factor,limit of detection(LOD)and limit of quantification(LOQ)were 67,169,0.025 mgL^-1and 0.083 mg L1,respectively.The relative standard deviation(%RSD)for the intraday(n?10)and interday(n?5 working days)were 1.8%and 3.3%,respectively.The developed UA-DMSPE/HPLC-DAD method was applied for the preconcentration and determination of E2 in wastewater samples.The obtained results indicated that E2 was present in the wastewater 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.
基金Supported by Tongren Science and Technology Planning Project (TSKY[2022]42)Education Science Planning Project of Department of Education of Guizhou Province (2023B111).
文摘[Objectives]This study was conducted to explore the occurrence levels of endocrine disruptors(EDCs)in rural areas around a county landfill in Tongren City.[Methods]The water around the landfill was sampled and analyzed.A solid-phase extraction and high performance liquid chromatography-tandem mass spectrometry(SPE-UPLC-MS/MS)method was established for the determination of 27 EDCs.After the HLB solid-phase extraction column was activated,a water sample,which was adjusted with phosphoric acid to a pH of 2(±0.5)and added with 500 mg of disodium EDTA,was loaded,and 5 ml of water and 20%methanol water was added for washing.Next,10 ml of elution solution was added for elution,and the collected eluate was evaporated under reduced pressure at 40℃to near dryness,and 1 ml of reconstitution solution was added to a constant volume.An ACQUITY UPLC BEH C18(100×2.1 mm,2.6μm)chromatographic column was adopted for LC separation by gradient elution with pure water solution-acetonitrile as the mobile phase.For MS detection,the MRM mode was adopted for collection,and the positive and negative ion modes were switched for simultaneous determination,and the internal standard method was used for quantification.[Results]The correlation coefficient R2 was greater than 0.99 in the linear range of each target substance.The limits of quantitation in the method were between 0.05 and 2.00 ng/L,and the recoveries ranged from 75.3%to 105.7%.[Conclusions]The method has high sensitivity,good accuracy and strong practical value.
基金supported by the National Natural Science Foundation of China(Grant Nos.:81703469 and 81973277)Open Fund of the State Key Laboratory of Quality Research in Chinese Medicine,University of Macao(Grant No.:SKL-QRCM(UM)-2020-2022,QRCM-OP21007)the World-Class Universities(Disciplines)and the Characteristic Development Guidance Funds for the Central Universities(Grant No.:PY3A012).
文摘In this study,ecofriendly and economic carboxy-terminated plant fibers(PFs)were used as adsorbents for the effective in-syringe solid phase extraction(IS-SPE)of fluoroquinolone(FQ)residues from water.Based on the thermal esterification and etherification reaction of cellulose hydroxy with citric acid(CA)and sodium chloroacetate in aqueous solutions,carboxy groups grafted onto cotton,cattail,and corncob fibers were fabricated.Compared with carboxy-terminated corncob and cotton,CA-modified cattail with more carboxy groups showed excellent adsorption capacity for FQs.The modified cattail fibers were reproducible and reusable with relative standard deviations of 3.2%-4.2% within 10 cycles of adsorptiondesorption.A good extraction efficiency of 71.3%-80.9% was achieved after optimizing the extraction condition.Based on carboxylated cattail,IS-SPE coupled with ultra-performance liquid chromatography with a photodiode array detector was conducted to analyze FQs in environmental water samples.High sensitivity with limit of detections of 0.08-0.25 mg/L and good accuracy with recoveries of 83.8%-111.7% were obtained.Overall,the simple and environment-friendly modified waste PFs have potential applications in the effective extraction and detection of FQs in natural waters.
基金Authors gratefully acknowledge the generous support provided by the National Key R&D Program of China(Grant No.2016YFE0112300)the National Natural Science Foundation of China(Grant Nos.51678290,51438008 and 51778281)+3 种基金Jiangsu Natural Science Fund,China(No.B K 20171342)Jiangsu Provincial Key Medical Discipline(Laboratory)of China(No.Z D X K A 2016008)Jiangsu Preventive Medicine Project of China(No.Y2018081)The authors also thank Dr.Zhe Wang from Nanyang Technological University(Singapore)for his support on this project.
文摘In this study,a hydrophilic resin named GCHM was fabricated based on poly(N-vinyl pyrrolidone-codivinylbenzene),characterized,and applied as a solid-phase extraction(SPE)material.Up to 44 pharmaceuticals and personal care products(PPCPs)belonging to 10 classes were recovered in environmental water samples.Different variables affecting extraction,such as adsorbent amount,sample pH,and loading speed,were optimized.Under optimal conditions,the average absolute recovgy of 44 PPCPs was 75.6%using GCHM,indicating a better performance than the commercial Oasis^HLB.SPE with home-made hydrophilic polymeric sorbent followed by ultra-performance liquid chromatography and tandem mass spectrometry was validated,and the method achieved good linearity(r2>0.991,for all analytes).In addition,the method detection limits of target compounds ranged from 0.03 to 0.6 ng/L.The developed method was applied to determine PPCPs in 10 environmental water samples taken from the Yangtze River,Huaihe River,and Taihu Lake,1 groundwater sample from Changzhou in Jiangsu Province,1 wastewater sample from Xiamen and 2 seawater samples from the Jiulong River in Fujian Province,China.In these samples,22 compounds were determined at levels ranging from 0.5 to 1590 ng/L.
基金Supported by the Grant from the Science and Technique Key Programs of Power China Ltd.(P45220)the Open-ended Fund of Chongqing University’s Large-Scale Equipment(202203150184)
文摘In order to optimize the solid phase extraction(SPE)conditions of perfluorooctanoic acid(PFOA)in the raw leachate and treated leachate,the effects of activator properties,SPE cartridge,p H value,ionic strength,and eluent properties were studied through single factor experiments.The optimal results of each single factor were obtained.Considering that the concentration of PFOA in the treated leachate is lower than that of the raw leachate,the SPE conditions of the treated leachate have been further optimized.Based on the above single-factor experiment,the main influencing factors were screened out as the volume of activator,ionic strength,and volume of eluent,and the three-factor threelevel response surface methodology(RSM)was optimized.The optimum SPE conditions of PFOA from treated landfill leachate were as follows:Activation of weak anion exchange(WAX)cartridge with 10 mL methanol,dosage of 600 mg KCl,6 m L 1%ammonia methanol eluted PFOA,the theory recovery rate is over95.67%.It has been verified that the error between the predicted value and the actual extraction recovery is small and has good repeatability.
基金supported by the National Key Research and Development Program of China(Grant No.:2018YFC0807402)the National Natural Science Foundation of China(Grant No.:82073810)。
文摘In this study,we developed a novel on-line solid phase extraction(SPE)-ultra-high-performance liquid chromatography tandem mass spectrometry(UHPLC-MS/MS)-based analytical method for simultaneously quantifying 12 illicit drugs and metabolites(methamphetamine,amphetamine,morphine,codeine,6-monoacetylmorphine,benzoylecgonine,3,4-methylenedioxymethamphetamine,3,4-methylenedioxyamphetamine,cocaine,ketamine,norketamine,and methcathinone)and cotinine(COT)in wastewater samples.The analysis was performed by loading 2 m L of the sample onto an Oasis hydrophilic-lipophilic balance cartridge and using a cleanup step(5%methanol)to eliminate interference with a total run time of 13 min.The isotope-labeled internal standard method was used to quantify the target substances and correct for unavoidable losses and matrix effects during the on-line SPE process.Typical analytical characteristics used for method validation were sensitivity,linearity,precision,repeatability,recovery,and matrix effects.The limit of detection(LOD)and limit of quantification(LOQ)of each target were set at 0.20 ng/L and 0.50 ng/L,respectively.The linearity was between 0.5 ng/L and250 ng/L,except for that of COT.The intra-and inter-day precisions were<10.45%and 25.64%,respectively,and the relative recovery ranged from 83.74%to 162.26%.The method was used to analyze various wastewater samples from 33 cities in China,and the results were compared with the experimental results of identical samples analyzed using off-line SPE.The difference rate was between 19.91%and-20.44%,and the error range could be considered acceptable.These findings showed that on-line SPE is a suitable alternative to off-line SPE for the analysis of illicit drugs in samples.
基金supported by the Research Foundation of the State of So Paulo (FAPESP/Brazil)National Council of Technological and Scientific Development (CNPq/Brazil)
文摘Didanosine is an effective antiviral drug in untreated and antiretroviral therapy-experienced patients with Human Immunodeficiency Virus (HIV). An automated system using on-line solid extraction and High Performance Liquid Chromatography (HPLC) with ultraviolet (UV) detection was developed and validated for pharmacokinetic analysis of didanosine in dog plasma. Modifications were introduced on a previous methodology for simultaneous analysis of antiretroviral drugs in human plasma. Extraction was carried out on C18 cartridges, with high extraction yield as stationary phase, whereas mobile phase consisted of a mixture of 0.02 M potassium phosphate buffer, acetonitrile (KH2PO4: acetonitrile: 96:4, v/v) and 0.5% (w/v) of heptane sulphonic acid. The pH was adjusted to 6.5 with triethylamine. All samples and standard solutions were chromatographed at 28 1C. For an isocratic run, the fiux was 1.0 mL/min, detection was at 250 nm and injected volume was 20 mL. The method was selective and linear for concentrations between 50 and 5000 ng/mL. Drug stability data ranged from 96% to 98%, and limit of quantification was 25 ng/mL. Extraction yield was up to 95%. Drug stability in dog plasma was kept frozen at 20 1C for one month after three freeze-thaw cycles, and for 24 h after processing in the auto sampler. Assay was successfully applied to measure didanosine concentrations in plasma dogs.
基金supported by the Health Institutes of Turkey(TüSEB)(Project No.2020CV01-8946)。
文摘A rapid,accurate,and sensitive analytical method,ultrasonication-assisted spraying based fine droplet formationeliquid phase microextractionegas chromatographyemass spectrometry(UA-SFDF-LPME-GCMS),was proposed for the determination of trace amounts of hydroxychloroquine sulfate in human serum,urine,and saliva samples.To determine the best extraction strategy,several liquid and solid phase extraction methods were investigated for their efficiencies in isolation and preconcentration of hydroxychloroquine sulfate from biological matrices.The UA-SFDF-LPME method was determined to be the best extraction method as it was operationally simple and provided accurate results.Variables such as the extraction solvent,spraying number,sodium hydroxide concentration and volume,sample volume,mixing method,and mixing period were optimized for the proposed method using the onevariable-at-a-time approach.In addition,Tukey’s method based on a post hoc comparison test was employed to evaluate the significant difference between the parameters inspected.After the optimization studies,the limit of detection(LOD)and limit of quantification(LOQ)were determined to be 0.7 and 2.4 mg/kg,respectively.The sensitivity of the GC-MS system based on the LOD was enhanced approximately 440-fold when the UA-SFDF-LPME method was employed.Spiking experiments were also conducted for the human serum,urine,and saliva samples to determine the applicability and accuracy of the proposed method.Recoveries for the human serum,urine,and saliva samples were found to be in the ranges of 93.9%-101.7%,95.2%-105.0%,and 93.1%-102.3%,respectively.These results were satisfactory and indicated that the hydroxychloroquine sulfate level in the above biological samples could be analyzed using the proposed method.
基金The authors greatly acknowledge the financial support from the National Science Foundation of China under Grant number 20299030, 60427001 and 60501020.
文摘Solid-phase extraction method has proven efficient and amenable to microchips.A novel DNA purification microchip was demonstrated using porous silicon dioxide as the solid phase matrix.Porous SiO_2 was coated on the wall of the channel of the microchip to provide a surface-enlarging matrix.The porous silicon was achieved by anodisation of the silicon reactor in a HF/ethanol mixture and then was oxidized thermally at a lower increasing/decreasing rate to form porous SiO_2.Through optimization of the preparing conditions a more stable microchip was established.Compared with the microchip without the porous layer,the microchip with the porous SiO_2 layer achieved higher extracted efficiency of DNA.Genomic DNA from rat whole blood could be extracted and purified in 35 minutes.
基金The authors acknowledge Ranbaxy Laboratories Limited to supports this study.
文摘A simple,rapid and robust high-throughput assay for the quantitative analysis of irbesartan in plasma from two species using liquid chromatography tandem mass spectrometric method was developed and validated.Solid phase extraction was used and quantification was achieved using a positive electrospray ionization interface under multiple reactions monitoring condition.Complete validation(as per recent regulatory requirements)was done using human plasma.The same method was validated using dog plasma and the validation parameters met respective acceptance criteria.The method has shorter run time of 3 min.This will help in high throughput.The low aliquot volume in the method helped us to take enough sampling time points for better pharmacokinetic profiles.The calibration curve was shown to be linear from 12.1 to 6018.7 ng/ml in human plasma and 12.1 to 5987.2 ng/ml in dog plasma.This method was successfully applied to samples collected during bioavailability studies of irbesartan in humans and dogs.
文摘Piperacillin/tazobactam and ciprofloxacin are often used in combination as initial empiric anti-biotic therapy in critical ill patients. Especially in patients undergoing continuous renal replacement therapy (CRRT) the pharmacokinetics of antimicrobial agents can be highly variable. In order to avoid under- or overdosage of antibiotics therapeutic drug monitoring (TDM) is highly re-commendable. Based on two known HPLC assays for piperacillin a new method in combination with solid phase extraction (SPE) for the simultaneous determination of piperacillin and ciprofloxacin was developed. Method validation was performed according to the EMA guideline on validation of bioanalytical methods. The HPLC column used was a Perfect Bond ODS-HD C18 analytical column (100 mm × 4.6 mm i.d., particle size 5 μm), equipped with a guard column (10 mm × 4.6 mm, particle size 5 μm) containing the same packing material. Detection wavelength was set at 228 nm for piperacillin and benzylpenicillin was used as internal standard (IS). Ciprofloxacin was determined at two wavelengths (280 nm, 315 nm). This newly developed HPLC method in combination with SPE-extraction allows an accurate, precise, specific and efficient determination of piperacillin and ciprofloxacin in biological matrices. Results allow the calculation of all relevant pharmacokinetic data for critically ill patients undergoing CRRT and the optimization of dosing and TDM.
基金supported by the Emilia Romagna Region (POR FESR 2014-2020),project IPA/BC-MONITOR (No. E32I16000030007 2016)
文摘A solid phase extraction procedure(SPE)is described for the quantitative analysis of polycyclic aromatic hydrocarbons(PAHs)in atmospheric particulate matter(PM),as ubiquitous environmental pollutants routinely measured in air qualitymonitoring.A SPE cartridge was used based on a molecular imprinted polymer(MIP-SPE)properly tailored for selective retention of PAHs with 4 and more benzene fused rings.The performance of the clean-up procedure was evaluated with the specific concern of selective purification towards saturated hydrocarbons,which are the PM components mostly interfering GC analysis of target PAHs.Under optimized operative conditions,the MIP-SPE provided analyte recovery close to 95%for heavier PAHs,from benzo(α)pyrene to benzo(ghi)perylene,and close to 90%for four benzene rings PAHs,with good reproducibility(RSDs:2.5%-5.9%).Otherwise,C_(17)-C_(32) n-alkanes were nearly completely removed.The proposed method was critically compared with Solid Phase Micro Extraction(SPME)using a polyacrylate fiber.Both methods were successfully applied to the analysis of ambient PM2.5 samples collected at an urban polluted site.Between the two procedures,the MIP-SPE provided the highest recovery(R%≥93%)for PAHs with 5 and more benzene rings,but lower for lighter PAHs.In contrast,SPME showed a mean acceptable R%value(∼80%)for all the investigated PAHs,except for the heaviest PAHs in the most polluted samples(R%:110%-138%),suggesting an incomplete purification from the interfering n-hydrocarbons.
文摘In this study for the first time, a novel copper Solid Phase Microextraction (SPME) fiber has been introduced for removal of naphthalene, phenanthrene and anthracene from aqueous solution. Copper was used as a solid support, which was at first coated by 3-mercaptopropyltrimethoxysi- lane. A stationary phase of oxidized multi walled carbon nanotube (MWCNTs)) was bonded to the surface of the copper wire. The developed SPME was characterized by IR and Scanning Electron Microscopy (SEM) and coupled to gas chromatography for separation of the analytes. Stability of the fiber, the effect of coating thickness and recovery time were optimized. The MWCNTs film thickness was about 5 μm which was perfect for a rapid mass transfer. The detection limits were at the range of 0.005 to 0.1 μg·L<sup>-1</sup>. The calibration curves were linear R<sup>2</sup> > 0.9813 in the range of 0.01 to 5 μg·L<sup>-1</sup>. The method has been successfully applied for real samples with standard addition of 5 μL<sup>-1</sup> of each sample. Stability study of the fiber to acid and alkali shows that it can be used for more than 50 times.
基金supported by the National Key R&D Program of China(No.2019YFC1605400)the National Natural Science Foundation of China(Nos.21874065 and 22176085)。
文摘Promethazine(PHZ)is used as a sedative in veterinary medicine,and its residue can threaten the health of human.The electrochemical detection of PHZ is suitable method for application in the field.However,the traditional electroanalysis is difficult to perform directly in meat samples due to matrix interference.This work integrates magnetic solid-phase extraction and differential pulse voltammetry for highly sensitive and selective determination of PHZ in beef and beef liver for the first time.CoFe_(2)O_(4)/graphene coated with C_(18)-functionalized mesoporous silica(MG@mSiO_(2)-C_(18))is synthesized as dispersed magnetic adsorbent to extract PHZ.Magnetic glassy carbon electrode modified with nitrogen-doped hollow carbon microspheres(HCM)attracts the MG@mSiO_(2)-C_(18)with PHZ,and directly detects the PHZ without elution procedure.MG@mSiO_(2)-C_(18)can separate PHZ to avoid the interference of impurities on following detection,and also concentrate PHZ on magnetic electrode.Additionally,the electrode modification with HCM can amplify the electrochemical signal of PHZ.Finally,the integrated PHZ determination method exhibits a wide linear range from 0.08μmol/L to 300μmol/L with a low limit of detection of 9.8 nmol/L.The beef sample analysis presents excellent recovery,demonstrating that this protocol is promising for the rapid and onsite detection of PHZ in real meat samples。
