最新刊期
卷 38 ， 期 3 ， 2019
- 摘要：A novel method was developed for the determination of thirteen nitroimidazoles in fish blood by ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） with supramolecular solvent based dispersive liquid-liquid microextraction.The target compounds in fish blood were extracted with a supramolecular solvent consisted of octanol,tetrahydrofuran and water.The analytes were separated on a Waters ACQUITY UPLC BEH C18 column（2.1 mm×50 mm×1.7 μm） by gradient elution with acetonitrile-water as mobile phases.The qualitative and quantitative analyses were conducted by electrospray ionization mass spectrometry in positive ion mode under multiple reaction monitoring（MRM） mode.Experimental results demonstrated that good linearities for the analytes were observed in their respective concentration ranges with correlation coefficients（r2） larger than 0.998.The limits of detection（LOD） and the limits of quantitation（LOQ） were in the ranges of 0.05-0.2 μg/L and 0.1-0.5 μg/L,respectively.Recoveries for 13 nitroimidazoles at three spiked levels ranged from 88.4% to 105% with relative standard deviations（n=6） of 4.3%-11%.The method was simple,rapid,accurate and reliable,and could be used for the analysis of nitroimidazole residues in fish blood samples.关键词：supramolecular solvent;dispersive liquid-liquid microextraction;ultra performance liquid chromatography-tandem mass spectrometry;nitroimidazoles;fish blood
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发布时间： - 摘要：An ultrahigh performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） with solid supported liquid-liquid extraction（SLE） was developed for the determination of seven hydroxyl polycyclic aromatic hydrocarbons（OH-PAHs） in urine samples.08 mL enzymatic hydrolyzed urine sample was extracted on a SLE cartridge.Parameters for SLE,including type and volume of eluting solvent,and nitrogen evaporation pressure were optimized.The adsorbed analytes were eluted with 6 mL ethyl acetate,and the collected eluate was evaporated to dryness under nitrogen at a pressure of 48 kPa at 25 ℃,then analyzed by UPLC-MS/MS and quantified by the internal standard method.Under the optimized conditions,the calibration curves for the analytes were linear in the range of 0.3-3 000 mg·L-1,with correlation coefficients not less than 0.995 1.The detection limits（S/N=3） and quantitation limits（S/N=10） were in the ranges of 0.05-1.0 mg·L-1 and 0.15-3.0 mg·L-1,respectively.The recoveries for OH-PAHs in urine samples at three spiked levels ranged from 70.8% to 117%,with the intra day（n=3） and inter-day（n=3） RSDs of 3.7%-9.6% and 3.7%-11%,respectively.The proposed method was successfully applied in the determination of OH-PAHs in urine from 10 petroleum workers and 10 control groups（college students）.Except 2-hydroxy phenanthrene and 9-hydroxy-phenanthrene,the concentrations of the other five OH-PAHs in the urine samples of petroleum workers were much higher than that in the control samples（p<0.05）.The proposed SLE method only included two steps,therefore,the proposed method is applicable for the facile and efficient monitoring of OH-PAHs in urine samples.关键词：hydroxyl polycyclic aromatic hydrocarbons（OH-PAHs）;solid supported liquid-liquid extraction（SLE）;ultrahigh performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）;urine
- 1090
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发布时间： - 摘要：A method of high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS） was established for the determination of migration of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide（DOPO）in plastic polymers.The migration regularity of the analyte in different simulants,temperatures and times were studied.Samples were soaked with the food simulants according to（EU）2017/752.The water based simulated sample was directly filtered,and the olive oil simulated sample was extracted with acetonitrile solution containing 38% methanol.The samples were separated on a C18 column with methanol-2 mmol/L ammonium acetate containing 0.1% formic acid as mobile phases,and analyzed under multiple reaction monitoring mode.The quantitation limits of the method for water based simulant（3% acetic acid,10% alcohol,50% alcohol）and olive oil simulant were 0.10 ng/mL and 1.0 ng/g,respectively.The spiked recoveries ranged from 85.3% to 110% with relative standard deviations（RSD）not more than 7.3%.This method was rapid,precise and convenient,and was appropriate for the determination of DOPO migration in plastic polymers.
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发布时间： - 摘要：In this paper,a label free C-reactive protein（CRP）photoelectricimmunosensor was constructed using porous porphyrin compound-Au nanoparticles（Au NPs@PAF）as an immobilized substrate.Under the optimal conditions,the CRP was quantitatively detected by chronograph current method.There was a good linear relationship for the sensor versus photocurrent in the range of 0.05-60 ng/mL,with a linear correlation coefficient of 0.994 6.The limit of detection was 0.017 ng/mL,and the average recovery was 102%.This sensor provided a sensitive method for the detection of C-reactive protein with good selectivity.关键词：porphyrin porous materials;photoelectric immunosensor;C-reactive protein;application
- 934
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发布时间： - 摘要：A method was established for the determination of 8 UV absorbents in soils and sediments by dispersive solid phase extraction combined with gas chromatography-tandem mass spectrometry（GC-MS/MS).50 g sample was extracted by mechanical oscillation method for 30 min after addition of 20 mL hexane-acetone（4∶1,by volume)and purification with 1.0 g SCX sorbent.After concentration by rotary evaporator,the extract was determined by GC-MS/MS and quantified by external standard method.Parameters such as extraction solvents,extraction times and types of sorbent were optimized.Results showed that there existed good linear relationships for the target compounds in the range of 2-150 μg/L with their correlation coefficients（r2) not less than 0.994 7.The detection limits of the method were from 0.077 ng/g to 0.226 ng/g.The average recoveries at three spiked levels ranged from 95.7% to 126% with the relative standard deviations（RSD,n=8)not more than 12%.This method was successfully applied in the analysis of UV absorbents in real samples.The results showed that the detection rate for UV-328 was the highest.The method is simple,accurate and sensitive,and is applicable for the determination of UV absorbents in different types of soil and sediment samples.关键词：gas chromatography-tandem mass spectrometry（GC-MS/MS);dispersive solid phase extraction;UV absorbents;soil and sediment
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发布时间： - 摘要：A poly neutral red modified glassy carbon electrode(PNR/GCE) was prepared by electropolymerization,and characterized by cyclic voltammetry(CV).The peak current in cyclic voltammogram as an indicator was used to investigate the effects of neutral red(NR) concentration,number of scanning segments,pH value of buffer and concentration of supporting electrolyte NaNO3 on the polymerization process.Subsequently,the optimum conditions for polymerization were selected.Then a new method for the rapid detection of antimicrobial efficacy in vitro was developed with NR as an electron mediator and E-coli as a model microorganism to investigate the relationship between activity of E-coli and concentration of antibacterials.The optimum conditions for electrode modification were as follows:concentration of neutral red:0.5 mmol/L,scan segment:30,buffer:pH 7.0,supporting electrolyte:0.5 mol/L NaNO3.The highest sensitivity for the detection of antibacterials efficacy was obtained when a final absorbance value(OD600 ) for bacterial suspension of 0.5,a standard glucose-glutamic acid solution(GGA,BOD220) as nutrition and an incubating time of 40 min were selected.Under the optimum experimental conditions,the half-inhibitory concentrations of cefoperazone,amikacin,gentamycin and levofloxacin on E-coli cells were 34.15,27.98,8.83 and 11.49 mg/L,respectively.However,vancomycin,as only an antibiotic affecting gram positive bacteria,showed a poor inhibition on E-coli cells.The results obtained above were in good agreement with those obtained by classical disk diffusion method.关键词：poly neutral red;modified electrode;electrochemical drug sensitivity test
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发布时间： - 摘要：An ultra high performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was developed for the simultaneous determination of tetrabromobisphenol A(TBBPA) and hexabromocyclododecane(HBCD) in aquatic products.Sample preparation was based on QuEChERS procedure.The target analytes in samples were extracted with acetonitrile，followed by a dispersive solid phase extraction clean up procedure using C18.Separation of TBBPA and HBCD isomers was achieved on a CORTECS- C18(4.6 mm×100 mm×2.7 μm) column with gradient elution using water-methanol as mobile phase at a flow rate of 0.7 mL/min.The MS/MS analysis was performed with electrospray ion source in negative mode under multiple reaction monitoring(MRM) mode.Good linearities for TBBPA and three HBCD isomers were achieved in the concentration range of 0.5-500 μg/L，with their correlation coefficients(r) above 0.998.The limits of detection(LOD) and the limits of quantitation(LOQ) were in the ranges of 0.04-0.16 μg/kg and 0.12-0.55 μg/kg，respectively. Recoveries at three spiked levels of 5，20 and 50 μg/kg ranged from 74.0% to 121%，with relative standard deviations(RSDs) of 0.20%-23%.The developed method was simple，rapid and reliable，and was suitable for the rapid determination of TBBPA and HBCD in aquatic products.关键词：tetrabromobisphenol A;hexabromocyclododecane;QuEChERS;ultra high performance liquid chromatography-tandem mass spectrometry;aquatic products
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发布时间： - 摘要：A new method of inductively coupled plasma-triple quadruple mass spectrometry（ICP-MS/MS） was developed for the determination of 14 trace rare earth metal and 4 trace other metal impurities in cerium chelate with ultrahigh purity.01 g sample was digested by low pressure autoclaves with 1 mL HNO3 for 30 min at 120 ℃.Under the MS/MS detection mode,typical strong poly atomic and overlapping interferences on La,Pr,Gd,Tb and Dy from the matrix of Ce were fully eliminated（about 2-3 orders of improvement in comparison with conventional detection modes）,when the O2 and NH3 based dynamic reaction cell（DRC） technique was used and a low ratio of 0.3% for CeO+/Ce+ was accomplished by using the high matrix introduction（HMI） sample introduction system；Similarly,isotopic and poly atomic interferences on Ca and Fe from Ar under high matrix concentration levels were successfully eliminated by using the cool plasma detection mode plus the H2 and He based DRC technique.Under the optimized detection conditions,a RSD with long term stability was less than 5%（2 h,4.0 g/L）,the recoveries of 926%-108% and the detection limits（3s） of 0.001 2-0.071 5 μg/g for all of the analytes were obtained,indicating that the method could be applied in the rapid batch analysis of cerium chelate with 6N purity.关键词：inductively coupled plasma-triple quadrupole mass spectrometry（ICP-MS/MS）;high pure cerium chelate;laser optical fiber;trace metal impurities
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发布时间： - 摘要：A carboxylated multi walled carbon nanotubes modified glassy carbon electrode（c-MWCNTs/GCE） was fabricated,and the electrochemical behavior of vanillin was studied in 0.5 mol/L HCl using cyclic voltammetry.Results revealed that the modified electrode showed an better electrocatalytic activity toward the oxidation of vanillin by a significant enhancement in the current response compared with that of the bare glassy carbon electrode.The oxidation of vanillin at this electrode was irreversible and diffusion controlled.Under the optimum conditions,by second order derivative linear scan voltammetry,the anodic peak current showed a linear relation versus vanillin concentration in the ranges of 0.1-6.0 μmol/L and 6.0-100 μmol/L with a detection limit（S/N=3）of 0.02 μmol/L.Moreover,the modified electrode demonstrated a good reproducibility（RSD=4.6%） and a long term stability.This method was applied in the determination of vanillin in food samples with recoveries of 96.3%-104%.关键词：carboxylated multi-walled carbon nanotubes(c-MWCNTs);vanillin;electrochemical behavior;voltammetric determination
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发布时间： - 摘要：A capillary electrochromatography with covalent porous organic cage chiral material（CC3-R） was developed for the separation of mandelic acid.The single CC3-R with three dimensional diamond network channel was synthesized,and used as a chiral stationary phase to prepare a capillary electrochromatography column.The chiral recognition performance for CC3-R capillary electrochromatography column was investigated.The variations of current with voltage and electroosmotic flow with pH value of buffer solution were measured,and then this column was used to separate mandelic acid.Results showed that the baseline separations for D-mandelic acid and L-mandelic acid were obtained with the degree of separation of 1.81,and the numbers of theoretical tray for them both were 36 700 N/m and 41 600 N/m,respectively.The retention time of mandelic acid on the same CC3-R capillary column was observed with the relative standard deviation of 1.2%.Results showed that the CC3-R chiral column not only has a good chiral recognition ability,but also has good stability and reproducibility.关键词：capillary electrochromatography;porous organic cage;chiral separation
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发布时间： - 摘要：An ultra performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was established for the determination of aflatoxins（AFB1,AFB2,AFG1 and AFG2）in aquatic feeds based on multi-component immunoaffinity column purification.The samples were ultrasonically extracted with 80%acetonitrile aqueous solution,then purified with a multi-component immunoaffinity column,finally analyzed by UPLC-MS/MS with electrospray ionization in positive ion mode（ESI+）under multiple reaction monitoring（MRM）mode and quantified by the external standard method.The separation was performed on an Acquity UPLC BEH C18 column by gradient elution with 0.1%formic acid-acetonitrile as mobile phases.Good linear responses were obtained in the concentration ranges of 2.25-22.5 ng/mL for AFB1 and AFG1,and 0.75-7.5 ng/mL for AFB2 and AFG2,with their correlation coefficients larger than 0.997,respectively.The limits of quantitation（LOQs） were 0.7 μg/kg for AFB1 and AFG1,and 0.2 μg/kg for AFB2 and AFG2,respectively.The average recoveries for AFB1 and AFG1 at a spiked level of 1.5 μg/kg,and AFB2 and AFG2 at a spiked level of 0.5 μg/kg ranged from 78.7%to 85.5%,with intra-day and inter-day relative standard deviations of 6.0%-6.5%and 6.6%-7.0%,respectively.The method was simple,rapid,sensitive and reliable,and was suitable for the determination of aflatoxins residues in aquatic feed samples.关键词：multi-component immunoaffinity column;ultra performance liquid chromatography-tandem mass spectrometry;feeds;aflatoxins
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发布时间： - 摘要：A surface enhanced Raman spectroscopy（SERS） combined with chemometrics algorithms was established for the quantitative detection of aspartame（APM） in soft drinks based on the application of ultrasonography.The sample was detected using nano silver as active substrate,with a nano silver to APM ratio of 1∶1 at pH 5.0,a mixing temperature of 30 ℃ and a heating time of 6 min.A quantitative analysis mode was set up by using the monadic linear regression method to analyse SERS spectra.Results showed that the calibration curves were linear in the range of 0.5-100 mg/L.The correlation coefficient was 0.993 3 and the detection limit（LOD）was 0.41 mg/L for APM standard.The correlation coefficients of standard solutions in Soda water,Sprite,Coke and Fanta ranged from 0.974 7 to 0.984 8.Furthermore,the average recoveries ranged from 88.4% to 121% with relative standard deviations less than 7%.Detection of APM in soft drinks by SERS has the advantages of fast analysis,nondestructive and low environmental pollution,which indicates that SERS technology is suitable for quantitative analysis of APM in food and has great potential of applying in the determination of chemical substances.
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发布时间： - 摘要：A liquid chromatography-tandem mass spectrometric（LC-MS/MS） method was developed for the quantitative determination of aflatoxin B1（AFB1）,aflatoxin M1（AFM1）,T-2 toxin（T-2）,HT-2 toxin（HT-2）,deoxynivalenol（DON）,ochratoxin A （OTA） and zearalenone（ZEN） in shrimp feed.Samples were extracted with 15 mL acetonitrile-water（4∶1,by volume）,and degreased with 10 mL acetonitrile saturated hexane.The extract was cleaned up with a MycoSpinTM400 multitoxin LC-MS/MS clean-up column.The target compounds were separated on an Hypersil Gold（150 mm×2.1 mm,5 μm）chromatographic column by gradient elution with methanol-water containing 0.03%ammonia as mobile phase,and analyzed simultaneously by electron spray ionization mass spectrometry in positive or negative ion mode,and quantified by the matrix-matched external standard method.Under the optimized conditions,there were good linearities for the analytes in corresponding concentration range with their correlation coefficients（r2） more than 0.991.The limits of detection（LOD）ranged from 1.83 μg/kg to 12.63 μg/kg.Average recoveries for the target mycotoxins at high,medium and low spiked levels ranged from 87.5%to 116%with relative standard deviations of 2.4%-18%.The developed method could provide a reference for the simultaneous determination of mycotoxins in aquatic feeds.关键词：mycotoxin;liquid chromatography-tandem mass spectrometry（LC-MS/MS）;feed
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发布时间： - 摘要：An ultra-sensitive electrochemical sensor for detection of ascorbic acid（AA)was constructed by drop casting method with electrochemical sensing interface.Multi-walled carbon nanotubes （MWCNTs) and graphene oxide（GO) preventing the aggregation of MWCNTs were first added to the surface of glassy carbon electrode（GCE) to form a film.Subsequently,gold platinum core-shell nanoparticles（Au@Pt NPs) were immobilized on the surface of GO/MWCNTs/GCE through layer by layer assembly,forming a GO/MWCNTs/Au@Pt NPs/GCE 3D composite film.The as prepared electrode was used in the electrochemical detection of AA in phosphate buffer solution by differential pulse voltammetry（DPV) with a wide linear range and very low detection limit.There were good linear relationships between the redox peak current and AA in ranges of 0.005-0.5 μmol/L and 0.5-1 000 μmol/L,respectively,with their correlation coefficients of 0.999 and their detection limits（S/N=3) of 4.0×10-9 mol/L.The recoveries for the real human serum sample at three spiked levels of 0.01,0.1 and 10 μmol/L were in the range of 90.9%-108%,with the relative standard deviations（RSD,n=3)of 1.2%-2.8%.With a good selectivity toward AA,the sensor could effectively eliminate any interferences from small biological molecules such as dopamine,uric acid and glucose,etc.Therefore,the sensor is simple,efficient and sensitive,and could be widely used in clinical detection.关键词：electrochemical detection;ascorbic acid;multi walled carbon nanotubes;graphene oxide;gold platinum core-shell nanoparticles
- 977
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发布时间： - 摘要：Based on the surface of nickel foam electrode（Ni foam)with high specific surface area,a carbon nanotubes（CNTs)/Ni foam was prepared through the electrodeposition of CNTs.With the help of cetyltrimethylammonium bromide（CTAB),horseradish peroxidase（HRP)was immobilized onto the surface of CNTs/Ni foam by one-step electrodeposition of Au nanoparticles（AuNPs),and an HRP-AuNPs/CNTs/Ni foam direct electrochemical enzyme sensor was prepared.SEM,electron dispersive spectroscopy（EDS)and electrochemical methods were adopted to characterize the modified electrode,and the test conditions for pH value and work potential were also optimized.The sensor was applied in the detection of hydrogen peroxide and two organic peroxides.Results showed that the sensor has a good catalytic detection performance toward hydrogen peroxide,cumene hydroperoxide and 2-butanone peroxide with the detection limits of 1.2×10-7,4.5×10-7 and 2.5×10-7 mol/L,respectively.关键词：peroxides;horseradish peroxidase;carbon nanotubes;sensor
- 927
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发布时间： - 摘要：A novel “turn on” fluorescence sensor for H2O2 detection was developed based on boron and phenyl doped graphitic carbon nitride nanosheets(BP-C3N4) as peroxidase mimic.The BP-C3N4 with peroxidase-like activity were prepared by thermal polymerization of cyanamide with 3-aminobenzeneboronic acid followed by ultrasonic exfoliation.Similar to horseradish peroxidase，the BP-C3N4 could catalyze the oxidation of amplex ultrared reagent(AUR) by H2O2 to generate the resorufin with strong fluorescence.Parameters for the peroxidase like catalytic reaction，including response time，pH value and temperature were further investigated.Under the optimal conditions，the obtained fluorescence signal showed a good linear response to H2O2 concentration over the range of 0-100 μmol/L，with a correlation coefficient(r2) of 0.992 2 and a limit of detection of 1.1 μmol/L.The fluorescence sensor was applied in the detection of H2O2 residue in real samples，and the results were consistent with those of the existed method.关键词：graphitic carbon nitride;codope;peroxidase mimic;H2O2;fluorescence sensor
- 951
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- 3
发布时间： - 摘要：1H nuclear magnetic resonance（1H NMR） spectroscopy combined with chemometrics was developed for the identification and classification of Chinese honey of different floral origins.33 acacia honeys,48 rape honeys and 63 lychee honeys were analyzed by NMR,and the NMR data were preprocessed in different modes.Supervised partial least squares discriminant analysis（PLS-DA） and orthogonal partial least squares discriminant analysis（OPLS-DA） were both used to set up discriminant models by extracting the useful information from NMR signals.Results showed that different data preprocessing methods have significant influences on the interpretation and prediction abilities of the models,and the unit variance（UV） scaling was more suitable for the analysis of honey NMR data than the others.The OPLS-DA model could effectively discriminate three kinds of honey of different floral origins.The explanation and prediction abilities based on the OPLS-DA model were 95.8% and 90.5%,respectively.Therefore,1H NMR spectroscopy combined with chemometric could effectively realize the rapid and accurate identification of Chinese honeys of different floral origins.关键词：1H nuclear magnetic resonance technology（1H NMR）;chemometrics method;honey;floral origins identification
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发布时间： - 摘要：A simple fluorescence analytical method was established for the quantitation of activity of β-glucosidase.The synthetic 2-O-β-glucopyranosyl ascorbic acid(AA-2βG) was used as the enzymatic substrate.β-Glucosidase catalyzed the hydrolysis reaction and released ascorbic acid,which would reduce non fluorescent resazurin to strongly fluorescent resorufin.Thus,β-glucosidase activity would be reflected by the fluorescent intensity variation of the system.Firstly,a validation assay was carried out to confirm the possibility to detect ascorbic acid taking advantage of reductive reaction.There was a linear relationship for the increased fluorescent intensity with the concentration of ascorbic acid in the range of 3-400 μmol/L with a correlation coefficient(r2) of 0.981,while β-glucosidase activity was successfully determined by measuring fluorescent intensity at 585 nm.Results showed that there also existed a good linear relationship between the increased fluorescent intensity and concentration of β-glucosidase in range of 1-30 U/L,with a correlation coefficient(r2) of 0.995 and a detection limit of 1.0 U/L.With the characteristics of simplicity,sensitivity and large detection range,the method could realize the quantitative detection on β glucosidase activity.关键词：β-glucosidase activity;resazurin;resorufin;ascorbic acid;fluorescence;determination
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发布时间： - 摘要：Magnetic labeling detection technology based on magnetic nanomaterials has the advantages of high sensitivity，wide linear range and easy operation，while the traditional labeling detection technology based on optical label usually could achieve qualitative detection or semi quantitative detection only.Most biological samples have low magnetic signal，leading to low background interference.Therefore，the magnetic labeling detection technology has shown higher sensitivity than optical labeling detection technology.It could not only carry out quantitative detection，but also reduce the pretreatment time.Point of care testing(POCT) could be performed at or near the sites of patient care，which is the trend of medical diagnosis.Magnetic labeling detection technology has an application potential in POCT，especially in biomedical use，such as detecting protein，nucleic acid，cell，pathogens and biological tissue.The latest research progress of magnetic nanoparticles in POCT is focused in this paper，and their applications in detecting protein，nucleic acid and several kinds of pathogens are discussed.Finally，the development direction and application prospect of POCT technology based on magnetic nanoparticles are outlined.关键词：magnetic nanoparticles;quantitative detection;biomedical diagnostics;point of care testing;superparamagnetism
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发布时间： - 摘要：Microcystin（MC）,a type of small molecule polypeptide biotoxin produced by algal blooms,is high toxic to humans and animals,and has been classified as a potential human carcinogen（Group 2B）.Algal blooms break out more and more frequently and tempestuously due to the large discharge of worldwide industrial and domestic wastewater and the climate warming worldwide,which caused the massive accumulation of MCs in water-bodies and soil,threatening the ecological environment and affecting the quality and safety of agricultural products.The immunoassay based on “antibody-antigen” recognition principle is a hot spot research in the rapid determination of biotoxins.The antibody preparation technology is developing in leaps and bounds in the late years,and now has been developed from traditional polyclonal antibody and monoclonal antibody to novel genetic engineering artificial antibody.The internal and external factors of microcystin production,and major hazards toward ecosystem,humans and animals are expounded systematically in the present paper,and the latest research progress of novel artificial antibody preparation technologies and their applications in MC-LR determination are combed comprehensively.Finally,combined with our latest research results,the development trend,existing problems and solutions of novel artificial antibodies in MC-LR determination are further discussed.关键词：genetically engineered antibody;microcystin;agricultural products;quality and safety;immunoassay
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