最新刊期
卷 36 ， 期 9 ， 2017
- 摘要：A scheme was presented for the tandem purification of phosphopeptide using desalting prior to immobilized metal ion affinity chromatography(IMAC).Both C18 tip and the cerium(Ⅳ)-modified chitosan material(Ce-MCM) were used in the desalting experiments.GMA-co-SR454/Iron(Ⅲ)-IDA was synthesized,and used as an excellent phosphopetides enrichment material.They were applied to selectively capture the phosphopeptides in standards and human serum.Results demonstrated that C18/IMAC and Ce-MCM/IMAC have different performances because of their hydrophobic or hydrophilic properties.Ce-MCM/IMAC tandem strategy notably decreased the complexity of peptides,and yielded a far greater coverage for phosphopeptides than single IMAC.关键词：desalting;IMAC;matrix-assisted laser desorption-ionization time of flight mass spectrometry(MALDI-TOF MS);phosphopeptides;tandem enrichment
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发布时间： - 摘要：An HPLC-ECD method was established for the determination of five neurotransmitters in cerebral tissues of rats to discuss the protective effects of alltride(DAS) on the monoamine neurotransmitters(MNTs) in paraquat(PQ) poisoning rats brain tissues. Male ICR rats were divided into four groups(n=6) according to their different treatments. The paraquat(PQ) group and the treatment(PQ+DAS) group exposed to 35mg/kg PQ i.g.. The control group and the alltride(DAS) group were given the same volume of sterile saline. The alltride(DAS) group and treatment group were administrated with 25mg/kg DAS i.p. after PQ was given intragastrically for 2,26,50 h.PQ group and normal group rats were injected with the same amount of sterile saline. The determination was performed on an Acclaim 120 C18 column with a mobile phase consisted of buffer salt(sodium citrate,monopotassium phosphate,sodium heptanesulfonate,EDTA-2Na,diethylamine hydrochloride )-methanol(93∶7,by volume) at a flow rate of 0.27mL/min,and the voltage of electrode was set at 450mV.Compared with the normal or DAS group，the PQ group showed significant decreases in the quantities of DA and 5-HT.The combination of PQ and DAS resulted in higher amounts of neurotransmitters than that of the administration with PQ alone(P<0.05).The spiked recoveries were in the range of 79.8%-112.1% with RSDs lower than 10%.DAS could prevent rats from the PQ-induced decrease of the neurotransmitters, which may be associated with its abilities to relieve oxidative damages.关键词：HPLC-ECD;paraquat;alltride;monoamine neurotransmitters
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发布时间： - 摘要：Using graphene sheet(GS) as a matrix connecting bovine serum albumin to label microcystins(MCLR)(BSA-MCLR),an electrochemical immunosensor was developed for the determination of MCLR with AuNPs as a signal probe. Scanning electron microscopy(SEM), transmission electron microscopy(TEM) and UV-Vis absorption spectroscopy were used to characterize the synthetic nanomaterials. Cyclic voltammetry was used to investigate the electrochemical properties of the modified electrodes. Analyte MCLR was competitively combined with immobilized BSA-MCLR to form anti-MCLR. After the immune reaction, AuNPs were electrochemically oxidized into AuCl4- at a constant potential. Then the AuCl4- ions were reduced into Au with the peak current as the detecting signal via cathodic potential scan of differential pulse voltammetry(DPV). Under the optimal conditions, the linear range was from 0.1μg/L to 50μg/L with a detection limit of 0.05μg/L. The reproducibility, stability and selectivity of the immunosensor were investigated．Compared with the enzyme-labeled probes, the AuNPs labeled probe could have the determined process finished with low cost, high stability and excellent detection result.关键词：AuNPs signal probe;graphene;microcystins;immunosensor
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发布时间： - 摘要：A novel polymer porous layer stationary phase containing the copolymer of glycidyl methacrylate and ethylene glycol dimethacrylate（GMA-EDMA） was fabricated, and applied as a porous layer open tubular capillary（PLOT） column.To obtain a suitable capillary for electrochromatography,various conditions including the polymerization time,the ratio of n-propanol/1,4-butanediol and GMA/EDMA in the polymerization mixture were optimized.Scanning electron microscopy demonstrated a nearly uniform polymer porous layer on the inner wall of the open tubular capillary column.In the capillary electrochromatographic mode,the PLOT column provided the reasonable separation of neutral,acidic and basic small molecules based on a reversed phase mechanism.After immobilizing the chiral selector human serum albumin（HSA）,the HSA-PLOT column performed a better chiral recognition for five pairs of enantiomers compared with the single-layer polymer coated open tubular capillary column modified with HSA.The intra-day, inter-day and column-to-column relative standard deviations for alkylbenzenes separated on the PLOT column were less than 1.7%,4.8% and 7.8%,respectively.关键词：porous layer open tubular capillary column;capillary electrochromatography;human serum albumin（HSA）;chiral separation
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发布时间： - 摘要：The interaction between Rhodamine B and calf thymus DNA（ct-DNA） at physiological conditions were studied by the techniques of absorption spectroscopy, fluorescence spectroscopy and confocal imaging. The results of spectroscopy experiments suggested that the hypochromicity of Rhodamine B could appear in the presence of ct-DNA from 450nm to 650nm in the absorption spectroscopy, and the fluorescence of Rhodamine B was quenched in the presence of ct-DNA from 560nm to 660nm in the fluorescence emission spectroscopy. At the same time，the fluorescence polarization of Rhodamine B varied with the addition of ct-DNA.It was indicated that Rhodamine B could interact with ct-DNA. In the competition experiments, Rhodamine B was unable to replace methylene blue（MB） from MB-ct-DNA complex. It was indicated that the interaction between Rhodamine B and ct-DNA took place by the mode of groove combination. The results of confocal imaging experiments showed that the fluorescence of Rhodamine B was quenched quite obviously after the addition of ct-DNA. HeLa cells were dyed with Rhodamine B and 4′,6-diamidino-2-phenylindole（DAPI）,then used for confocal imaging. It was further verified that the cell nucleus could be dyed red through the groove combination interaction between Rhodamine B and ct-DNA.关键词：rhodamine B;ct-DNA;groove combination;spectroscopy;confocal imaging
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发布时间： - 摘要：A simultaneous method was developed for the analysis of 28 free amino acids using ultrahigh performance liquid chromatography-quadrupole/orbitrap high resolution mass spectrometry with pre-column derivatization,and was used to detect the free amino acids in cruciferous plants.The samples were extracted using ultra pure water,and derivatized with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate(AQC) to enhance chromatographic retention.A Waters BEH C18 column was used as stationary phase.Ammonium acetate solution(pH 5.0) and 80% acetonitrile in water were applied as mobile phases for gradient elution.MS detector with electrospray ion source worked in positive ion mode.The results showed that there were more than 25 kinds of free amino acids in cruciferous plants,including 8 essential amino acids.All calibration curves of the analytes exhibited good linearity.The average recoveries of this method ranged from 80.5% to 104.4% with the relative standard deviations of 0.6%-4.4%.The sensitivities of amino acids were different,and the quantitation limit was between 0.01 μmol/L and 1.45 μmol/L.With the advantages of little impurity interference,rapidness and high sensitivity,the method is suitable for the simultaneous detection of free amino acids in plant samples.关键词：ultra-high performance liquid chromatography;high resolution mass spectrometry;free amino acids;cruciferous vegetables
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发布时间： - 摘要：In this study,double pulse laser induced break down spectroscopy(LIBS) technique was used to detect the content of fenthion in solution.The spectra of different concentrations’ samples in range of 206.28-481.77 nm band were collected using a two channel spectrometer with high precision.And then several preprocessing methods such as multiplicative scatter correction(MSC),standardized normal variate(SNV) and 3 point smoothing were conducted on the spectra.The optimal pretreatment method was confirmed according to partial least square(PLS) modeling.On this basis,competitive adaptive reweighted sampling(CARS) was used to screen the important variables related to fenthion.Then,the quantitative analysis model for fenthion in solution was established by PLS regression.Finally,the CARS-PLS quantitative analysis model was compared with the single variable quantitative analysis model and the PLS quantitative analysis model without variable selection.The results indicated that the CARS-PLS quantitative analysis model has a better performance compared with single variable quantitative analysis model and PLS model,and its determination coefficient and average relative error of calibration set and prediction set are 0.969 4,15.537% and 0.995 9,5.016%,respectively.Furthermore,the CARS-PLS model adopted only 1.9% of the wavelength variables,but the average error of the prediction set was decreased from 9.829% to 5.016%.Thus it is found that LIBS technology has a certain feasibility to detect the content of fenthion in solution.And CARS could simplify the quantitative analysis model and improve the prediction accuracy of the model.关键词：laser induced breakdown spectroscopy;partial least square;competitive adaptive reweighted sampling;fenthion
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发布时间： - 摘要：A gas chromatography-mass spectrometric(GC-MS) method was developed for the determination of karanal and its isomers in detergents.Samples were extracted with methanol through ultrasonic method.The target ingredients were separated on a DB-5MS column(30 m×0.25 mm×0.25 μm) and analyzed with MS under scan mode(SCAN).Gas chromatography was used to confirm the proportion of karanal and its isomers in standard solution.The linear equations of karanal and its isomers were set up between 5 mg/L and 100 mg/L.The limits of quantitation were 0.25 mg/g.The recoveries ranged from 97.4% to 111.5%,with relative standard deviations(RSDs,n=6) of 3.7%-7.2%.This method was rapid,accurate and convenient to operate,and it was appropriate for the determination of karanal and its isomers in detergents in routine tests.关键词：detergents;karanal;isomer;gas chromatography-mass spectrometry(GC-MS)
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发布时间： - 摘要：To solve the time-consuming problem of traditional detective methods,such as total viable counts and ATP bioluminescence technique,and the complicated operations of the existing spectrum techniques,a method for the quantitative analysis of the total number of bacteria in milk by UV-Vis spectroscopy combined with chemometrics,followed by application of the optimized partial least squares to set up the model of the total amount of milk bacteria.With the milk cultured in the same time period(0，2，4，…，20 h) as target,the quantitative relationship between the spectrum and the total number of milk bacteria was explored.The successive projections algorithm was applied to select 19 characteristic waves,and then the partial least squares model was used to establish the model relationship between the characteristic waves and the total number of milk flora.The correlation coefficient R of 0.978 in the optimized model was higher than that of 0.968 in primitive model,and the root mean square error(RMSE) of 0.265 in the optimized model was lower than that of 0.324 in the primitive model.The proposed method provided a new idea and direction for the rapid detection of the number of milk flora.
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发布时间： - 摘要：An amperometric glucose oxidase(GOx) biosensor based on gold nanoparticles(AuNPs) -reduced graphene oxide(rGO) was fabricated for the detection of glucose in beverages.AuNPs-rGO composite was synthesized by one-pot method with chitosan as reducing and stabilizing agent.It was used as the matrix for GOx immobilization via physical adsorption technique to fabricate the GOx-based biosensor.The biosensor was applied in the amperometric determination of glucose at -0.45 V(vs.Ag/AgCl) in a phosphate buffer (0.1 mol/L，pH 6.0).There was a linear response to glucose in the concentration range of 0.01-0.88 mmol/L,with a sensitivity of 22.54 μA?mmol-1?L?cm-2 and a detection limit of 1.01 μmol/L.The apparent Michaelis-Menten constant was rather small(0.497 mmol/L).The constructed biosensor was successfully applied in the detection of glucose in beverages.关键词：gold nanoparticles;reduced graphene oxide;glucose oxidase;amperometric determination;beverage;glucose
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发布时间： - 摘要：A method was developed for the simultaneous determination of carbon monoxide，carbon dioxide and three light hydrocarbons i.e.methane，ethylene and acetylene in air by gas chromatography.The GC system consisted of auto-injection，one ten-port valve together with a six port valve and one ten-port valve in series with a four-port valve.Sample injection，column isolation and column back-flushing were realized in this way mentioned.An HP-PLOT Q open tubular capillary column was employed for the separation of the five gases followed by thermal conductivity detection.After the separation was completed，carbon monoxide and carbon dioxide were converted into methane with the use of a nickel-based methanizer for the detection by flame ionization.Separation of all the target analytes was achieved in one single analysis within 9 min.Carbon monoxide，methane，carbon dioxide，ethylene and acetylene were found to be linear over the ranges of 3.3-4 990.0，3.3-5 010.0，6.6-4 990.0，4.2-5 080.0,3.9-5 030.0 μmol/mol，respectively.The correlation coefficients were not less than 0.997 with the detection limits of 1.0-2.0 μmol/mol.Reproducibility of two levels，namely std1 and std2 were found to be not more than 3.5%(n= 5).This method was simple，accurate and maneuverable.关键词：greenhouse gas;open tubular capillary columns;gas chromatography;air;ethylene;acetylene
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发布时间： - 摘要：In this paper,the poly(3-amino-5-mercapto-1,2,4-triazole)/multi-walled carbon nanotubes modified glassy carbon electrode(pTA/MWCNTs/GCE) was successfully prepared by electrodepositing 3-amino-5-mercapto-1,2,4-triazole(TA) on the MWCNTs/GCE.The electrochemical behaviors of uric acid(UA),xanthine(XA) and hypoxanthine(HX) at the pTA/MWCNTs/GCE were investigated using cyclic voltammetry(CV) and differential pulse voltammetry(DPV).The results showed that the chemically modified electrode displayed excellent electrochemical catalytic activities towards UA,XA and HX.The calibration curves for UA,XA and HX were obtained over the ranges of 9.0-739.0，2.0-259.0,1.0-353.0 μmol/L with the detection limits of 0.67，0.17,0.33 μmol/L,respectively.In addition,the modified electrode was applied in the determination of UA,XA and HX in real samples(urine and serum),with the recoveries of the samples ranged between 98.8%-105.5%.关键词：multi-walled carbon nanotubes;3-amino-5-mercapto-1,2,4-triazole;uric acid;xanthine;hypoxanthine;electrochemistry
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发布时间： - 摘要：A rapid analytical method was developed for the determination of ibuprofen arginine by contactless conductivity detection with microfluidic chip.Influence parameters on separation and detection such as type and concentration of buffer,additive,separation voltage and injection time were investigated and optimized.Under the optimum conditions,i.e.20 mmol/L Tris-20 mmol/L H3BO3(pH 8.6)as buffer solution,no additive,a separation voltage of 2.0 kV and an injection time of 10.0 s,ibuprofen arginine could be separated and detected within 45.0 s.The results showed that good linearities for ibuprofen and arginine existed in 80.0-1.00×103 mg/L,with their correlation coefficients(r)of 0.998 and 0.997,respectively．The limits of detection(S/N=3)for them were 60 mg/L with RSDs of 1.9%and 1.8%，respectively.And their recoveries were in the ranges of 97.9%-103%and 97.3%-102%，respectively.This method was rapid and simple，and could be used for the detection and quality control of non-steroidal arginine ibuprofen anti-inflammatory drugs.关键词：microfluidic chip;contactless conductivity detection;arginine ibuprofen tablets;arginine ibuprofen granulesmicrofluidic chip;arginine ibuprofen granules
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发布时间： - 摘要：A method was established for the rapid determination of 11 algal toxins in sediments by ultra performance liquid chromatography - tandem mass spectrometry.Firstly，the sample was freezingly dried out，and then sieved，followed by purification with 0.1 mol/L EDTA-Na4P2O7 solution and HLB solid phase extraction column，elution with methanol-0.2% formic acid，and finally concentrated and mixed with nitrogen to 1 mL.The separation of the analyte was performed on a Waters BEH C18 chromatographic column with acetonitrile -0.2% formic acid solution as mobile phase by gradient elution.The sample was analyzed by ultra performance liquid chromatography-tandem mass spectrometry in positive ions electrospray mode under multi-stage monitoring mode (MRM)，and quantified by external standard method.The results showed that the detection limits for 11 algal toxins in sediment were in the range of 1.0-5.0 ng/kg.The average recoveries for the same environmental samples at three spiked concentrations of 0.1，1.0，4.0 μg/kg were in the range of 70.3%-112.5% with relative standard deviations of 2.2%-9.3%.The method was rapid，sensitive and accurate，and could be effectively applied in the rapid monitoring of 11 algal toxins in sediments.A method was established for the rapid determination of 11 algal toxins in sediments by ultra performance liquid chromatography - tandem mass spectrometry.Firstly，the sample was freezingly dried out，and then sieved，followed by purification with 0.1 mol/L EDTA-Na4P2O7 solution and HLB solid phase extraction column，elution with methanol-0.2% formic acid，and finally concentrated and mixed with nitrogen to 1 mL.The separation of the analyte was performed on a Waters BEH C18 chromatographic column with acetonitrile -0.2% formic acid solution as mobile phase by gradient elution.The sample was analyzed by ultra performance liquid chromatography-tandem mass spectrometry in positive ions electrospray mode under multi-stage monitoring mode (MRM)，and quantified by external standard method.The results showed that the detection limits for 11 algal toxins in sediment were in the range of 1.0-5.0 ng/kg.The average recoveries for the same environmental samples at three spiked concentrations of 0.1，1.0，4.0 μg/kg were in the range of 70.3%-112.5% with relative standard deviations of 2.2%-9.3%.The method was rapid，sensitive and accurate，and could be effectively applied in the rapid monitoring of 11 algal toxins in sediments.A method was established for the rapid determination of 11 algal toxins in sediments by ultra performance liquid chromatography - tandem mass spectrometry.Firstly，the sample was freezingly dried out，and then sieved，followed by purification with 0.1 mol/L EDTA-Na4P2O7 solution and HLB solid phase extraction column，elution with methanol-0.2% formic acid，and finally concentrated and mixed with nitrogen to 1 mL.The separation of the analyte was performed on a Waters BEH C18 chromatographic column with acetonitrile -0.2% formic acid solution as mobile phase by gradient elution.The sample was analyzed by ultra performance liquid chromatography-tandem mass spectrometry in positive ions electrospray mode under multi-stage monitoring mode (MRM)，and quantified by external standard method.The results showed that the detection limits for 11 algal toxins in sediment were in the range of 1.0-5.0 ng/kg.The average recoveries for the same environmental samples at three spiked concentrations of 0.1，1.0，4.0 μg/kg were in the range of 70.3%-112.5% with relative standard deviations of 2.2%-9.3%.The method was rapid，sensitive and accurate，and could be effectively applied in the rapid monitoring of 11 algal toxins in sediments.关键词：sediments;algal toxin;ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)
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发布时间： - 摘要：A novel styrene-divinylbenzene copolymer monolithic capillary column was prepared using dimethylsulfoxide/dodecanol as binary porogenic agent.The polymer was prepared with styrene as monomer,divinylbenzene as crosslinker,benzoperoxide as initiator.In order to optimize the properties,the contents of the polymerized mixtures were investigated.Key variables such as composition of porogenic agent and crosslinking degree and content of porogenic agent in the mixtures could be controlled easily during the on-column polymerization.The PS-DVB monolithic column was characterized by scan electric microscopy(SEM),inverse size exclusion chromatography(ISEC),and measured under back pressure at different flow rates to evaluate the porous properties.Homologous compounds of benzene and some proteins were used as objective probes in reverse phase chromatography mode for evaluating the separation performance of the synthesized column.The optimum preparation conditions were as follows:the volume ratio of styrene and divinylbenzene and dimethylsulfoxide and dodecanol was 18.7∶15.3∶13.2∶52.8,that is,the content of dimethylsulfoxide in binary porogenic agent occupied 20%,the degree of crosslinking tooked up to 45% and the content of binary porogenic agent reached to 66%.The flow rate reached to 104 μL?min-1 in the experiment for the separation of protein,and the line speed was about 12 mm?s-1,while the conventional speed was about 1-2 mm?s-1.With the advantage of excellent chromatographic separation efficiency for biological macromolecules,the monolithic capillary column could be available in other separation modes if it is chemically modified.
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发布时间： - 摘要：The enzyme-free detection of glucose was achieved by using the nano-copper/graphene-chitosan composite matrix modified glass carbon electrode.The microstructure of the composite matrix was characterized by scanning electron microscopy(SEM),FT-IR spectrum and electrochemical impedance spectroscopy(EIS).The electrochemistry behavior of the modified electrode was investigated by cyclic voltammetry and chronoamperometry.The results showed that the modified electrode exhibited a good catalytic oxidation of glucose in 0.1 mol/L NaOH and with a wide linear range of 5.6×10-5-1.2×10-3 mol/L and a low detection limit of 2.3×10-5 mol/L(at signal/noise ratio S/N = 3).The modified electrode could be used to detect the real samples with a good stability and repeatability.关键词：nano-copper;graphene-chitosan composite membrane;modified electrode;glucose
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发布时间： - 摘要：The cataluminescent(CTL) phenomenon in the reaction of hydrogen sulfide on nano-MgO surface was studied.It was found that nano-MgO showed a good specificity towards hydrogen sulfide,a CTL sensor for hydrogen sulfide was developed on the basis of this phenomenon,then a rapid method for the detection of hydrogen sulfide was proposed after optimal design.The linear range for this method was 2.00-200 ppm(r=0.999 3),and the detection limit was 0.8 ppm at a signal to noise ratio(S/N) of 3.The sensor was applied in the spiked analysis of the artificial samples containing hydrogen sulfide with the recoveries between 88.4% and 97.2%.With the advantages of sensitivity,rapidness and easy operation,the sensor showed an application potential in the rapid detection of hydrogen sulfide.The possible CTL reaction mechanism of hydrogen sulfide was also discussed.关键词：hydrogen sulfide;cataluminescence;sensor;Nano-magnesium oxide
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发布时间： - 摘要：Gold nanoclusters were synthesized based on oxidized glutathione(GSSG) with a mean diameter of 2.9 nm.The fluorescence of GSSG-Au NCs was strongly quenched when Fe3+ ions were present.The sensor was used to detelt Fe3+ ions has a wide linear range of 0.1-30 μmol/L,a high sensitivity of 0.03 μmol/L and a good selectivity.The method described was successfully applied in real sample(tap water,lake water and river water samples) determination.关键词：gold nanoclusters(Au NCs);oxidized glutathione(GSSG);fluorescent probe;Fe3+
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发布时间： - 摘要：Graphene(G) is an efficient adsorbent in many fields,which composes of a two-dimensional monolayer with a honeycomb-like aromatic structure.It possesses a great specific surface area and a huge π-π conjugated system.However,the stable chemical property,indissolubility with solvents and the strong π-π interaction between the layers,lead to the irreversible agglomerates of G in aqueous solution and restrict its further application.G could be composited with some other materials such as polypyrrole,polymeric ionic liquids,Fe3O4@SiO2 ,etc.G composites could not only improve the dispersion of G in solution,but also give some novel characteristics to the composites.In this paper,the preparation of G composites by chemical or physical methods was summarized.The adsorption performances of G composites as adsorbents for environmental pollutants including pesticide residues,benzene derivatives,organic dyes and heavy metal ions was reviewed.Besides,the future development trends of G composites as adsorbents were also discussed.关键词：graphene composite;adsorbent;preparation;environmental pollutants;review
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发布时间： - 摘要：The research progress on pretreatment technologies in determination of phenolic compounds in edible vegetable oil and oilseeds was mainly summarized,such as liquid-liquid extraction,ultrasonic-assisted extraction,microwave-assisted extraction,supercritical fluid extraction,solid phase extraction and magnetic solid phase extraction.Advantages and disadvantages of these technologies were compared and analyzed.The trends and future perspectives of pretreatment technologies for phenolic compounds in edible vegetable oil and oilseeds were also discussed.关键词：edible vegetable oil;oilseeds;phenolic compounds;pretreatment;review
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