最新刊期
卷 34 ， 期 10 ， 2015
- 摘要：Three types of magnetic nanopaticles(CoFe2O4，Fe3O4 and CuFe2O4) were prepared by a simple solvothermal reaction and used to remove biological contaminant microcystin-LR in water.Concentrations of microcystin-LR were detected by high performance liquid chromatography(HPLC).CoFe2O4 showed the best adsorption ability for biological contaminant microcystin-LR.Transmission electron microscope,FT-IR,magnetization curve and X-ray diffraction were used to structurally characterize CoFe2O4 nanopaticles which were evaluated to be magnetizable and distributedly homogeneous,with a diameter of about 250 nm.CoFe2O4 nanopaticles and the adsorbed toxin could be separated conveniently from solution with the help of an applied magnetic field.Factors influencing the adsorption capacity including microcystin-LR concentrations,pH conditions,temperature,ionic strength,and the presence of natural organic matter were studied.Adsorption of microcystin-LR on CoFe2O4 increased with the increase of initial concentration and temperature.However,it decreased with the increase of solution pH value and ionic strength.Interestingly,adsorption process was not significantly influenced by the low concentration of humic acid(0-2.5 mg/L),and adsorption ability decreased at higher humic acid concentrations.The results indicated that electrostatic interactions and coordination interactions were important in controlling the adsorption of toxin onto CoFe2O4 nanoparticles.Because of its unique magnetic responsibility,excellent dispersibility in water,and ease in synthesis,CoFe2O4 has a great potential in removing biological contaminants from environmental water.关键词：magnetic nanoparticles;high performance liquid chromatography(HPLC);microcystins;adsorption
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发布时间： - 摘要：compounds,namely,2-thenaldehyde-4-dimethylaminobenzoylhydrazone(1),2-furaldehyde-4-dimethylaminobenzoylhydrazone(2) and benzaldehyde-4-dimethylamino benzoylhydrazone(3) were synthesized，and fully characterized by 1H NMR,13C NMR and MS spectra.The interactions between metal ions and compound 1,2 and 3 were investigated by UV-Vis absorption spectroscopy.The results indicated that compound 1 selectively bound with Hg2+ by formation of a 1∶1 stable complex of 1-Hg2+ with binding constant of 9.7×104 L?mol-1.A good linear relationship was obtained for Hg2+ in the range of 1.0-18 μmol/L,and the limit of detection was 0.28 μmol/L.Some other coexistent competitive cations such as Cu2+,Fe3+ and Ni2+ did not interfer the detection of Hg2+.Thus compound 1 could be used as a potential colorimetric and naked-eye chemosensor for Hg2+.For compound 2,it showed spectral responses to Hg2+,Cd2+ and Zn2+by formation of 1∶1 metal complexes.The binding constants were determined to be 6.5 × 104 L?mol-1 for the complex of 2 with Hg2+ and 5.0× 105 L?mol-1 for the complex of 2 with Zn2+ in acetonitrile,respectively.However,compound 3 did not show any spectral response for the metal ions tested.Obviously,the high selectivity of compound 1 toward Hg2+ was ascribed to the binding sites from assembly of various atoms,in which both S and O atoms participated in the coordination interaction with Hg2+.关键词：benzoyl hydrazone derivatives;heavy metal ion;Hg2+;absorption spectroscopy
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发布时间： - 摘要：A simple and efficient method based on high performance liquid chromatography(HPLC) was established to separate twelve analytes of sweeteners(rhamnose, xylose, fructose, glucose, rebaudioside, sucrose, maltose, lactose, 1-kestose, raffinose, nystose, stachyose) in feeds.The target analytes were separated on a XB-NH2 column with gradient elution of acetonitrile-water as mobile phases.The analytes were detected by the evaporative light-scattering detector (ELSD).The result indicated that all twelve sweeteners had good linearities within 0.05-5 g/L with correlation coefficients of 0.996 3-1.000 0.The limits of detection were all not more than 0.04 g/L.The average recoveries for the sweeteners ranged from 86.6% to 112% with RSDs of 0.5%-6.7%.The results showed the method was simple， rapid and reliable,and was suitable for the determination of sweeteners in feeds.关键词：feeds;sweeteners;high performance liquid chromatography(HPLC);evaporative light scattering detection (ELSD)
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发布时间： - 摘要：The aim of the study was to build UV spectrum of Ganoderma lingzhi and 11 kinds of counterfeits,compare the differences of UV spectra between samples and distinguish G-lingzhi and its counterfeits by UV spectroscopy combined with chemometrics.The results showed that the UV spectra,which ranged from 220 nm to 255 nm,of G-capense,Amauroderma niger,G-kunmingense,G-dahlia,A-rugosum and G-ramosissimum were different from G-lingzhi’s spectrum.The UV spectra of G-applanatum,G-philippii,G-subtornatum and G-lucidum were very different from G-lingzhi.Similar analysis showed that the UV spectra of G-capense,A-niger,G-dahlia and A.rugosum had the highest Pearson correlation coefficients(rr).The coefficients were 0.949,0.961,0.948 and 0.919,respectively.However,G-philippii and G-subtornatum had the lowest Pearson correlation coefficients.The coefficients were 0.657 and 0.299,respectively.UV spectral data of 13 batches of samples were processed and subjected to principal component analysis(PCA).The result showed that SG+SNV was the best mathematical pretreatment.PCA showed that the first principal component contribution rate was 54.24%.The second principal component contribution rate was 36.45%.Total contribution rate was 90.69%.According to the results of PCA,all the samples could be divided into seven groups.G-lingzhi and its counterfeits were distinguished successfully.All the results could help to discriminate G-lingzhi and its counterfeits，and provide a theory evidence for safety usage and quality control of G-lingzhi.关键词：medicinal fungi;Ganodermataceae;UV spectrum;chemometrics;quality evaluation
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发布时间： - 摘要：In this work，resveratrol and piceid were non-isothermally analyzed by differential scanning calorimetry(DSC) and thermogravimetric(TG) methods under the nitrogen atmosphere.The melting point and purity were calculated by Vant Hoff equation while the kinetic parameters(including the most probable mechanism function，apparent activation energy Ea and pre-exponential factor A) were inferred by three thermal analysis kinetics methods(Coats-Redfern method，Achar method and Malek method ).The results showed resveratrol and piceid(99.76% and 98.90%) of high purity melted at 257.09 ℃ and 198.79 ℃，respectively.The thermal decomposition of resveratrol began at 220 ℃ and ended up at 468 ℃ with mass loss of 46.69%.Piceid decomposed from 198 ℃ to 369 ℃ with mass loss of 37.47%，which could be explained by the cracking of glycosidic bond.The most probable thermal decomposition mechanisms of resveratrol and piceid were Chemical Reaction and three dimensional diffusion，respectively，corresponding with reaction order equation(the order of reaction n=2) and Z.-L.-T.equation.According to kinetic parameters of thermolysis，the shelflives of resveratrol and piceid at room temperature(25 ℃) were inferred as 3 years and 4-5 years，respectively.关键词：resveratrol;piceid;melting point;thermal stability;thermal decomposition kinetics
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发布时间： - 摘要：Based on molecular design,a kind of molecularly imprinted membranes with graft type for the pesticide pirimicarb was firstly prepared by using a new imprinting technology of “synchronously graft-polymerizing and imprinting”.In this process,chloromethylated polystyrene(CMPSF) membrane was as base membrane,the anionic monomer sodium p-styrenesulfonate(SSS) was used as functional monomer and N,N’-methylenebisacrylamide(MBA) was as crosslinker.By the initiating of a surface-initiating system of-NH2/S2O2-8,the graft-polymerization/crosslinking of SSS and MBA that were combined around the template molecule of pirimicarb was realized,resulting in the pirimicarb-imprinted membrane.The imprinted membrane was characterized by infrared spectroscopy(FITR) and optical microscope(OM).On this basis,the molecular recognition ability and mechanism of the imprinted membrane were examined and investigated in depth.Finally,pirimicarb-potentiometric sensor was constituted by using the pirimicarb-imprinted membrane as sensitive membrane,and the detecting performance of this potentiometric sensor was evaluated.The results show that the prepared imprinted membrane possesses the specific recognition selectivity and excellent binding affinity for the template pirimicarb molecule,and the binding capacity gets up to 92 μg/cm2.Relative to another pesticide,atrazine,whose structure is similar to that of pirimicarb in a certain degree,the coefficient of selectivity of the imprinted membrane could reach to 4.537.In pH 4.0 aqueous medium,this sensor offers a linear response to pirimicarb over the range of 1.0×10-6-1.0×10-3 mol/L(r=0.999 9) with a lower detection limit of 2.5×10-8 mol/L.The potentiometric sensor constituted with pirimicarb-imprinted membrane as sensitive membrane shows the advantage of simple establishment process, sensitive detection and faster response(t<10 s).关键词：molecularly imprinted membrane;selectivity of molecule recognition;polysulfone;sodium p-styrenesulfonate;pirimicarb;potentiometric sensor
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发布时间： - 摘要：A new high-capacity imidazole type chelating resin was synthesized via surface-initiated atom transfer radical polymerization（SI-ATRP) method.1-Vinylimidazole（VIM) was grafted onto the surface of the chloromethyl polystyrene resin by SI-ATRP using organic metal compound formed in the CuBr/2,2’-bipyridine（Bpy) system as catalyst at room temperature.The chelating resin was characterized by means of isoelectronic X ray spectrum,elementary analysis and electron microscopy，and its adsorption properties,parameters of kinetics and thermodynamics were determined.The amount of VIM on the surface of polystyrene resin was calculated to be 1.008 mg/m2.Adsorption capacity for cadmium（Ⅱ) and zinc（Ⅱ) increased with increasing initial metal ion concentration and temperature，and its highest values were 653.1 mg/g for cadmium（Ⅱ) at pH 3.6 and 793.3 mg/g for zinc（Ⅱ) at pH 2.4.The experimental results showed that the equilibrium adsorption data fitted well to both Langmuir and Freundlich isotherms.The thermodynamic equilibrium functions were also determined as follows:ΔG<0，ΔH=24.47 kJ/mol，ΔS>0，so the adsorption was spontaneous，endothermic and entropy increasing.The kinetic experimental data were correlated with second-order kinetic model.关键词：imidazole type chelating resin;surface-initiated atom transfer radical polymerization（SI ATRP);adsorption property;Cd（Ⅱ);Zn（Ⅱ);kinetics;thermodynamics
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发布时间： - 摘要：A new method for the automated determination of three kinds of trace aromatic amines(o-toluidine，3,3′-dimethylbenzidine，β-naphthyl amine) was developed using on-line hollow fiber liquid phase microextraction/high performance liquid chromatography. An online detection device was built by connecting the hollow fiber liquid-phase microextraction device and high performance liquid chromatography with sequential injection device. The influences of extraction parameters including extracting solvent，donor phase，acceptor phase，salt effect，stirring rate and extraction time were investigated with this online device.The optimum experimental conditions were as follows:extraction reagent:1-octanol，donor phase:0.1 mol?L-1 NaOH-300 mg?L-1 NaCl，acceptor phase:0.1 mol?L-1 HCl， stirring rate:400 revolution per minute(r/min),extraction time:40 min.Under the optimum conditions，the qualitative and quantitative analyses of three kinds of trace aromatic amines were preformed by HPLC.The proposed method provided enrichment folds of 48-96.Good linearities were obtained in the range of 0.01-0.25 mg?L-1 with correlation coefficients not less than 0.998 4.The detection limits(S/N=3) were in the range of 0.3-2.2 μg?L-1 ,and RSDs(n=10) were 3.1%-4.0%.The spiked recoveries of aromatic amines in printing and dyeing wastewater ranged from 98.0% to 102.0%.With the advantage of simplicity，rapidness，less consumption of extracting solvent，high enrichment factor，and great precision for detection,this method is effective for fast and accurate analysis of trace aromatic amines.关键词：Liquid-phase microextraction;liquid chromatography;aromatic amines;on-line determination
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发布时间： - 摘要：A high performance and facile method was developed for analysis of geniposide and baicalin by reversed-phase pressurized capillary electromatography(pCEC).The separation was performed on a reversed-phase EP-100-20/45-3-C18 column(total length 45 cm,effective length 20 cm,diameter 100 μm,ODS packing inside diameter 3 μm) with column temperature of 25 ℃.The mobile phase was composed of 20 mmol/L NaH2PO4-acetonitrile(71∶29), mobile phase overall flow rate was set at 0.035 mL/min,separation voltage was +2.0 kV,and the UV detection wavelength was 240 nm.In an isocratic mode pCEC,the relative standard deviations(RSDs) for peak area were not more than 2.8%,and the recoveries were in the range of 91.9%-101.2%.This method was applied in the detection of Xiongju Shangqing Pian with geniposide content of 2.616 mg/g and baicalin content of 11.220 mg/g.The method showed advantages of good selectivity,high column efficiency and low consumption of sample and reagent,and was successfully applied in the separation and detection of geniposide and baicalin in real sample.关键词：pressurized capillary electromatography(pCEC);geniposide;baicalin;Xiongju Shangqing Pian
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发布时间： - 摘要：Ionic liquid modified graphene(IL-GR) was firstly dispersed in polyvinyl alcohol(PVA) to form IL-GR-PVA dispersion,then IL-GR-PVA and acetylcholinesterase(AChE) was mixed evenly and was coated on the glass carbon electrode via PVA film-forming.A novel biosensor was developed for the detection of organophosphorus pesticide(OP).Different techniques were employed to study the construction process and the electrochemical properties of the biosensor.The IL-GR-PVA nanocomposites with excellent conductivity and biocompatibility offered an extremely hydrophilic surface for AChE adhesion.Linear relationship between the inhibition percentage(I%) and logarithm of phorate concentration was found in the ranges of 1.0×10-14-1.0×10-9 mol/L and 1.0×10-9-1.0×10-6 mol/L,with a detection limit(S/N=3) of 8.0×10-15 mol/L.The easily prepared electrochemical sensor has a favorable stability and sensitivity,thus providing a new OPs detection method关键词：graphene;ionic liquid;polyvinyl alcohol;phorate;biosensor
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发布时间： - 摘要：A conjugated polymer fluorescent probe was synthesized by Schiff reaction using the compounds of p-phenylenediamine and 1,10-phenanthroline-5,6-dione prepared with 1,10-phenanthroline.This polymer was characterized by means of 1H NMR,IR,viscosity,etc.The selective and sensitive properties of the polymer to detect metal ions were investigated by UV-vision absorption and fluorescent spectroscopy.Furthermore,in order to explore the interaction mechanism between the polymer fluorescent probe and Fe3+，the UV-Vis absorption and fluorescent spectra and IR absorption spectra of 1,10-phenanthroline-5,6-dione and polymer fluorescent probe at the presence and absence of Fe3+ were measured and analysed.The experiment results showed that the colours of the solution changed from colourlessness to reddish brown only at presence of Fe3+,which indicating that Fe3+ could be detected by naked eyes.Moreover,the change of the UV-vision absorption and fluorescent spectra of the polymer revealed that the polymer fluorescent probe owned a high sensitivity and selectivity for the detection of iron(Ⅲ).The instant response time was less than 1 s,and the abslute response time was 30 min.Moreover,the linear response range of iron(Ⅲ)was in the range of 0-12.5 μmol/L and the detection limit was 2.72 μmol/L.The quenching constant of Fe3+ to the probe was 1.52×104 L/mol.In addition,the possible interactional diagrammatic sketch between the polymer fluorescent probe and iron(Ⅲ)was drawn by analysing the interactional mechanism of the polymer probe-Fe3+ complex.关键词：conjugated polymer;fluorescent probe;detect;iron(Ⅲ)
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发布时间： - 摘要：A quantitative method using ultra performance liquid chromatography（UPLC） with UV detector was developed for the determination of lufenuron residue in apple and soil.The sample was extracted with acetonitrile and the extractants were separated from water caused by the addition of salts.The supernatant was concentrated to dryness without any further clean-up step,and the residue was redissolved with methanol and then diluted with water prior to HPLC analysis.A BEH C18 column(50.0 mm×2.1 mm，1.7 μm) was used to separate the sample by using a mixture of methanol-water(60∶40) as mobile phase at a flow rate of 0.4 mL/min.The ultraviolet detection wavelength was set at 255 nm.The method had a good linear relationship in the range of 0.025-2.5 mg/L with a correlation coefficient(r) of 0.999 7．The average recoveries of lufenuron at a spiked range of 0.05-0.5 mg/kg ranged from 84.5%to 98.7%with relative standard deviations(RSDs)of 0.7%-6.1%.The limit of detection(LOD) was 0.01 mg/kg．关键词：ultra performance liquid chromatography(UPLC);lufenuron;apple;soil;residue analysis
- 1978
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发布时间： - 摘要：A highly sensitive platform for adenosine triphosphate(ATP)assay was designed based on exonuclease Ⅲ(Exo Ⅲ)induced target recycling amplification and fluorescence quenching of graphene.The system mainly consists of two nucleic acid strands P1 and P2 carrying a part of aptamer sequences for ATP,and P1 with FITC labeled on its 3’ end.Upon addition of target ATP to the system,P1 hybridizes with P2,and forms a DNA duplex sandwich structure.The formation of DNA duplex sandwich structure triggers selective enzymatic cleavage of 3-recessed end by Exo Ⅲ,resulting in the release of target ATP and FITC.Released target ATP then hybridizes with nucleic acid strands P1 and P2,generating many FITC molecule.As a result,the FITC molecule break away from the G surface,and lead to the fluorescence recovery of the dye FITC.This assay exhibits a high sensitivity with a detection range of 0.02-1 μmol/L and a detection limit(S/N=3) of 9 nmol/L.关键词：adenosine triphosphate;exonuclease Ⅲ;graphene;fluorometry;aptasensor
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发布时间： - 摘要：A RP-HPLC method was established to separate B3 and B3iso desamido human insulin in recombinant human insulin injection and HPLC-QTOF mass spectrometry was used to identify the amino acid sequence.On the base of the method of recombinant human insulin injection in Chinese pharmacopeia(edition 2010,second part), the pH of mobile phase was optimized using 0.2 mol/L sulfate buffer solution with pH 3.6 acetonitrile(90∶10) as phase A,and acetonitrile-water(50∶50) as phase B by gradient elution.The peak 1 and peak 2 were collected,desalted and concentrated,then digested with V8 enzyme,and reduced with TCEP,then identified by LC-MS/MS.The peaks were identified as B3 and B3iso desamido human insulin.Using the optimized method to compare the related substance results of recombinant human insulin injection on market,the test results revealed that different brands of insulin injection had different degree of B3 and B3iso desamido human insulin.The optimized method did not influence other impurities determination.It is useful for effectively monitoring the increasing trend of deamido insulin during storage.关键词：recombinant human insulin;B3 and B3iso desamido human insulin;RP-HPLC;LC-MS/MS
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发布时间： - 摘要：In this paper,a new method based on smartphone was proposed for the rapid detection of organophosphorus residues pesticide,and effects on the detection results with three smartphones of different bands were also studied.In order to minimize the influences of ambient light on the images,a surface source based on light-emitting diode(LED) was used,and the accuracy of the detection was also improved.In the experiment,the LED surface source was placed upon the samples vertically and the smartphone was arranged in front of the samples to capture the images.The results are consistent with that obtained by the UV-Vis spectrophotometer.关键词：colorimetric;smartphone;malathion;light-emitting diode(LED)
- 2031
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发布时间： - 摘要：An oxygen flask combustion-ion chromatography employed electrical conductivity detector for the determination of chloral hydrate in gliquidone main ring was developed.The organochlorines in gliquidone main ring was transformed to inorganic chlorines by oxygen flask combustion method,and eventually changed into chloride ion after absorbed by NaOH solution.Various ion chromatography conditions,e.g.mobile phase,flow rate and column temperature were investigated,and the optimal conditions were as follows:column:TSKgec SuperIC-Anion HS anion column;mobile phase: 7.5 mmol/L NaHCO3-1.1 mmol/L Na2CO3 solution;column temperature:40 ℃;flow rate:1.0 mL/min;detector:electrical conductivity detector.The results indicated that the method had a good specificity and precision(RSD≤2.0%).The calibration curve was linear over the chlorion concentration range of 0.025-0.080 mg/L with correlation coefficient of 0.999 9.The limit of detection(LOD)was 0.01 μg/L and the limit of quantitation was 0.05 μg/L.The spiked recoveries at 3 levels were in the range of 92.9%-103.4%with relative standard deviation of 6.4%.The method is convenient and effective for determinating the content of chloral hydrate in gliquidone main ring,and it could satisfy the requirement for qulity control of chloral hydrate as impurity in gliquidone main ring.关键词：oxygen flask combustion;ion chromatography;chloral hydrate;gliquidone
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发布时间： - 摘要：A highly water-soluble fluorescent carbon dots(CDs) was prepared by hydrothermal method using glucose as carbon source，and polyethylene glycol-200(PEG-200) as dispersant and surface modifier. A new fluorophotometric method for the determination of nickel ion was developed using CDs as fluorescent probes，based on the significant fluorescence quenching of CDs in the presence of nickel ion in pH 5.72 Britton-Robinson(B-R) buffer.The maximum excitation wavelength of the system was set at 350 nm and the maximum emission wavelength was 435 nm.Under the optimal conditions, the relative fluorescence intensity of CDs was proportional to concentration of nickel ions in the range of 3.0-80 μmol/L，with a linear regression equation of ΔF= 1.009+0.031 0 c(μmol/L) and a correlation coefficient(r) of 0.998 3.The detection limit was 0.13 μmol/L.The proposed method was applied in the determination of trace nickel in the environmental water samples，and the results were consistent with those obtained by the atomic absorption spectrometry.The spiked recoveries of standard addition were in the range of 98.1%-103.5%, with relative standard deviations(RSD) less than 2%.关键词：carbon dots(CDs);nickel;fluorescence quenching;polyethylene glycol-200(PEG-200);environmental water
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发布时间： - 摘要：The interactions between human serum albumin(HSA)and five kinds of amino acid enantiomers were studied by surface plasmon resonance (SPR) without any labeling for the first time.The dynamic informations of their interactions were well shown in real time,and the kinetics parameters were also obtained.The difference in interactions between each of amino acid enantiomers and HSA could be recognized obviously by comparison of the sensorgrams.Although the binding rate constants and the dissociation rate constants of them did not have any rule,the results showed that the affinity of HSA and L-amino acid was bigger than that of HSA and D-amino acid,which indicated the chiral recognition force may contribute to the discrimination interactions between amino acid enantiomers and HSA.关键词：surface plasmon resonance(SPR);amino acid;human serum albumin(HSA);chiral recognition;affinity;dynamics
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发布时间： - 摘要：Sulfaguanidine can significantly inhibit the chemiluminescence(CL) intensity of Ni(Ⅳ) complex-luminol system.Based on this，a new method of Ni(Ⅳ) complex-luminol CL system coupled with flow-injection for the determination of sulfaguanidine is developed.Under the optimum conditions，the linear range is 6.0×10-7 mol/L to 6.0×10-6 mol/L to the CL relative intensities with a detection limit(3σ) of 2.4×10-10 mol/L.The RSD(n=11) is 1.4%for 2.4×10-6 mol/L sulfaguanidine.The proposed method was applied in the analysis of sulfaguanidine in swine feed samples with satisfactory results.关键词：sulfaguanidine;Ni(Ⅳ) complex;chemiluminescence;luminol;feed;determination
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发布时间： - 摘要：Graphene-based nanomaterial is a new kind of adsorbent material over the past decade.They are widely applied in removal and analysis of various toxic pollutants and hazardous substances.Recently,mycotoxin contamination is one of the main factors which can endanger food safety.Moreover,analysis of mycotoxins is often restricted by sample preparation methods.This paper describes the current graphene based nanomaterials as adsorbents applied in sample pretreatment techniques.And the latest application advances in the detection of mycotoxins using such sample pretreatments are also summarized.关键词：graphene;adsorbents;mycotoxins;sample pretreatment technology;application;review
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