最新刊期
卷 33 ， 期 6 ， 2014
- 摘要：An ultra-performance liquid chromatography-quadrupole-time of flight mass spectrometric（UPLC/Q-TOF MS） method was developed for the study on metabolic variations of urine from diabetes mellitus patients and healthy volunteers.PLS-DA was used for group differentiation and potential biomarkers selection.As shown in the scores plot,the distinct clustering among diabetes mellitus patients and health controls was observed.In carbohydrate metabolites,the sodium glucuronic acid content of the patients was significantly higher than that of the normal control group.Compared with the normal control group,the fatty acids contents of the patients were higher than those of the control group,contents of 20-carboxy-arachidonic acid,palmitic acid in the urine of patients with diabetes were higher than that in normal subjects.The metabolite contents of amino acids including tyrosine,N-beta-alanyl-L histidine and tryptophan of the patients were lower than those of the normal,but the contents of glutaric acid,nicotinoyloxy glycine,aspartic acid,phenylalanine,etc.of the patients were lower than those of the normal people.These metabolites are associated with glucose and lipid regulating substances.This study showed the potential of metabolomic strategies for explanation of the mechanism of diseases and detection of specific biomarkers.关键词：diabetes mellitus;metabonomics;UPLC;TOF MS
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- 1012
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发布时间： - 摘要：The highly specific antibody was prepared with CNH（6-［（1-naphthyloxy） carbonyl］ amino hexanoic acid）coupled with BSA（bovine serum albumin）as immunogen.Three coating antigens,CNH-OVA,CNB-OVA and CNA-OVA were obtained with CNH（6-［（1-naphthyloxy） carbonyl］ amino hexanoic acid）,CNB（4-［（1-naphthyloxy） carbonyl］ amino butyric acid）and CNA（3-［（1-naphthyloxy） carbonyl］ amino propanoic acid）coupled with OVA,respectively.Taking antibody and coating antigens mentioned above as key materials,the influences of homologous coating antigen,heterologous coating antigen and each ELISA influence factor on detection sensitivity were investigated,the indirect competitive ELISA of carbaryl was established,and the method’s applicability to the measurement of carbaryl residues in rice and its soil was studied.The results showed that the sensitivity of the ELISA assay with CNA-OVA heterologous coating was high,and the IC50 was (10.51±0.11) μg?L-1.The detection range of ELISA was in the range of 2.07-47.30 μg?L-1（IC20-IC80 as a standard）.Taking 0.5,1.0,2.0,4.0 mg?kg-1 as additive concentration,the spiked recoveries of carbaryl in the rice and soil samples were in the ranges of 92.3%-111.6% and 85.3%-103.2%,respectively.The relative standard deviations were less than 10%.There were no distinct difference between the results of ELISA and HPLC（P>0.05）.关键词：carbaryl;heterologous coating;ELISA;rice;soil
- 1812
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- 1111
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- 6
发布时间： - 摘要：A sensitive ultra performance liquid chromatography-tandem mass spectrometric（UPLC-MS/MS） method was developed for the simultaneous determination of 9 progesterones,7 androgens,7 glucocorticoids,2 estrogens in anti-aging oral samples.The analytes were stepwise extracted with acetonitrile containing 1% acetic acid and methanol,the extract was concentrated to dryness,redissolved in methanol-water（1∶1）.25 hormones were gradient separated on a Shim-pack XR-ODS Ⅱ column,and analyzed by electrospray ionization under positive ion mode with matrix standard curve.As a result,the calibration curves for all target compounds were linear in the range of 0.5-50 μg/L with correlation coefficients larger than 0.99.The limits of detection（LOD） ranged from 0.029 μg/kg to 0.147 μg/kg and the limits of quantitation（LOQ） ranged from 0.099 μg/kg to 0.492 μg/kg.The average recoveries of 25 compounds at spiked levels of 0.5,1.0,5.0 μg/kg were in the range of 73.3%-122.2% with relative standard deviations（RSD） of 5.1%-14.9%.The method is simple,rapid and accurate,and is suitable for the rapid determination of hormones in anti-aging function foods.关键词：oral;hormone;ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）
- 1927
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- 992
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- 12
发布时间： - 摘要：Applied in modified QuEChERS（Quick,Easy,Cheap,Effective,Rugged and Safe） method with nano Bamboo Charcoal（NBC） as sorbents for analysis of multi pesticide residues in green tea was developed.Pesticides in tea were extracted with acetonitrile-H2O followed by liquid-liquid partitioning by adding NaCl.The extract was cleaned up using the mixture of NBC-PSA（primary secondary amine）-MgSO4 in dispersive solid-phase step.After separated on an Acquity UPLC TSS-3 C18 column（100 mm×2.1 μm,1.8 μm）,the analytes were determined by ultra high performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） under multiple reaction monitoring mode（MRM）,and quantified by the external standard method.The recoveries for 10 pesticides in tea sample in the fortified concentration range of 0.02-0.50 mg/kg ranged from 72.3% to 116.3% with relative standard deviations（RSD） of 1.4%-13.9%.The limits of quantitation（LOQs） were in the range of 0.02-0.04 mg/kg.The method could meet the requirements for pesticide residue analysis.Furthermore,the method is more commercial than other QuEChERS methods with advantage of low cost of NBC．关键词：tea;pesticide residue;nano Bamboo Charcoal;QuEChERS;ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）
- 1861
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- 1025
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- 11
发布时间： - 摘要：A method was developed for the simultaneous determination of bromoadiolone and brodifacoum in water by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) and ultrasonic assisted extraction with ionic liquid ［C4mim］［PF6］.An ionic liquid,1-butyl-3-methylimidazolium hexafluorophosphate(［C4mim］［PF6］) was used to extract the rodenticides in water samples.The extraction parameters,including sample volume,temperature,ultrasonic-extraction time,inorganic salt concentration and solution pH were investigated.The separation of target compounds was performed on an XDB C18 (150 mm×2.1 mm,5 μm) column with methanol- 0.2% acetic acid(85∶15) as mobile phase.The detection was carried out by LC-MS/MS using a negative electrospray ionization interface in multi-reaction monitoring(MRM) mode.Calibration curves were linear within the range of 0.005-1.0 μg?L-1 with correlation coefficients more than 0.999.The limits of quantitation(LOQs)were both 0.005 μg?L-1.The extraction recoveries were between 91.0% and 97.8%,the intra-day RSDs were between 1.1% and 6.6%,and the inter-day RSDs were between 2.5% and 9.1%.The developed method was simple,accurate and distinctive,and could be used for the determination of trace bromoadiolone and brodifacoum in environmental water.关键词：ultrasound assisted ionic liquid dispersive liquid phase microextraction;water;［C4mim］［PF6］;bromoadiolone;brodifacoum;LC-MS/MS
- 2029
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- 960
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- 6
发布时间： - 摘要：An acetylcholinesterase biosensor for the rapid detection of paraoxon was developed based on composites of magnetic Fe3O4-Au nanoparticles(Fe3O4-AuNPs) prepared by chemical co-precipitation.This magnetic nanoparticle composites and carbon nanotubes(CNTs) were immobilized on a home-made magnet/glassy carbon electrode(MGCE) and served as matrix for immobilizing AChE.The chemical composition,magnetic properties and morphology of magnetic nanoparticles composite Fe3O4-AuNPs were characterized by X-ray diffraction,vibrating sample magnetometry and transmission electron microscopy,respectively.The electrochemical characteristics of home made MGCE and enzyme biosensor were characterized by electrochemical impedance spectroscopy(EIS),cyclic voltammetery,and differential pulse voltammetry(DPV).The determination of paraoxon using the biosensor were investigated by DPV.Under the optimal conditions，the inhibition efficiency of the immobilized AChE was proportional to the logarithm of paraoxon concentration over the range of 3.6×10-6-2.9×10-2 mol/L with a detection limit of 1.6×10-7 mol/L.The proposed method was successfully applied in the determination of paraoxon in real water sample with recoveries of 98.0%-107%.关键词：Fe3O4-Au nanoparticles;magnet/glassy carbon electrode;acetylcholinesterase;paraoxon
- 2048
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- 948
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- 0
发布时间： - 摘要：A high performance liquid chromatography-tandem mass spectrometric（HPLC-MS/MS） method was established for the determination of six deoxynivalenols and their derivatives in grains such as wheat,barley,corn and rice.And the pollutions of those mycotoxins in grains were surveyed.The six mycotoxins in grains were extracted with acetonitrile-water（84∶16） in supersonic instrument,and purified with MycosepTM 227 multifuntional column.Then the purified solution was concentrated with nitrogen,and redissolved with acetonitrile-0.1% ammonia water（5∶95） and cleaned with 0.22 μm millipore filter.The filtrate was detected by HPLC-MS/MS,identified by electrospray ionization（ESI） in negative mode using multiple reaction monitoring（MRM） mode,and quantified by the external standard method.The calibration curves of six mycotoxins showed good linearities in the range of 5.0-200 μg/L with correlation coefficients of 0.998 8-0.999 3.The detection limits of the method ranged from 0.10 μg/kg to 0.18 μg/kg.The recoveries of six mycotoxins at three spiked levels of 5.0,20.0,100.0 μg/kg were in the ranges of 90.6%-101.6%,91.4%-99.4% and 90.3%-105.0%,respectively,with RSDs less than 10%.With the advantages of operation convenience,less interference from impurities and good accuracy,the method could meet the requirements of national food risk monitoring method for the determination of six deoxynivalenol in grains.关键词：high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）;deoxynivalenol;mycotoxins;grain
- 2251
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- 1144
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- 11
发布时间： - 摘要：The characteristics of the near infrared（NIR） spectra from the electricity coal samples were investigated.During the whole process of the study,with principal components score,Mahalanobis distance and Partial Least Squares cross validation for picking out outliers,the first three principal components and six discrete Fourier transformation（DFT） coefficients were obtained,and finally partial least squares regression（PLSR）,grid-support vector regression（G-SVR）,genetic algorithm-support vector regression（GA-SVR） and particle swarm optimization-support Vector Regression（PSO-SVR） quantitative analysis models were constructed.The results indicated that when the particle swarm optimization-support vector regression generation was 300,the population was 20,when c1 was 1.5 and c2 was 1.7,the calibration correlation coefficient was 0.990,the prediction correlation coefficient was 0.954,the calibration standard error was 0.366 and the prediction standard error was 0.128.The method was accurate and reliable,and was applied in the near infrared electricity coal calorific value detection system,which could also be used in other extremely complex near infrared online systems.关键词：NIR;SVR;discrete Fourier transform;calorific value of coal;quantitative analysis model
- 1901
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- 833
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- 0
发布时间： - 摘要：Monodisperse macroporous poly（glycidylmethacrylate-co-ethylenedimethacrylate） （PGMA/EDMA） beads were synthesized,and a new kind of strong anion stationary phase was prepared by chemical modification of the PGMA/EDMA beads.This column has a superior separation ability for some inorganic anions（e.g.F-,Cl-,NO-2,Br-,NO-3 and SO2-4） and organic acids（e.g.methane acid,acetic acid,monochloroacetic acid and oxalic acid） by elution of 6.0 mmol/L sodium carbonate and 5.5 mmol/L sodium bicarbonate at a flow rate of 1.0 mL/min.Moreover,the separation of a mixture of anions and organic acids can also be well obtained at the same chromatographic conditions.The influences of eluent type,pH value and organic solvent on retention of six inorganic anions were studied.Under the optimized chromatorgraphic conditions,the six anions had good linear relationships in the certain concentration range and low detection limits.The column was used in the separation of inorganic anions in running water,and four anions were separated in 22 min.The recoveries of four anions were between 96.4% and 100.6%.关键词：monodisperse polymer resins;strong anion ion chromatography;inorganic anions;organic acids;running water
- 2484
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- 951
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发布时间： - 摘要：A rapid determination method for amantadine and rimantadine in swine urine was established using ultra performance liquid chromatography-electrospray tandem mass spectrometry（UPLC-ESI-MS/MS） in multiple reaction monitoring（MRM） mode.The urine sample was extracted with acetonitrile by ultrasonic,and cleaned up with solid-phase extraction Oasis MCX column.The separation of compounds was carried on an Eclipse Plus C18（RRHD 1.8 μm，2.1 mm×100 mm） by gradient elution using methanol-0.1% formic acid as mobile phase.The electrospray was operated in the positive mode and the samples were monitored under the multiple reaction monitoring（MRM） mode．The chromatographic retention time and mass fragment ion abundance ratio were taken for qualitative confirmation,and the internal standard method was employed for quantification analysis.The limits of detection（LOD） for both compounds were 0.05 μg/L,and the limits of quantitation（LOQ） were 0.2 μg/L in swine urine.The correlation coefficients of the swine urine were greater than 0.999（r2>0.999） within 0.2-20.0 μg/L linear ranges.Recoveries of amantadine and rimantadine at spiked levels of 0.5-20.0 μg/L were in the range of 89.7%-102.8% with intra-day relative standard deviation（RSDs） of 2.8%-4.2%.关键词：ultra performance liquid chromatography-electrospray tandem mass spectrometry（UPLC-ESI-MS/MS）;amantadine;rimantadine;swine urine
- 1996
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- 1188
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- 4
发布时间： - 摘要：A voltammetric sensor for the determination of acid orange Ⅱ（AO2） was developed based on molecularly imprinted electropolymerized membrane.The sensor was obtained by electropolymerization of o-phenylenediamine（o-PD） and m-dihydroxybenzene（m-DB） on a platinum electrode in the presence of AO2 as a template.The recognition performance of the sensor was studied in the presence of potassium ferricyanide（K3［Fe（CN）6］） by cyclic voltammetry（CV） and differential pulse voltammetry（DPV）.The template was removed by washing with methanol-acetic acid（7∶3） solution.The studies revealed that the imprinted sensor showed an excellent selectivity,sensitivity and stability for AO2.The response of the imprinted sensor was linear with concentration of AO2 from 1.0 μg/L to 100.0 μg/L,and the detection limit（S/N=3） was 0.10 μg/L.The method was applied in the detection of AO2 in drinks and beer samples with satisfactory results.关键词：molecular imprinting;electropolymerization;o-phenylenediamine;m-dihydroxybenzene;acid orange Ⅱ
- 2608
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- 1055
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- 2
发布时间： - 摘要：A liquid chromatography coupled with tandem mass spectrometric(LC-MS/MS) method was developed for the simultaneous determination of streptomycin and dihydrostreptomycin residues in eels and honey samples.The samples were extracted with sodium 1-heptanesulfonate and phosphate buffer,and cleaned up with a SUPELCO LC-C18 solid phase extraction(SPE) column.The extracts were separated on a Thermo Aquasil-C18 column(150 mm×4.6 mm,3 μm) using acetonitrile containing 0.3% acetic acid -0.3% acetic acid as mobile phase by gradient elution.The detection of streptomycin and dihydrostreptomycin was carried out by MS/MS under multiple reaction monitoring(MRM) mode.An external standard method was used for quantitative analysis.The method showed good linearities in the range of 10-100 μg/kg for streptomycin and dihydrostreptomycin,and the limits of quantitation(LOQ) were 10 μg/kg.The spiked recoveries of streptomycin and dihydrostreptomycin ranged from 89.6% to 110.3% with relative standard deviations of 2.3%-20.9%.The method was simple,rapid and practical,and could meet the requirements for determination of streptomycin and dihydrostreptomycin residues in eel and honey samples.关键词：liquid chromatography-tandem mass spectrometry(LC-MS/MS);honey;eel;streptomycin;dihydrostreptomycin;residues
- 2648
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- 962
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- 5
发布时间： - 摘要：The anti-ractopamine monoclonal antibody and anti-clenbuterol monoclonal antibody were both coupled with CNBr activated Sepharose 4B to make the immunoaffinity column.The column performance was tested and the use conditions were optimized by HPLC-MS/MS.The results showed that the column capacity to ractopamine,salbutamol and clenbuterol were 49,27,24 ng/mL glue,respectively,the storage time was five months,and the best eluent was methanol.The average recoveries of three lean meat essences ranged from 78.9% to 96.5% with relative standard deviations(RSD) lower than 1.5%.The limits of detection(LOD) ranged from 0.1 ng/g to 1 ng/g.The method could be applied in the simultaneous determination of the lean meat essence contents in feed samples.关键词：ractopamine;salbutamol;clenbuterol;immunoaffinity-column;high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS)
- 1950
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- 965
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- 2
发布时间： - 摘要：A reverse phase high performance liquid chromatographic（RP-HPLC） with variable wavelength detector(VWD) method was developed for the simultaneous determination of nine pesticide residues,including imidacloprid,acetamiprid,carbendazim, thiophanate-methyl, pyrimethanil,diflubenzuron,benzoylphenyl,phxim,avermectins in vegetables,fruit and edible fungi.The sample was extracted with acetonitrile and purified by Primary secondary amine（PSA）dispersive solid phase extraction.The analytes were separated on a C18（250 mm×4.6 mm,5 μm）column by gradient elution with methanol-acetonitrile（3∶1） and water as mobile phase,and detected at the wavelengths of 270,258,275,254,280,245 nm,respectively.The flow rate was set at 1.0 mL/min and the column temperature was 40 ℃.The results indicated that the calibration curves of nine pesticides showed good linear relationships in the concentration of 0.05-10.0 mg/L with correlation coefficients more than 0.999.The detection limits ranged from 0.006 mg/kg to 0.07 mg/kg.The recoveries ranged from 81.0% to 115.2% with relative standard deviations（RSD） of 0.5%-10.2%.The method was simple,rapid,sensitive and accurate,and was suitable for the determination of the above 9 pesticide residues in vegetables,fruit and edible fungi.关键词：reverse phase high performance liquid chromatography（RP-HPLC）;vegetables;fruit;edible fungi;pesticide residues
- 2305
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- 1114
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- 7
发布时间： - 摘要：With the kelp as a test vector,a new method of seperation and purification of metallothionein-like protein（MT-like） in algae was developed by using sephadex column.Then the MT-like protein and the Zn-MTs standard were measured by UV spectrophotometry.The molecular weight of MT-like protein were characterized by gel electrophoresis and accurately analysed by mass spectrometry.The enrichment ability of heavy metals was studied,and the response of MT-like to Zn and Cu was investigated after the kelp was cultured with ZnCl2,CuCl2,ZnCl2+CuCl2.The results showed that the MT-like and Zn-MTs had a similar UV absorption peak at 294 nm and displayed the similar range in SDS-PAGE gel electrophoresis.The molecular weight of the MT-like determined by electrospray ionization mass spectrometry was about 6.5 ku.The kelp showed a strong enrichment ability for metals,in which the enrichment ability for Zn was stronger than that for Cu.The Zn2+ could promote the MT-like production,while the growth of MT-like induced with Cu2+ increased at first,and then decreased.The Cu2+ had an antagonistic effect on Zn2+ inducing process.关键词：metallothionein like protein;heavy metal;inductive effect;mass spectrometric characterization;algae
- 1881
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- 884
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- 2
发布时间： - 摘要：In pH 7.4 borax-boric acid buffer solution and in the presence of NaCl,gold nanoparticles（GNPs） interacted with kanamycin aptamer to form a stable nanogold-aptemer complex.When kanamycin was added in the solution,it could interact with the aptamer to form a more stable composite while GNPs were released.The uncombined GNPs aggregated into large clusters,which could cause the increase of resonance Rayleigh scattering（RRS） intensity at 571 nm in high concentration of NaCl.Effects of pH value,NaCl concentration and reaction time on the resonance scattering intensity were studied.Moreover,influences of different aptamers and coexistent substances on the determination were also investigated.The results showed that the method had good selectivity.Under the optimum conditions,the increased RRS intensity was linear over kanamycin concentration range of 0.02-0.3 mg/L,with a correlation coefficient（r） of 0.995 6 and a detection limit（3σ） of 2.3 μg/L.The method was applied in the determination of kanamycin in kanamycin injection with satisfactory results.关键词：kanamycin;aptamer;gold nanoparticles（GNPs）;resonance Rayleigh scattering spectra
- 2604
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- 1038
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- 2
发布时间： - 摘要：Kaolin was used as a modifier for the fabrication of high electrochemical performance kaolin composite carbon paste electrode（KCPE）,and hydroquinone（HQ） as a new mediator was applied in indirect electrochemical determination of glutathione（GSH）.The results showed that GSH can distinctly increase the peak current of HQ at KCPE,and the electrocatalytic current was linear with concentration of added GSH.Furthermore,the properties of modified electrode were characterized.Cyclic voltammetry（CV）,tafel and chronoamperograms（CA） were used to determine the effective surface area（0.118 6 cm2）,charge transfer coefficient（0.68）and catalytic rate constant（1.08×104 cm3?mol-1?s-1）,respectively.The good linear relationship between electrocatalytic current and concentration of GSH was obtained in the ranges of 0.1-1 μmol/L（r2=0.999 5） and 2.5-25 μmol/L（r2=0.999 1） with a detection limit（S/N=3） of 0.073 μmol/L by differential pulse voltammetry（DPV） under the optimal conditions.The proposed method was successfully applied in the determination of GSH in eye drops.关键词：glutathione;hydroquinone;kaolin;carbon paste electrode;indirect electrochemistry
- 1864
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- 1105
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- 3
发布时间： - 摘要：A GC/μECD method was established for the simultaneous detection of 10 chlorinated phenols in fungus.The fungus samples were hydrolyzed with H2SO4,evaporated and acetylated with acetic anhydride,then extracted with n hexane.After concentrated and setting the volume,chlorinated phenols were analyzed by GC/μECD and quantified by the external method.The experimental results showed that good linear relationships between peak area and concentrations of chlorinated phenols were obtained in the range of 0.010-0.50 mg?L-1,with correlation coefficients more than 0.995.The method detection limits were in the range of 0.5-2.0 μg?kg-1,and the spiked recoveries were in the range of 83.4%-103.5% with relative standard deviations of 1.5%-10.2%.关键词：fungus;chlorinated phenols;GC/μECD;detection
- 1879
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- 916
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- 2
发布时间： - 摘要：A GC-MS method was established for the determination of tetrabromobisphenol A(TBBPA) in coatings.The pretreatment conditions and the parameters of GC-MS were optimized.The sample was extracted with dichloromethane-acetone(1∶1) mixed solvent,and purified with silica gel solid phase extraction cartridge,then quantitatively concentrated with parallel evaporation instrument.Under the optimal conditions,the standard curve was linear over TBBPA concentration range of 1-50 mg/L with correlation coefficient more than 0999.The recoveries were in the range of 83.2%-104% with relative standard deviations(n=8) of 2.6%-4.7%.The limit of quantitation(LOQ) was 2 mg/kg.This method was rapid,simple and accurate,and was suitable for the qualitative confirmation and quantitative analysis of TBBPA in coatings.关键词：coating;tetrabromobisphenol A;GC-MS
- 2034
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- 942
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- 4
发布时间： - 摘要：An ion chromatographic method was developed for the determination of maleic acid and fumaric acid in starch by using a home-made multi-mode stationary phase based on poly（ionic liquid）-grafted silica （Sil-pC11C1Im column,4.6 mm×150 mm）.The optimized chromatographic conditions were as follows:mobile phase:methanol-10 mmol/L NaH2PO4 solution （5∶95,pH 7.0）;flow rate:1.0 mL/min;detection wavelength:215 nm;sample volume:15 μL.The calibration curves of maleic acid and fumaric acid were linear in the concentration range of 0.1-2.0 mg/L.The average spiked recoveries were between 93.0% and 99.6%with RSDs of 1.1%-7.6%.The limits of detection（S/N=3） were 0.02 mg/L,and the limits of quantitation（S/N=10） were 0.66 mg/kg.The method was simple and rapid,and was suitable for the determination of the maleic acid and fumaric acid in starch sample.关键词：ion chromatography;ionic liquid;maleic acid;fumaric acid;starch
- 1982
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- 1027
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- 2
发布时间： - 摘要：Several sample pretreatment techniques for the trace extraction,enrichment and concentration of pesticide residues in cereals,oil crops and tea before their rapid determinations,including supercritical fluid extraction,accelerated solvent extraction,stir bar sorptive extraction,QuEChERS,solid phase microextraction and online gel permeation chromatography,etc,were reviewed.The important role of sample pretreatment was cited,and the principles,advantages,and scope of application of these techniques were introduced.This article could provide a reference for the development of test technology in detection of pesticide residues in cereals,oil crops and tea.关键词：oil crops;tea;pesticide residues;pretreatment
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