最新刊期
卷 38 ， 期 6 ， 2019
- 摘要：An ultra performance liquid chromatography-quadrupole-orbitrap high-resolution mass spectrometry(UPLC-Q-Orbitrap HRMS) with data dependent acquisition mode was developed for the analysis of 15 functional ingredients in food supplements of pueraria,and a corresponding standard library was also established.By studying the fragmentation mechanism of the functional ingredients,the fragments during fragmentation were obtained.Data-independent acquisition mode was used for the rapid screening of known and unknown functional ingredients in food supplements of pueraria.There existed good linear relationships for 15 functional components in corresponding concentration ranges with correlation coefficients(r2) larger than 0.99.The recoveries at different spiked levels ranged from 83% to 110%,with relative standard deviations(RSD) of 2.1%-8.6%.The established method was applied in actual sample analysis,in which 16 components were screened out,and 4 of them were components beyond the established standard library.Results indicated that the method was feasible in the screening of functional components in food supplements of pueraria.关键词：non-directive screening;ultra performance liquid chromatography-quadrupole-orbitrap high-resolution mass spectrometry(UPLC-Q-Orbitrap HRMS);functional components;pueraria
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发布时间： - 摘要：A fluorescent sensor was fabricated for the detection of radon based on the daughter lead inducing G-rich aptamer T30695 to form G-quadruplex.According to the characteristics of radon radioactive decay,it only takes about 3.82 days for radon to decay and form a stable daughter lead,and 210Pb derived from radon decay is very stable.The half-life period of the stable daughter（210Pb）resulted from radon is 21 years,and the lead daughter product could be used as the target for detection.When there was no lead in the system,T30695 combined with its complementary chain to form a double-stranded DNA structure,and the fluorescent signal of N-methyl mesoporphyrin IX（NMM）was weak.When the system contained daughter lead,aptamer T30695 was induced to form a G-quadruplex structure,and NMM combined with G-quadruplex structure to produce strong fluorescence.Within a certain range, the fluorescence intensity is positively correlated with the concentration of Pb2+ and radon.There existed a linear relationship btween the fluorescence value（ΔIF）of reaction system and Pb2+ concentration in the range of 5.13×10-9-1.25×10-7 mol/L,with a linear regression equation of ΔIF=77.30+5.05c,a detection limit of 1.54×10-9 mol/L and a correlation coefficient（r）of 0.995 0.The detection limit for radon was 1.07×104 Bq?h/m3.关键词：radon;lead;aptamer;G-quadruplex;conformation transformation;fluorescence sensor
- 791
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发布时间： - 摘要：A method was developed for the determination of trace amount of MC-RR and MC-LR in surface water by ultra performance liquid chromatography-mass spectrometry（UPLC-MS/MS）combined with magnetic solid-phase extraction（MSPE） based on ionic liquid modified magnetic zeolitic imidazolate framework material（IL@M/ZIF-8）.The synthesized material was characterized by scanning electron microscopy（SEM） and transmission electron micorscopy（TEM）.The experimental conditions in MSPE and UPLC-MS/MS,including dosage of adsorbent,pH value,type of elution solvent and oscillation time were optimized.Results showed that,under the optimal conditions,there were good linear relationships for MC-RR and MC-LR in the ranges of 0.01-5 μg/L and 0.05-5 μg/L,with their correlation coefficients（r） of 0.999 5 and 0.999 3,respectively.The detection limits were 1.98,3.94 ng/L,and the quantitation limits were 6.52,12.98 ng/L,respectively.The method was applied in the analysis of microcystins in water with spiked recoveries of 88.5%-108% and relative standard deviations of 1.5%-7.2%.The method could be used for the detection of trace microcystins in water samples owing to its simplicity and high sensitivity.关键词：magenetic solid-phase extraction （MSPE）;zeolitic imidazolate framework;ionic liquid;ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）;microcystins(MCs)
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发布时间： - 摘要：A disposable paper-based plate was developed for the use of matrix-assisted laser desorption/ionization time-of-flight mass spectrometer(MALDI-TOF MS) as the existing stainless steel plate or disposable plastic plate requires a complicated cleaning process,which is easy to generate residues causing cross-contamination.Besides,it is not environmentally-friendly when these plates are recycled.Being low-cost and easy to handle after employment,the plate makes no pollution to the environment.The paper-based plate was tested in four aspects,i.e.resolution,sensitivity,reproducibility and microorganism identification.Results showed that the paper-based plate is basically consistent with the steel plate in terms of resolution and sensitivity,and it has a potential in the clinical identification of microorganism with good reproducibility.关键词：matrix-assisted laser desorption/ionization time of flight mass spectrometry(MALDI-TOF MS);paper-based plate;microorganism identification
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发布时间： - 摘要：A selective accelerated solvent extraction method combined with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) was developed for the simultaneous determination of 19 triazole fungicides in Chrysanthemum morifolium.The sample was extracted with acetonitrile,and the mixed dispersive sorbents(PSA,GCB and C18) were dispersed in the extract to reduce the effects of interfering components during the extraction procedure.After concentration,the extract was separated on a BEH C18 column using 2 mmol/L ammonium formate containing 0.1% formic acid and methanol as mobile phases,and detected under multi-reaction monitoring mode in electrospray positive ion mode.Matrix matched method was used for quantitative analysis.There were good linear relationships for 19 triazole fungicides in the range of 1.0-100.0 μg/L with their correlation coefficients(r2) not less than 0.99.The limits of detection and quantitation were 0.6-3.0 μg／kg and 2.1-10.0 μg／kg,respectively.Under the optimal conditions,the average recoveries for those compounds at three spiked levels of 10,50 and 100 μg／kg ranged from 70.3% to 95.3%,with relative standard deviations(RSD) of 0.60%-12%.This method is simple,reproducible and sensitive,and is applicable for the simultaneous determination of triazole fungicides in Chrysanthemum morifolium samples.关键词：selective accelerated solvent extraction;ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS);triazole fungicide;Chrysanthemum morifolium
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发布时间： - 摘要：A surface-enhanced Raman spectroscopy（SERS）with chemometrics was developed for the rapid detection of methotrexate and voriconazole in mixtures.An gold nanocomposite(AuNPS-PDDA) subtrate was fabricated to obtain the SERS spectra signals of methotrexate and voriconazole,which were transformed into wavelet space by continuous wavelet transform（CWT）,then analyzed by features matching in wavelet space（FMWS）.This method could alleviate the influence of baseline variations and random noise,with detection limits for methotrexate and voriconazole of 1.0×10-8 mol/L and 2.86×10-4 mol/L,respectively.The feature matching coefficients for methotrexate and voriconazole were both higher than 0.96,which were significantly better than the traditional hit quality index.Besides,the actual ratio for two kinds of substance in the mixtures was determined by nonnegative least squares method,and the correlation between predicted values and real values was larger than 0.98.The results confirmed that the proposed method could be applied in the effective identification and semi-quantification of target compound in mixtures.关键词：surface-enhanced Raman spectroscopy;features matching;methotrexate;voriconazole
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发布时间： - 摘要：In this paper,the flowerlike MoS2/GO/o-MWNTs composites were synthesized by using Na2MoO4?2H2O as molybdenum source,thiourea as sulfur source and reducing agent,and mixed oxidized multi-walled carbon nanotubes(o-MWNTs) and graphene oxide(GO) as raw material,respectively.Then,the gold nanoparticles were deposited on the surface of MoS2/GO/o-MWNTs by in situ chemical reduction method.The characterization of this nanocomposites was performed by field emission scanning electron microscopy(FESEM),transmission electron microscopy(TEM),X-ray diffraction(XRD) and X-ray photoelectron spectroscopy(XPS).Results demonstrated that the MoS2/GO/o-MWNTs composites were synthesized successfully via the hydrothermal method,and gold nanoparticles were modified on the flower sheets.The nanocomposites were modified on the glassy carbon electrode(GCE) to investigate the electrochemical behavior for H2O2.The results showed that the electrode exhibited a strong catalytic activity toward H2O2，and there was a linear relationship between the electrode and H2O2 in the concentration range of 12.0×10-9-31.0×10-6 mol/L with a sensitivity of 56.6 μA/(mmol?L-1) and a detection limit of 12.0×10-9 mol/L.关键词：gold nanoparticles;MoS2;multi-walled carbon nanotubes;graphene oxide;H2O2
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发布时间： - 摘要：An analytical method was developed for the simultaneous determination of 38 antibiotics residues in 5 classes of drugs,including sulfonamides,quinolones,tetracyclines,chloramphenicols and macrolides in milk by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The samples were extracted with acetonitrile containing 0.5%(by volume) formic acid,and cleaned up with an Oasis PRiME HLB solid phase extraction column.The target components were separated using an Acquity UPLC HSS T3 column(100 mm×2.1 mm i.d.,1.8 μm),then identified and quantified by UPLC-MS/MS with electrospray ion source(ESI) under multi-reaction ion monitoring(MRM) mode.Results showed that 38 antibiotics had good linear relationships in their respective linear ranges with correlation coefficients(r2) higher than 0.99.The limits of quantitation for 38 antibiotics were between 0.10 μg/kg and 1.0 μg/kg.Average recoveries for 38 antibiotics in milk at spiked levels of 1.0,5.0,10.0 μg/kg ranged from 70.7%to 94.9%,with relative standard deviations(RSD,n=6) of 4.0%-9.4%.With the advantages of easy operation,high sensitivity and good reproducibility,the method was applicable for the determination of antibiotics residues in milk.关键词：milk;antibiotics;sulfonamides;quinolones;tetracyclines;chloramphenicols;macrolides;ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)
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发布时间： - 摘要：Two acylhydrazone based fluorescent probes 1 and 2 were synthesized.Probes 1 and 2 both showed an excellent selectivity toward Al3+ in DMSO-H2O(7∶3,by volome) solution at emission wavelengths of 478 nm and 460 nm,respectively.The stoichiometric ratios of 1∶2 for the Al3+ complexes were determined by Jobs plots,1H NMR titration experiments and LC-MS analysis.The detection limits of probes 1 and 2 for Al3+ were found to be 9.58×10-8 mol/L and 6.52×10-8 mol/L,respectively.The fluorescent sensing mechanisms for probes 1 and 2 to Al3+ were proposed.Furthermore,the applied research revealed that the probes 1 and 2 could be used for the detection of Al3+ in river water and tap water samples.关键词：acylhydrazone;fluorescent probe;synthesis;aluminum
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发布时间： - 摘要：In this paper,nitrogen-doped graphene quantum dots(N-GQDs) were prepared by one-step hydrothermal synthesis.Cu2+ ions were combined with the specific functional groups on surfaces of the quantum dots to form N-GQDs-Cu2+ complexes,which could quench fluorescence effectively.Furthermore,when 2-mercaptobenzothiazole(MBT) was added,Cu2+ were dissociated from the surface of the quantum dots due to the strong force of MBT and Cu2+,and the fluorescence from the quantum dots was recovered.Thus,a highly sensitive fluorescence sensor based on Cu2+ modified N-GQDsnitrogen-doped graphene quantum dots was constructed for the detection of MBT.Under the optimal experimental conditions,there was a good linear relationship between MBT and fluorescence recovery intensity in the concentration range of 0.4-40.0 μmol/L,and the limit of detection was 0.1 μmol/L.The method could be applied in the detection of MBT in real water samples with spiked recoveries of 95.0%-101%.关键词：nitrogen-doped graphene quantum dots(N-GQDs);fluorescent sensor;copper ion;2-mercaptobenzothiazole(MBT)
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发布时间： - 摘要：The conditions for extracting volatile components in Hippophae rhamnoides L.by headspace solidphase microextraction(HS-SPME) were optimized.Gas chromatography-mass spectrometry(GC-MS) was used to detect the extracts by HS-SPME and steam distillation(SD).Results showed that the optimum conditions for HS-SPME were as follows:the extraction temperature and the extraction time were 70 ℃ and 50 min,respectively,and the desorption time and the equilibrium time were 7 min and 20 min,respectively.Under this condition,76 components were identified from the HS-SPME extracts,accounting for 90.19% of the total,and the main components were esters,aldehydes and ketones,respectively,while 56 components were identified from the SD extracts,accounting for 91.98% of the total,and the main components were esters.20 common components were detected in both the extracts.There are great differences in the types and contents of volatile oil in Hippophae rhamnoides L.extracted by the two extraction methods.The HS-SPME is more suitable for the rapid detection of volatile components in Hippophae rhamnoides L.关键词：Hippophae rhamnoides L.;headspace solidphase microextraction(HS-SPME);steam distillation(SD);volatile components;gas chromatography-mass spectrometry(GC-MS)
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发布时间： - 摘要：A phenanthroline based fluorescent probe 1 was synthesized.The structure of the probe was characterized by nuclear magnetic resonance spectroscopy(NMR),masss pectrometry(MS) and infrared spectroscopy(IR),and the recognition performance of the probe toward Hg2+ and Ag+ was investigated by fluorescence emission spectroscopy.Results indicated that Hg2+ and Ag+ in pure water medium were recognized by the probe via fluorescence quenching with the ratios of 1∶1 and 2∶1,respectively.There were linear relationships for Hg2+ and Ag+ in the concentration ranges of 9.0×10-7-1.1×10-5mol/L and 8.0×10-7-7.0×10-6mol/L,respectively,with their correlation coefficients(r2) larger than 0.99.The limits of detection were both as low as 10-8 mol/L.A visual analysis method was established for the detection of trace Hg2+ and Ag+ using the probe based on the obvious changes of fluorescence intensity.The thermodynamic parameters and recognition mechanism were evaluated using isothermal titration calorimetry(ITC) and 1H NMR titration.This method has a potential application value for the real-time monitoring of Hg2+ and Ag+ in the biological and environmental fields.关键词：aqueous medium;phenanthroline derivative;fluorescence probe;Hg2+;Ag+
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发布时间： - 摘要：A novel,simple and effective method was developed for the detection of Cr6+ using a photoelectrochemical(PEC) sensor based on Fe∶TiO2 nanosheets in this paper.Fe∶TiO2 nanosheets was synthesized by hydrothermal method using C16H36O4Ti and FeF3 as raw materials,which were characterized by scanning electron microscopy(SEM),X-ray diffraction(XRD) and UV absorption spectroscopy(UV-Vis).Electrochemical methods were adopted to characterize the modified electrode.And the test conditions for Fe doped amount,Fe∶TiO2 concentration and bias voltage were investigated.Under the illumination of light,the Fe∶TiO2 nanosheets reduced Cr6+ to Cr3+.When Cr3+ reacted with OH-,Cr(OH)3 was formed and deposited on the surface of the electrode,resulting in the decrease of photocurrent so as to achieve the purpose of detection.Results showed that the linear range of the sensor for detection of Cr6+ varied from 0.008 μmol/L to 100 μmol/L(r2=0.999 5),with a detection limit of 0.004 μmol/L.The sensor was applied in the detection of actual samples with good sensitivity and selectivity.The spiked recoveries were in the range of 99.3%-119% with relative standard deviations(RSD) of 2.3%-2.8%,indicating that the photoelectrochemical sensor has a great application potential in the selective detection of Cr6+.关键词：Fe∶TiO2 nanosheets;photoelectrochemical sensor;Cr6+
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发布时间： - 摘要：A gas chromatography-triple quadrupole tandem mass spectrometry(GC-MS/MS) with dispersive solid phase extraction(d-SPE) was developed for the determination of azo colorants in paper.The azo colorants were reduced as aromatic amines after pretreatment.Sequentially,4 mL 10 mol/L sodium hydroxide solution,0.5 mL three internal standards(naphthalene-D8,2,4,5-trichloro-aniline and anthracene-D10)working solution,10 mL tert-butyl methyl ether and 15 g anhydrous sodium sulfate were added into the suspension to adjust the pH value from faintly acid to alkaline and absorb water.The aromatic amines were extracted with 10 mL tert-butyl methyl ether via 40 min thorough oscillation.The extract was further purified with d-SPE kits.After centrifugation,the supernatant was determined by GC-MS/MS in highly sensitive and selective multiple reaction monitoring mode(MRM),and quantified by internal standard method.There existed good linear relationships for the target compounds in respective concentration ranges,with their correlation coefficients(r2) larger than 0.99.The recoveries at three spiked levels of 10,20 and 50 ng/mL were between 80.7% and 128%,with the relative standard deviations(RSDs) of 0.79%-6.5%.The limits of detection(LODs) and limits of quantification(LOQs) were in the ranges of 0.05-2.1 ng/mL and 0.18-5.5 ng/mL,respectively.Results showed that the method was simple,rapid and sensitive,was applicable for the rapid detection of aromatic amines in paper.关键词：dispersed solid phase extraction(d-SPE);gas chromatography-triple quadrupole tandem mass spectrometry(GC-MS/MS);aromatic amines;paper
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发布时间： - 摘要：A method was developed for the simultaneous determination of chromium(Ⅵ) and chromium(Ⅲ) by high performance liquid chromatography-inductively coupled plasma mass spectrometry(HPLC-ICP-MS).The sample was extracted with 10 mmol/L EDTA solution(pH 7.0).The chromatographic separation was performed on an Agilent Bio-WAX column(4.6 mm×50 mm,5 μm) utilizing 0.075 mol/L nitric acid(pH 7.0) as mobile phase.Identification and quantitation were achieved by ICP-MS.Under the optimal conditions,the linear ranges for Cr(Ⅵ) and Cr(Ⅲ) were observed from 0 μg/L to 100 μg/L with correlation coefficients(r2) of 0.999 9.The limits of detection for Cr(Ⅵ) and Cr(Ⅲ) were 6 μg/kg and 2 μg/kg,and the limits of quantitation were 18 μg/kg and 6 μg/kg,respectively.Average recoveries for Cr(Ⅵ) and Cr(Ⅲ) at three spiked levels ranged from 85.1% to 113% with relative standard deviations of 0.4%-4.6%.Through the analysis of actual samples,Cr(Ⅵ) and Cr(Ⅲ) were detected out in cream lotion and powder cosmetics.With good reproducibility and high sensitivity,this method is suitable for the simultaneous determination of Cr(Ⅵ) and Cr(Ⅲ) in different types of cosmetics as Cr(Ⅵ) is stable under neutral conditions.关键词：high performance liquid chromatography-inductively coupled plasma mass spectrometry(HPLC-ICP-MS);cosmetics;chromium(Ⅵ);chromium(Ⅲ)
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发布时间： - 摘要：Taking the detection of three fat-soluble vitamins in human serum as an example,an analytical method for human endogenous metabolites was explored.A mixed human serum matrix was prepared by adding standard substances and internal standards followed by background subtraction of endogenous substances,and another simulating matrix substrate was made of bovine serum albumin(BSA).They both were detected by liquid chromatography-tandem mass spectrometry(LC-MS/MS).Results showed that the limits of detection for vitamin A,D3 and E in the mixed human serum matrix were 4.2,0.8 and 67.2 ng/mL,while the limits of quantitation were 13.7,2.6 and 221.9 ng/mL,respectively.There existed good linear relationships for the two methods with good accuracy and reproducibility,and their correlation coefficients were both above 0.996.The recoveries for the actual samples at low and high spiked concentrations were between 90.7% and 112%,with relative standard deviations(RSD) of 1.0%-4.5%.There were no statistical differences between the two methods for 40 unknown samples.Therefore,for the endogenous metabolites from human body,the accurate analysis on the matrix matched between the standard sample and the sample to test could be achieved by adding the standard substance and deducting the background from the human serum matrix,which is beneficial to the convenient diagnosis on clinical related diseases.关键词：fat-soluble vitamins;liquid chromatography-tandem mass spectrometry(LC-MS/MS);endogenous metabolite;human serum matrix
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发布时间： - 摘要：fabricated by a layer-by-layer assembly immobilizing the GO nanosheets onto capillary wall.The characterization on the colomn was carried out by measuring the electro osmotic flow(EOF) and Raman spectrum,etc.Based on this,an about 1 cm length of capillary electrochromatography trypsin micro-reactor was prepared by immobilizing the trypsin on end of capillary column through ion bonding.The performance of this technique was investigated.Results showed that the introduction of GO to the capillary column not only improved its separation efficiency on sample,but also promoted its enzyme catalytic performance.The separation degree of the GO-coated capillary on a mixture of N-benzuyl-L-arginine ethyl ester hydrochloride(BAEE) and N-benzuyl-L-arginine(BA) was increased from 3.70 to 4.71 compared with that of bare capillary.Meanwhile,the enzyme activity of immobilized enzyme with GO as carrier(Michaelis constant Km=1.10 mmol/L,the maximum reaction rate Vmax=0.32 mmol?L-1?s-1) was also enhanced significantly compared with that of the immobilized enzyme on unmodified capillary(Km=109.77 mmol/L,Vmax=0.000 46 mmol?L-1?s-1.The prepared trypsin micro-reactor was finally employed as a model for the screening of enzyme inhibitors from ten kinds of herbs in the crude extracts.Results showed that the Pseudo-ginseng and the Rheum officinale both contained trypsin inhibitor activity,which indicated that the prepared enzyme immobilized micro-reactor is a potential tool for rapid inhibitor screening.关键词：enzyme microreactor;graphene oxide;capillary electrochromatography;trypsin;inhibitor
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发布时间： - 摘要：A method of headspace gas chromatography-mass spectrometry(HS/GC-MS) was developed for the determination of eight volatile benzene homologues,i.e.benzene,toluene,ethylbenzene,p-xylene,m-xylene,isopropylbenzene,o-xylene and styrene in ball-point pen.The equilibrium temperature and time for headspace sampler were set at 70 ℃ and 40 min,respectively.The analytes were separated on an HP-INNOWax column(60 m×320 μm×0.25 μm),then detected in selected-ion monitoring mode and quantified by external standard method.Results showed that the standard curves for eight benzene homologues were linear over the concentration range of 0.005-0.05 mg/L with the linear correlation coefficients greater than 0.999.The detection limits of the method(S/N=3) were in the range of 0.01-0.02 mg/kg.The spiked recoveries ranged from 86.0% to 104% with RSDs of 2.3%-9.6%.The method is simple,rapid and high sensitive,and is suitable for the determination of volatile benzene homologues in ball-point pen.关键词：headspace gas chromatography-mass spectrometry(HS/GC-MS);ball-point pen;benzene homologues
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发布时间： - 摘要：As a pre-concentration method with the advantages of simplicity,high efficiency and low consumption,gas phase enrichment techniques(GPE) have become the key factors for various atomic spectrometers to enhance analytical sensitivity and eliminate matrix interference for the purpose of instrumental miniaturization and on-site analysis.Samples have to be converted into gaseous analytes for the sample introduction of GPE by means of hydride generation,ultraviolet vapor generation and electrothermal vaporization,then the elements for measurement are trapped or released with materials like quartz,carbon and metal,etc.,of which the trapping or releasing approaches are also the crucial factors for GPE,such as cold trapping,alloy trapping,thermal trapping and dielectric barrier discharge,etc.Hereon,the development progresses of GPE in atomic spectrometry are discussed,including the sample introduction,trapping materials and trapping or releasing approaches.Furthermore,the prospectives for research and application of GPE techniques are proposed as well.关键词：gas phase enrichment;atomic spectrometry;elemental analysis;sample introduction;trapping/releasing
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发布时间： - 摘要：With the continued development of green chemistry,how to apply and reflect the characteristics of green chemistry in analysis process,avoiding the secondary pollution of the analysis process and the possible harm to the analysts have received an extensive attention.Therefore,the development and use of solvents with green chemistry characteristics is one of the main work for analysts.Deep eutectic solvents(DESs) are another type of solvents with similar physical properties to ionic liquids(ILs).Compared with ILs,DESs have showed some advantages such as environmental friendliness,non-combustibility,biodegradablity,low cost and simple preparation,etc.DESs have been used as green solvents in the extraction and separation of target compounds in different samples.The preparation,properties and classification of DESs are summarized this review,and their applications in extraction and separation are also presented.关键词：green chemistry;deep eutectic solvent;extraction separation;review
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