最新刊期

    38 5 2019
    • Vol. 38, Issue 5, Pages: 503-509(2019)
      摘要:A two-component signal transduction system is the most important signal transduction system for bacteria to cope with external stimuli and self regulate physiological activities.Histidine kinase is an important component of the two-component signal transduction system.Most histidine kinases are multifunctional,they could autophosphorylate and then deliver phosphate groups to the cognate response regulators(RR),and they could also catalyze the dephosphorylation of the response regulator proteins.It is found that the dephosphorylation activity of histidine kinase HK853 is pH dependent.The pH regulation mechanism of HK853 is investigated by using selectively isotopic labeling and NMR spectroscopy.It is revealed that the pKa value of His260 side chain involved in the interaction has a good relationship with the pH dependent phosphatase activity of HK853,which will decrease after HK853 forms a complex with the substrate.The deprotonated imidazole ring plays an important role in the catalytic reaction.This change contributes to the enhancement of HK853 phosphatase activity,ensures the efficiency of acid-base regulation and clarifies the acid-base regulation mechanism of HK853 when performing phosphatase function.  
      关键词:NMR;site-selective labeling;two-component signal transduction system;phosphorylation;histidine kinase   
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    • Vol. 38, Issue 5, Pages: 510-516(2019)
      摘要:Hindered by the difficulties in preparation and purification,it is always a challenge to obtain the gold nanotriangles(AuNTs) products with purer and better morphology.In this paper,a method was systematically proposed for the rapid fabrication of triangular gold nanoparticles with various sizes,single morphology and less rounded corners by centrifuge accelerated depletion effect using cetyltrimethylammonium chloride(CTAC) as flocculant.The optimum concentrations of flocculant for different sizes of gold nanotriangles were found by using UV-Vis spectrophotometer to compare the colors and the extinction spectra of supernatant and redispersed precipitate colloids obtained with different concentrations of flocculant.By comparing the morphology variations of the nanoparticles before and after purification with transmission electron microscope(TEM),the limitations for the existing purification method through natural precipitation overnight were found,which took a long time and had a significant impact on the morphology of the particles.Results showed that the method could not only achieve a rapid and efficient purification toward the gold triangular nanoparticles with different sizes,but also effectively reduce the tip loss of nanoparticles in the purification process.Especially for the triangular nanoparticles with small sizes containing side length less than 50 nm,the tips of particles purified by centrifuge accelerated depletion induced coagulation could still maintain their sharpness.This method is simple and efficient for the separation of triangular gold nanoparticles.And it is expected to be extended to the purification of nanoparticles of other components,non spherical and low symmetry shapes.  
      关键词:depletion effect;centrifugation;gold nanoparticles;gold nanotriangles;self assembly;flocculation;precipitation   
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    • Vol. 38, Issue 5, Pages: 517-524(2019)
      摘要:A rapid,simple and visual lateral flow test strip(LFTS) based on gold nanostars(AuNSs) was fabricated for the detection of human immunodeficiency virus DNA(HIV-DNA) in this paper.The AuNSs as a color label for visual detection were synthesized by an environmentally friendly chemical method.The “sandwich structure” was utilized in the measurement process:the target was firstly captured with the DNA modified AuNSs,then trapped on the test line in accordance to the principle of complementary base pairing.Afterwards,the variation of the color on test line could be visually observed for qualitative and semi-quantitative analyses,and a portable strip reader recording the color intensity of the band was used for quantitative analysis.Under the optimum conditions,this AuNSs based LFTS strategy presented a good linear relationship for target DNA in the range of 0.2-50 nmol/L with a detection limit of 0.14 nmol/L,which sensitivity was 5 fold higher than that of the traditionanl gold nanoparticles test strip.Moreover,this LFTS exhibited a good anti-interference ability in the detection of HIV DNA in human serum,which meant it has a great potential in early diagnosis and treatment.  
      关键词:gold nanostar;lateral flow test strip;human immunodeficiency virus DNA(HIV-DNA);visual detection   
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    • Vol. 38, Issue 5, Pages: 525-531(2019)
      摘要:A Fourier transform ion cyclotron resonance mass spectrometry(FTICR-MS) with cluster analysis and principal components analysis(PCA) was developed for the identification of chemical constituents in Ganoderma lucidum and the analysis of its fingerprintings used for origin differentiation.The Ganoderma lucidum samples were extracted with a reflux using 50% methanol as solvent,then analyzed directly by FTICR-MS.The MS spectra were recorded at m/z 100-1 000 Da with ESI source under a negative ion detection mode.The chemical constituents in Ganoderma lucidum were identified by accurate mass determination in MS/MS experiments,and total of sixty-three active ingredients,including one terpene aldehyde,three sugars,four triterpene alcohols,six organic acids and forty-nine triterpene acids,were identified by comparing their mass spectrometric inforamtion with those of reference compounds and literatures.The Ganoderma lucidum samples derived from different origins were distinguished by cluster analysis and PCA,and a good origin differentiation was obtained under 95% confidence interval.Experimental results showed that the developed method could be applied in the rapid,direct and efficient analysis of Ganoderma lucidum and its fingerprintings,and was a promising approach for analysis of traditional Chinese medicine.  
      关键词:Ganoderma lucidum;Fourier transform ion cyclotron resonance mass spectrometry(FTICR-MS);chemical constituent identification;fingerprint analysis;origin differentiation   
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    • Vol. 38, Issue 5, Pages: 532-538(2019)
      摘要:A comprehensive analytical method was developed and validated for the simultaneous and rapid determination of nine exogenous impurities in edible oils by ultra high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS).The analytes in sample were extracted with acetonitrile using vortex mixer.The chromatographic separation was performed on an XSelect-HSS PFP chromatographic column(100 mm×2.1 mm,3.5 μm),with 5 mmol/L ammonium formate and acetonitrile as mobile phases by gradient elution.The qualitative and quantitative analyses were performed by electrospray ionization mass spectrometry in positive mode under multiple reaction monitoring(MRM) mode.Results showed that there were good linear relationships for nine analytes in corresponding concentration range with their correlation coefficients(r2) larger than 0.996.Average recoveries for 9 analytes in sample at three spiked levels ranged from 68.2% to 104%,with relative standard deviations(RSD) of 2.2%-12%.The limits of detection(LOD,S/N≥3) and quantitation(LOQ,S/N≥10) were in the ranges of 0.02-0.10 μg/kg and 0.05-0.25 μg/kg,respectively.The established method is simple,rapid,sensitive,accurate and reliable,and is suitable for the simultaneous and rapid determination of nine exogenous characteristic impurities in edible oils.  
      关键词:ultra high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS);edible oils;exogenous impurities;capsaicin;piperine;6-gingerol;hydroxy-α-sanshool   
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    • Vol. 38, Issue 5, Pages: 539-545(2019)
      摘要:Gene engineering technology has become a key technique for research and production of recombinant human serum albumin(rHSA) replacing human serum albumin(HSA),while the methods for rHSA purification are the key point to this technique.A novel method for rHSA purification from transgenic pig plasma was introduced in this paper,in which thermal ethanol precipitation combined with multi stage liquid chromatography was chosen for rHSA purification.The rHSA was firstly extracted from pig plasma by the modified thermal ethanol precipitation method,with its purity and recovery of 69.5% and 51.3%,respectively.Then,the crude extract was further purified by multi stage liquid chromatographic techniques,i.e.anion exchange chromatography and reversed phase chromatography,with the purity and recovery for rHSA actually up to 100.0% and 41.1%,respectively.This method provides an opportunity for the large scale purification of rHSA from transgenic pig plasma for clinical and biochemical research,and lays a foundation for the application of rHSA in place of HSA.  
      关键词:recombinant human serum albumin(rHSA);purification;thermal ethanol precipitation;multi-stage liquid chromatographic techniques   
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    • Vol. 38, Issue 5, Pages: 546-551(2019)
      摘要:A matrix assisted laser desorption/ionization time of flight mass spectrometric(MALDI-TOF MS) method with N alkylpyridinium isotope quaternization(NAPIQ) was developed for the rapid identification of microbial contamination in herbs in this paper.The sterols in herbs were extracted with chloroform,and then derivatized with three reagents,ie.pyridine,D5 pyridine and trifluoromethanesulfonic anhydride.The derivatization could significantly enhance the ionization of sterols in the analysis by MALDI-TOF MS.Only phytosterols such as sitosterols and stigmasterols in the fresh traditional Chinese medicine were detected by this method,while the zoosterols and the mycosterol such as lanosterol and ergosterol were observed in the mass spectra of moldy herbs.Furthermore,the method was compared with the microbial enumeration method in Chinese Pharmacopoeia(2015 edition).No molds in the fresh herbs were detected by the microbial enumeration method,while the microbial counts in the moldy herbs significantly exceeded the threshold of 102 cfu/g.Results showed that the MALDI-TOF MS combined with NAPIQ provided an alternative method for the identification of potential moldy herbs.  
      关键词:herbs;microbial contamination;phytosterols;zoosterols;NAPIQ;matrix assisted laser desorption/ionization time of flight mass spectrometry(MALDI-TOF MS)   
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    • Vol. 38, Issue 5, Pages: 552-557(2019)
      摘要:Microchip electrophoresis has shown its potential of application in many fields,but its utilization in real world is still limited.To achieve a successful separation on a microchip through electrophoresis,many details have to be carefully taken into account,such as the liquid levels of each reservoir,the exact location of each electrode etc.,skillful operation is therefore required.In this paper,branched microchannels were introduced at the inlet end of the sampling channel and the outlet of the separation channel of traditional microchips for electrophoresis with a cross configuration.Additional reservoirs were made,and the liquid levels of these two reservoirs were lower than that of the sample reservoir and the buffer waste reservoir,maintaining continuous refreshing at the branched points through siphoning.With 2 fluorescein isothiocyanate labeled organophosphorus herbicides,ie.glyphosate and glufosinate,and a degradation product,(aminomethyl)phosphonic acid,the applicability of the proposed microchip was investigated.Results showed that with this kind of microchips,several improvements could be achieved.Firstly,the injection time for the consecutive analysis with pinched injection could be shortened due to its effectiveness to prevent the dilution of the sample in the sampling channel by the buffer during the separation periods.Secondly,the baseline drift due to the entrance of separation waste back to the detection point during the injection periods could be effectively eliminated.Thirdly,the repeatability of the consecutive analysis was therefore significantly improved,120 times of consecutive injection gave a relative standard deviation(RSD) of peak height as low as 056%(calculated for(aminomethyl)phosphonic acid) with replenishing of the buffer and sample every 40 injections.More importantly,by using the proposed microchip,a pre separation could be performed by controlling the injection time.Components migrating slower in the sample could be excluded from the injection into the separation channel,making it possible to get rid of most of sample matrix by tuning the separation condition to make analytes migrate faster than the matrix components.This kind of pre separation could simplify the electropherogram and avoid possible contamination of the separation microchannel,which is also beneficial to the reliability of microchip electrophoresis.  
      关键词:microchip electrophoresis;pinched injection;microchannel;organophosphorus herbicide;repeatability   
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    • Vol. 38, Issue 5, Pages: 558-562(2019)
      摘要:Ferron dosage([Ferron]) has a significant effect on the accurate determination of Al3+ concentration and its speciation by Ferron colorimetric method.However,the importance of this most critical factor has not been clearly realized.Different Ferron concentrations have been used in Al-Ferron system by researchers from different laboratories.Various molar absorption coefficient ε values for different Ferron concentrations have been obtained,which have affected the accuracy for determination of Al speciation in polyaluminum chloride(PAC) solution unavoidably.Systematic and comprehensive studies were conducted in this work.It is found that the molar absorption coefficient ε increases in exponential form with the increase of [Ferron] in mononuclear Al solution.ε-could be regarded as the maximum value at a plateau from “ε-[Ferron]” curves when [Ferron] reaches to 2.0×10-3 mol/L.The suitable [Ferron] range is from 2.0×10-3 mol/L to 3.0×10-3 mol/L,and 2.0×10-3 mol/L is the recommended optimal dosage achieving the most sensitive and accurate results.  
      关键词:Al-Ferron colorimetric method;Ferron dosage;ε-[Ferron] curve;mononuclear Al concentration   
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    • Vol. 38, Issue 5, Pages: 563-568(2019)
      摘要:A metal-organic framework ZIF-8@Fe3O4 composite was synthesized for the extraction of endocrine disrupting chemicals(EDCs) in water samples by magnetic solid phase extraction(MSPE).Effects of ZIF-8 growth cycles,extraction time,ionic strength,pH,desorption solvent and desorption time on MSPE were investigated.The developed MSPE combined with high performance liquid chromatography was successfully applied in the detection of 4 endocrine disrupting chemicals(EDCs),i.e.bisphenol A,nonyl phenol,octyl phenol and estrone in water samples.Under the optimized conditions,there existed linear relationships for the 4 analytes in the range of 1.0-1 000 μg/L,with the detection limits(S/N=3) of 0.42-0.81 μg/L and the enhancement factors of 61-144.The relative standard deviations(RSDs) for inter-day(n=6) and intra day(n=3) were 2.1%-4.3% and 3.5%-5.8%,respectively.  
      关键词:metal-organic frameworks;composite;magnetic solid phase extraction;endocrine disrupting chemical   
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    • Vol. 38, Issue 5, Pages: 569-573(2019)
      摘要:A fourier transform ion cyclotron resonance mass spectrometry(FT-ICR-MS) was developed for the qualitative analysis of unknown components in an imported aluminum sealer as surface treatment agent,which was processed from a variety of ingredients.Naphthalene sulfonate,nickel acetate,sodium benzoate and other components were discovered in this kind of product.Through the precise molecular ion data derived from FT-ICR-MS analysis and the isotope fine structure,the unknown material ion formula was inferred.Then,combined with inductively coupled plasma mass spectrometry(ICP-MS) and gas chromatography-mass spectrometry(GC-MS) analysis,the structures of unknown components were deduced.In addition,another two groups of unknown masses in the mass spectra with a difference of 62:234.8,296.8,358.9 and 410.7,472.7,534.7,combined with two-stage mass spectrometry,could be concluded to derive from the polymerization of nickel acetate with formic acid and benzoic acid,and some dimer and trimer ions were produced simultaneously.The attribution of all ions in the mass spectra of this product was certified,and most of the components in this product were analyzed.A new train of thought and method for the analysis of unknowns in chemical products was provided in this paper,and it could be used for the qualitative identification of unknowns in complex systems,and the ionization law about the metal ion of nickel combined with organic acid ionized in mass spectrometry was also founded.  
      关键词:fourier transform ion cyclotron resonance mass spectrometry(FT-ICR-MS);imported aluminum sealer(surface treatment agent);nickel acetate;the analysis of unknowns   
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    • Vol. 38, Issue 5, Pages: 574-580(2019)
      摘要:A novel colorimetric method for iron ion(Fe3+) detection was proposed by using asymmetrically modified Janus gold nanoparticles(Janus AuNPs) in this paper.Initially,citrate stabilized AuNPs with relatively large size were prepared through reduction reaction.Then,the large sized citrate stabilized AuNPs were immobilized on the glass slide,through which some binding sites on the surface of AuNPs were concealed.The stabilizing agent of polyethylene glycol(PEG) was further introduced onto the exposed surface of AuNPs to obtain the PEG and citrate asymmetrically modified Janus AuNPs.After the introduction of Fe3+,the aggregation behavior of Janus AuNPs was adjusted in an oriented and controllable manner to form oligomers which could remain stable in aqueous solution for a long time.Such an asymmetrical modification could significantly improve the dynamic detection range(1 μmol/L-10 mmol/L) of AuNPs based colorimetric assay.Meanwhile,a linear calibration curve,i.e.A750/A536=0.129c(μmol/L)+0.317 was also obtained,with a detection limit of 715 nmol/L.Compared with other nanoparticle based colorimetric system for Fe3+detection,this method is simple and sensitive,and surprisingly broadens the linear range for detection.  
      关键词:Janus gold nanoparticles;asymmetrical modification;oriented aggregation;iron ion;colorimetric detection   
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    • Vol. 38, Issue 5, Pages: 581-585(2019)
      摘要:A fluorescent analytical method for the detection of trace Fe2+ and Fe3+ in water was established using ellagic acid(EA) as fluorescent probe.The effects of common metal ions,methanol concentration and pH value of media on the quantitative detection of Fe2+ or Fe3+ were investigated in detail.Results illustrated that a good linear relationship between the flourescence quenching and the concentrations of Fe2+ and Fe3+ was obtained within the range of 0.08-1.1 μmol/L with the detection limits of 72 nmol/L and 63 nmol/L,respectively.Meanwhile,Fe2+ could be detected accurately without significant interference using 10 mmol/L ammonium tartrate to mask Fe3+.In addition,the Job's plot analysis showed that the coordination ratios for EA to Fe2+ or Fe3+ were 1∶3 and 1∶2,respectively.The established method was used in the detection of Fe2+ and Fe3+ in tap water and Zhujiang River water with average recoveries of 81.0%-116%.  
      关键词:ellagic acid;fluorescent probe;ferrous/ferric ions;detection   
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    • Vol. 38, Issue 5, Pages: 586-594(2019)
      摘要:Alkaloids are a class of natural compounds with good pharmacological properties.In the field of separation science and technology,alkaloid separation has always been a hot and difficult problem.In recent years,with the development of high performance liquid chromatography(HPLC) materials and separation methods,great progresses in alkaloid analysis and preparation have been achieved.In this article,the theoretical development and technological advances with respect to peak tailing problems of basic compounds are summarized,and the applications of HPLC in natural alkaloid analysis and preparation are discussed.The further development of HPLC separation on alkaloids is also looked forward.  
      关键词:alkaloids;peak tailing;preparative HPLC;orthogonal separation   
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    • Vol. 38, Issue 5, Pages: 595-602(2019)
      摘要:Electrogenerated chemiluminescence cytosensors,with the advantages of high sensitivity,strong reaction controllability,low background interference,real time analysis and nondestructiveness to the targets,have become a research hotspot in fields of biological analysis and clinical diagnosis in recent years.In this review,the discussion is focused on their applications in quantitative detection of cancer cells and tumor markers,single cell and cell function analysis through the construction of electrogenerated chemiluminescence cytosensors and the design of nanoluminescent probes.Simultaneously,the research trend for electrogenerated chemiluminescence technology in cell sensing is prospected.  
      关键词:electrogenerated chemiluminescence;electrochemiluminescence probe;cytosensor;tumor marker;cell analysis   
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    • Vol. 38, Issue 5, Pages: 603-611(2019)
      摘要:The research and application progresses of near infrared spectroscopy(NIR) analytical technique in China in the past five years(2014-2018) are reviewed in this paper.It includes progresses on the methodology,research and development of hardware and software,characteristics and trends of NIR applications in typical fields,with 97 references cited.The development trends for near infrared spectroscopy technique in China in the near future are proposed and discussed.  
      关键词:near infrared spectroscopy;chemometrics;portable analysis;on-line analysis;review   
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    • Vol. 38, Issue 5, Pages: 612-617(2019)
      摘要:Raman spectroscopy techniques have been widely used in field of on site fast detection owing to their unique advantages such as simplicity,rapidness,nondestruction,abundant fingerprint information and low aqueous interference,etc.Especially,surface enhanced Raman spectroscopy(SERS) technique has significantly improved the sensitivity for on site detection,and further complemented the ultrasensitive application.Herewith,a comprehensive overview on applications of Raman spectroscopy techniques in on site fast detection was presented.This review was divided into two parts,ie.direct and indirect detections,including typical Raman sensing strategies for food security,criminal investigation,biomedicine management,and environmental regulation.Finally,the tendency for future development of Raman spectroscopy techniques in on site fast detection was proposed.  
      关键词:Raman spectroscopy;surface enhanced Raman spectroscopy(SERS);on-site fast detection   
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    • Vol. 38, Issue 5, Pages: 618-623(2019)
      摘要:In recent years,chiral porous organic frameworks(CPOFs) materials have been applied in fields such as chiral catalysis,recognition and separation owing to their outstanding porous properties,high specific surface area,good stability,easy to be functionalized,etc.Chiral porous organic frameworks materials include chiral metal organic frameworks(CMOFs),chiral covalent organic frameworks(CCOFs) and their composites,which have special chiral recognition and adsorption.These materials have become one of the research hotspots in the field of chromatographic separation and analysis.In this paper,the synthesis of chiral porous materials and their applications in chromatographic separation and selective adsorption are reviewed.The possible applications and development directions of CPOFs materials in future are prospected.  
      关键词:chiral porous organic frameworks (CPOFs);chromatographic separation;selective adsorption;review   
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    • Vol. 38, Issue 5, Pages: 624-630(2019)
      摘要:Bisphenol-diglycidyl ethers(BDGEs) may pose a potential threat to humans due to its widespread use and the mutagenicity and teratogenicity observed in vitro and in vivo studies.The sample treatment methods and detection methods for BDGEs in canned foods and biological matrices are discussed in this paper.Furthermore,the future development tendency for analysis of BDGEs is prospected.  
      关键词:canned foods;biological matrices;bisphenol-diglycidyl ethers;pretreatment methods;detection methods   
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    • Vol. 38, Issue 5, Pages: 631-634(2019)
      摘要:The development course of electron microscopy(EM) and its new functions in recent years are introduced in this article.In bio nanomaterials research,EM could be employed to carry out morphology characterization and in situ chemical analysis,but higher standards of experimental methods are necessary because of the diversity of biomaterials,the complexity of newly created nanostructures and their functionalities tightly connected with living cells/organs.Therefore,the strategies to develop advanced EM hardware and software required by these specialties of bio nanomaterials are systematically explained.Besides,the development directions for EM in field of bio nanomaterials research such as large size mosaic image with high resolution,three dimensional modeling of tiny and complicate structures,real time and in situ characterization and analysis during experiments are prospected.  
      关键词:electron microscopy;transmission electron microscope;scanning electron microscope;bio nanomaterials   
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