摘要:To investigate the potential immunomodulatory mechanism of low molecular weight seleno aminopolysaccharide,an untargeted metabonomics method based on ultra high performance liquid chromatography-time of flight mass spectrometry(UPLC-TOF-MS) was developed for analysis of the variations of spleen endogenous metabolites in Acathopagrus schlegelii after they were extracted with frozen methanol,then isolated with a C18 column and a HILIC column,respectively.The potential biomarkers were screened out by non-targeted mass spectrometry with XCMSplus software and Metabolite HR MS2 library,and the related metabolic pathways were analyzed by Metabo Analyst 4.0 website.Results showed that the spleen metabolites in the group fed with the low molecular weight seleno aminopolysaccharide were significantly different from those in the blank group,and 36 biomarkers were found and identified.Low molecular weight seleno-aminopolysaccharide could enhance the immune function of Acathopagrus schlegelii through 9 metabolic pathways.This study provides a scientific basis for elucidating the immunoenhancement mechanism of low molecular weight seleno aminopolysaccharide.  
关键词:ultra high performance liquid chromatography-time of flight mass spectrometry(UPLC-TOF-MS);metabonomics;Acathopagrus schlegelii;low molecular weight seleno-aminopolysaccharide;immunomodulatory
摘要:Effects of fabric testing thickness,equipment running speed,scan integration time and scan times on the online near infrared detection of equipment were discussed by using a self developed “high efficiency identification and sorting device for the main components in fiber products”.The online near infrared spectrum was compared with the offline spectrum acquired using a raster type near infrared spectrometer.Although the resolution of the online near infrared spectrum of each kind of fabric was reduced,there were obvious characteristic absorption peaks,and the repeatability for the acquired spectrum was good,which indicated that the device could be used for online identification and sorting of fabrics.The best detection conditions were as follows:the test thicknesses for the tight woven fabric samples and the loose knitted fabric samples:1 mm or more and 2.5 mm or more,respectively,the equipment running speed:0.41 m/s,scan integration time:1 millisecond(ms),and the scan times:10 times.The test conditions obtained provided a reference for the online detection of the subsequent fiber fabric.  
关键词:fiber fabric;online near infrared;influencing factors;detection conditions
摘要:Size distribution of particles and their associated polycyclic aromatic hydrocarbons(PAHs) from indoor burning source is one of the most important factors for the risk assessment of human breathing exposed to indoor burning smoke.In this study,smokes of incense,mosquito coil incense,moxa and cigarette burning were simulated in a chamber,respectively.The smoke particles were collected with a MOUDI sampler and used for further PAHs analysis.In addition,an airborne particle counter was used to monitor the indoor particle number concentrations of moxa and cigarette smokes.The emission factors for particles varied in the range of 3.68-22.46 mg/g,and the size distribution peaked at 0.25-0.44 μm.As for the US EPA 16 priority PAHs,the emission factors ranged from 10.52 μg/g to 91.30 μg/g.The size distribution of PAHs from moxa smoke peaked at 0.44-1.0 μm,which was slight higher than those from other burning sources.The toxic equivalency(BaPTEQ) for benzo[a]pyrene(BaP) in particles less than 1 μm accounted for 85%-98%.The source characteristics ratios showed that moxibustion,cigarette smoke and incense burning could be categorized into biomass burning.The indoor particle number concentrations increased rapidly after the cigarette and moxa were lighted,then reached the maximum when they were burned out,and finally decreased exponentially in 4 h.Furthermore,the number concentrations of particles less than 0.3 μm decayed the fastest.  
关键词:indoor pollution;burning simulation;particulate matter;polycyclic aromatic hydrocarbons(PAHs);size distribution
摘要:An analytical method was developed for the non directional screening of 34 residues in 7 categories of veterinary drugs by ultra high performance liquid chromatography-hybrid quadrupole-orbitrap mass spectrometry(UHPLC-Q-Orbitrap MS) based on mass spectrometry fragmentation.The qualitative screening of the analytes was performed by MS in a data independent acquisition mode,based on retention time,accurate mass number,secondary fragmentation information of 34 veterinary drug standard substances.The characteristic fracture fragments of 7 categories of veterinary drugs were obtained by exploring the molecular ion mass spectrometry rupture process and cracking mechanism.A method for untargeted screening of target and non target substances in deep processed lamb products was established by combining the compound database with characteristic ion fragments in the data independent collection mode.Results showed that there were good linear relationships for 34 veterinary drugs in respective concentration ranges with their correlation coefficients(r2) larger than 0.99.The limits of detection and quantitation were 0.04-4.76 μg/kg and 0.07-8.24 μg/kg,respectively.Average recoveries at three added levels ranged from 79.4% to 110%,with relative standard deviations(RSD) of 0.30%-7.5%.The method was applied in the non directional screening of veterinary drug residues in commercially available deep processed lamb samples,and difloxacin outside the standard library was also detected beside sulfamethazine.Hence,the proposed method is simple and efficient,and could be employed for accurate determination of veterinary drug residues in lamb products.  
关键词:ultra-high performance liquid chromatography-hybrid quadrupole-orbitrap mass spectrometry(UHPLC-Q-Orbitrap MS);non-directional screening;veterinary drug residues;deep processed lamb products
摘要:Milk powder authenticity is one of the critical issues in food safety,which non-directional screening remains a hotspot and frontier in analytical science.A robust model driven Raman hyperspectral imaging method(RMD-RHIM) for the non-directional screening of milk powder authenticity was proposed by utilizing the spectral features and spatial features of milk powder samples efficiently,which enabled RMD-RHIM to identify the unknown adulterants in milk powder as outliers,thus avoiding to estimate the uncertainty of numerous adulterants.In RMD-RHIM,the adaptive iterative reweighted penalized least square(airPLS) was adopted to suppress the background information in Raman spectra,and then modified iterative reweighted partial least square(mIRPLS) was used to detect outliers in thousands of Raman spectra.As a result,RMD-RHIM was capable of identifying any adulterant in milk powder as an outlier,which was illustrated as a distorted pix in binary image.The classification accuracies of RMD-RHIM for positive and negative samples were 98.3% and 93.3%,respectively.The results obtained indicated that RMD-RHIM was a promising tool for the non directional screening of milk powder,which may be well extended to other food systems.  
关键词:Raman hyperspectral image;milk powder authenticity;robust model driven;non-directional screening
摘要:A photoelectrochemical aptamer sensor for the detection of oxytetracycline(OTC) was constructed with nano-TiO2/graphene composites as photoelectric sensor substrate.Firstly,the nano TiO2 was synthesized by hydrothermal method on the fluorine doped tin dioxde(FTO) conductive glass.Then the graphene oxide was reduced to graphene by the simple electrochemical method,which was deposited on the surface of TiO2/FTO.The morphology of the obtained TiO2/graphene composites was characterized by scanning electronic microscopy(SEM).The electrochemical working station was applied to measure the photoelectric response.Results showed that the TiO2/graphene composite material could obviously increase the photoelectric current and improve the sensitivity.Based on the fact that the oxytetracycline aptamer could specifically recognize oxytetracycline,it was immobilized on the surface of TiO2/graphene nanocomposite modified FTO electrode for oxytetracycline detection.The method was applied in the detection of oxytetracycline with a linear range of 5.0×10-9-5.0×10-6 mol/L(r=0.988 7) and a detection limit of 1.0×10-9 mol/L.With the advantages of simplicity,low cost and wide linear range,the method is applicable for the determination of oxytetracycline residues in real samples.  
摘要:In this study,a “turn off” fluorescent sensor based on aptamer functionalized grapheme oxide(GO) decorated gold nanoparticles(AuNPs) composites was developed for the detection of Hg2+.Firstly,the GO@AuNPs with certain fluorescence properties were fabricated by wet chemical method,then the sulfhydryl modified single chain T-rich nucleic acid DNA(aptamer) was immobilized on the surface of gold nanoparticles to form aptamer functionalized graphene oxide decorated gold nanoparticles complexes(aptamer-GO@AuNPs).In the presence of Hg2+,due to the coordination of seven T-Hg2+-T structures,T-rich aptamer was folded to form a rigid and double stranded hairpin structure,making coordinated Hg2+ close to the graphene surface(less than 1 nm).In that case,electrons could transfer from graphene to mercury ion along the double stranded DNA channel,which caused the graphene fluorescence quenched.Based on this,a “turn-off” fluorescence sensor was constructed.Under the optimal experimental conditions,the linear detection range for Hg2+ was 0.5-80 nmol/L,and the detection limit was 0.3 nmol/L.The method was applied in the detection of Hg2+ in environmental water samples.The recoveries ranged from 96.0% to 105% with the relative standard deviations of 1.4%-3.2%.With the advantages of simple operation,strong anti-interference,high sensitivity and selectivity,label-free and rapid detection,the method could be used for the high sensitive detection of Hg2+ in environmental water samples.  
摘要:CdSe/CdS quantum dots(CdSe/CdS QDs) were prepared using thioglycollic acid(TGA) as stabilizer.A method was established for the rapid determination of cyromazine(Cyr) residues in pepper,cowpea,balsam pear,cucumber and cherry tomato using the CdSe/CdS QDs as a fluorescence probe,based on the phenomenon that the enhanced fluorescence of CdSe/CdS QDs was observed in the presence of Cyr.Experimental conditions for the determination of Cyr in five vegetables were optimized,including concentration of QDs,pH value,reaction time and coexistence substances.Results showed that the emission wavelength(λem) for CdSe/CdS QDs was 580 nm when the excitation wavelength(λex) was set at 481 nm.Under the optimum conditions,the established method exhibited a good linear in the range of 5.0-120 nmol/L with correlation coefficients(r) not less than 0.999 1.The limits of detection(LOD,S/N=3) and limits of quantitation(LOQ,S/N=10) were 0.8-1.4 nmol/L and 2.4-46 nmol/L,respectively.Recoveries at three spiked levels of 4,40,100 μg/kg ranged from 82.5% to 108% with relative standard deviations(RSD,n=3) not more than 6.9%.With the advantages of high selectivity,good sensitivity and simple operation,the method was successfully applied in the determination of Cyr in five real vegetables.  
摘要:An effective method was established for the simultaneous determination of fifteen glycol ethers and four glycol ether acetates residues in dyeing and finishing additives by gas chromatography-tandem mass spectrometry(GC-MS/MS).Residual glycol ethers and their acetates in dyeing and finishing additives were ultrasonically extracted with ethyl acetate as extraction solvent.The extract was then purified using a Waters Sep-Pak Vac Silica(1 g/6 mL) solid phase extraction(SPE) column.The chromatographic separation of 19 target compounds was performed on a DB-Wax(60 m×0.25 mm×0.25 μm) column.GC-MS/MS analysis was carried out in multiple reaction monitoring(MRM) mode,and the concentrations of glycol ethers and their acetates were calibrated by the external standard method.The peak areas(A) for the analytes were linearly related to their mass concentrations(ρ) in each linear range,and the correlation coefficients were no less than 0.999 2.The limits of detection(LODs) and quantitation(LOQs) of the method were calculated by the signal to noise(S/N) ratios of three and ten,respectively.LODs for MOPA and DEGME were both 30 μg/kg,LOD for DEGDEE was 20 μg/kg,LODs for EGEE and EGME were 10 μg/kg,and LODs for the other fourteen target compounds ranged from 1 μg/kg to 5 μg/kg,while LOQs for EGEE,EGME and DEGDEE were 20,30 and 50 μg/kg,respectively,while that for MOPA and DEGME were both 100 μg/kg,and LOQs for the other fourteen varied from 1 μg/kg to 15 μg/kg.The average recoveries at three spiked levels ranged from 82.4% to 94.6% with the relative standard deviations(RSDs) of 2.7% to 9.2%.The proposed method was simple and sensitive,and could meet completely the demands for routine analysis of residual glycol ethers and their acetates in dyeing and finishing additives.  
关键词:gas chromatography-tandem mass spectrometry(GC-MS/MS);dyeing and finishing additives;glycol ethers;glycol ether acetates;ultrasonic extraction
摘要:A palladium/graphitic carbon nitride(g-C3N4)-single walled carbon nanotubes(SWCNTs) composite sensor was constructed for the detection of estradiol(E2).Firstly,the g C3N4- SWCNTs were synthesized via solid grinding and followed by thermal polymerization with melamine(MAM) and single walled carbon nanotube(SWCNTs) as precursors,then Pd nanoparticles were loaded on the as prepared nanocomposite by self-assembly method.The morphology and composition of the Pd/g-C3N4-SWCNTs material were characterized by SEM,TEM,XRD and FTIR techniques,and its electrocatalytic performance toward estradiol(E2) was investigated by cyclic voltammetry.The Pd/g-C3N4-CNTs nanocomposite sensor was used for the detection of E2 in feedstuff sample.Under the optimum conditions,the DPV current response for E2 increased linearly in the concentration range of 5-150 μmol/L with a linear equation of Ipa(μA)=0.834 7+0.007 0CE2(r=0.990) and a detection limit(LOD,S/N=3) of 1.7 μmol/L.With good stability and selectivity,and no significant difference with the HPLC method,this method could meet the requirements for detection of E2 in feed samples.  
摘要:The Ti4+ immobilized silica nanocomposites(SiO2-Ti4+) were fabricated by synthesizing silica nanoparticles with tetraethoxysilane(TEOS) and γ-mercaptopropyl trimethoxysilane(γ-MPTS) as precursors,followed by “thiol-ene” click reaction and “one pot” process.The morphology and structure properties of the resultant SiO2-Ti4+ were characterized by transmission electronic microscopy(TEM),Fourier transform infrared spectroscopy(FT-IR) and X ray photoelectron spectroscopy(XPS).The adsorption behavior of the SiO2-Ti4+ towards phosphoproteins was investigated.Under the optimized conditions,the SiO2-Ti4+ showed a rather higher adsorption capacity towards phosphoproteins(α-casein,12.27 μmol/g) than non phosphoproteins(horseradishperoxidase,1.12 μmol/g).In addition,the practicality of the SiO2-Ti4+ was further demonstrated by their selective enrichment of phosphoproteins from milk samples.  
关键词:“thiol-ene” click reaction;“one pot” process;phosphoproteins;nano sized SiO2;separation and enrichment
摘要:In this paper,phosphorus doped carbon dots(P-CDs) were prepared by a self catalysis method with diphosphorus pentoxide and citric acid as raw materials.The P-CDs were characterized by transmission electron microscopy,Fourier transform infrared spectroscopy,X ray photoelectron spectroscopy,UV-visible absorption and fluorescence spectrometry.Results showed that the sizes of P-CDs mainly ranged from 5.0 nm to 10.2 nm,and on the surfaces of which existed hydroxyl,carboxyl and phosphorous groups.A novel method was developed for the sensitive and selective detection of hyperin(HP) based on the phenomenon that HP could quench the fluorescence of P-CDs.Under the optimum conditions,a good linear relationship was obtained between the fluorescence quenching efficiency(IF0/IF) and the concentration of HP in range of 0.22-55 μmol/L with a detection limit of 78 nmol/L.The method was successfully applied in the determination of HP in fufangmuji granules with recoveries of 93.3%-107% and relative standard deviation of 1.5%-1.7%.  
摘要:In this paper,two double quaternary ammonium salts(N1,N3-bis(2-hydroxyethyl)-N1,N1,N3,N3-tetramethylpropane-1,3-diaminiumbromide(QAS-1) and N1,N1,N3,N3-tetrahydroxyethyl-N1,N3-dimethyl-1,3-diaminium bromide(QAS-2) were prepared by grafting N,N dimethylethanolamine and N methyldiethanolamine onto both ends of 1,3-dibromopropane,respectively.They were characterized by FTIR,NMR and Elemental analysis,and their antibacterial properties against five species of bacteria and fungus were subsequently evaluated by inhibition zone method and tube double dilution method,which proved their good antibacterial effects.Especially,the antibacterial effect against fungus(Canidia Albicans) was more obvious,and the minimal inhibitory concentrations(MIC) for QAS-1 and QAS-2 were 100 mg·L-1 and 50 mg·L-1,respectively.SEM and TEM images showed that the antibacterial mechanism of QAS-1 toward S-aureus morphologies might be the antibacterial agents were adsorbed on the membrane surfaces to puncture the cell membranes,resulting in the release of bacterial cytoplasm.In addition,cytotoxicity results showed that IC50 values of QAS-1 on human normal heptical cell line(LO2) and human keratinocyte cell line(HaCat) were 110.34 mg·L-1 and 92.68 mg·L-1,respectively,which were significantly lower than that of the positive drug.The study suggests that this kinds of quaternary ammonium salts have potential application value in the field of antibacterial drugs.  
摘要:An ultra performance liquid chromatography-tandem mass spectrometric method with solid phase extraction was established for the simultaneous determination of 14 macrolide drugs in pork samples.Samples were extracted with 70%(volume fraction) acetonitrile,purified by solid phase extraction using a hydrophilic lipophilic balanced(HLB) polymer,and separated on a C18 column(100 mm×2.1 mm,1.7 μm) with acetonitrile and 01% formic acid-2 mmol/L ammonium acetate solution as mobile phases by gradient elution.The analytes were detected by mass spectrometry in positive ion mode under multiple reaction monitoring(MRM) scanning mode,and quantified by external standard method.Results showed that good linearities for 14 macrolide drugs were obtained in the corresponding mass concentration ranges with correlation coefficients(r2) larger than 0.995.The detection limits and quantitation limits of the method were in the ranges of 0.1-0.8 μg/kg and 0.5-3.0 μg/kg,respectively.Recoveries at low,medium and high spiked levels were in the range of 71.1%-102%,with relative standard deviations(RSD) less than 6.0%.This method could be applied in the analysis of macrolide drugs in pork samples with good accuracy and reliability.  
关键词:solid phase extraction;ultra performance liquid chromatography-tandem mass spectrometry;macrolide drugs;pork
摘要:Based on the conductivity of two dimensional transition metal carbide (MXene)-Ti3C2Tx and catalytic activity of Au@Pt nanoflowers,a Ti3C2Tx/Au@Pt nanoflowers enzyme free sensor was assembled for the ultrasensitive and rapid detection of H2O2 content.The prepared Ti3C2Tx was characterized by emission scanning electron microscopy and X-ray diffraction spectrometry.Results showed that the Ti3C2Tx material exhibited a unique accordion structure, while the Ti3C2Tx/Au@Pt are centered on Au particles and surrounded by Pt particles to form the surrouding dandelion structure.The cyclic voltammogram and time current curve of H2O2 on the Ti3C2Tx/Au@Pt modified electroded were studied.Results showed that the modified electrode based on Ti3C2Tx loaded Au@Pt nanoflowers presented good linear relationship for H2O2(0.03-1 100 μmol/L),high sensitivity(detection limit:0.02 μmol/L),good anti-interference and reproducibility.Compared with the traditional titration method,the new enzyme free sensor could be more rapidly and accurately used in the detection of H2O2 in a complex environment.  
关键词:two-dimensional transition metal carbide(MXene);Ti3C2Tx;Au@Pt nanoflowers;H2O2;enzyme free sensor
摘要:An analytical method was developed for the determination of ethoxyquin in apple,pear,grape and orange samples by high performance liquid chromatography combined with fluorescence detection.Samples were pretreated by mixing vitamin C,alkalescence adjustment,n hexane extraction and acetonitrile redissolution.Ethoxyquin residue in samples were detected by high performance liquid chromatography with fluorescence detector,and quantified by external standard method.There were good linear relationships for ethoxyquin in the concentration range of 2-100 μg/L,with their correlation coefficient(r) of 0.999 99.The limits of detection and quantitation were 0.01 mg/kg and 0.02 mg/kg,respectively.Average recoveries at four spiked levels of 0.02,0.04,0.2 and 1 mg/kg ranged from 80.4% to 108%,with relative standard deviations(RSD,n=6) of 1.4%-8.1%.With simplicity,rapidness,good repeatability and stability,this method is suitable for the determination of ethoxyquin in fruits.  
关键词:fruits;ethoxyquin;high performance liquid chromatography with fluorescence detection;quantitative determination
摘要:A novel molecular probe of N-(2-hydroxy-5-chlorophenyl) based rhodamine B hydrazide(HCPRH) was synthesized through a simple two-step reaction.Then its structure and fluorescence response were studied.Addition of Zn2+ into N,N-dimethylformamide(DMF) solution containing HCPRH resulted in increasement of fluorescence,while a fluorescent color change from colorless to yellow could be observed promptly with naked eyes under 365 nm ultraviolet lamp,indicating that the probe HCPRH could be used for rapid,sensitive and naked eye recognition of Zn2+.Moreover,the fluorescence emission of this probe toward Zn2+ was hardly affected by other metal ions.The binding constant between HCPRH and Zn2+ was calculated by Benesi-Hildebrand equation,and the 1∶1 binding mode was proposed based on the Job's method.In addition,according to the experimental results of fluorescence titration,the difference value of fluorescent intensity was proportional to Zn2+ concentration in the range of 10-250 μmol/L with a detection limit of 3.6 μmol/L.Results showed that HCPRH could be used in detection of trace amount of Zn2+.Subsequent experimental studies also showed that this molecular probe could be successfully applied in the continuous fluorescence response toward Zn2+ and S2-.  
摘要:A colorimetric method for the detection of traces of Cr(Ⅲ) was established by adsorbing methyl violet with N electron donor coordinating atoms on the surface of silver nanoparticles through bridging action and coordinate reaction,then the adding of Cr(Ⅲ) in the solution could lead to the precipitation phenomenon of silver nanoparticles sol,and followed by the solution color changing from bright yellow to grey red.Under the optimized conditions,the linear range for Cr(Ⅲ) was 2.0-10.0 μmol·L-1(r=0.997 6) and the detection limit for naked eye was 0.3 μmol·L-1.This method was applied in the determination of Cr(Ⅲ) in environmental samples,with recoveries of 93.2%-100% and relative standard deviations(RSD) less than 1.5%.It was rapid,sensitive and selective.  
摘要:A background removing algorithm based on wavelet transform was proposed in this paper as background leads to overestimate of peak intensity in various spectroscopy analysis,which needs to be removed before further data processing.The spectrum and its descendants were decomposed by wavelet transform iteratively until the estimated backgrounds converged.A criterion to determine the optimal iteration times was proposed by comparing errors of consecutive estimated backgrounds.By removing the converged estimated backgrounds,the spectrum was ready for peak intensities estimation.This method was evaluated with simulated and experimental Energy Dispersive X ray Fluorescence(EDXRF) spectra.The proposed method was compared with traditional wavelet transform and polynomial fitting method.The analyzed results showed that the proposed method could be used for the accurate elimination of spectral background,which was applicable for other kinds of spectral pre processing.  
摘要:Telomerase is a nuclear protein reverse transcriptase that adds the repeat sequence(TTAGGG)n to the end of chromosome with its own RNA template to stabilize the telomere length.Telomerase is activated in 85% to 90% of cancer cells,which has attracted a widespread concern and become an important breakthrough in tumor diagnosis and clinical treatment.Therefore,accurate and efficient determination of telomerase activity is of great significance.In recent years,many sensitive and accurate in vitro or in situ detection techniques have been developed for the detection of telomerase activity.In this paper,recent advances in the detection of telomerase activity have been reviewed,and the development trend for telomerase detection has been prospected.