最新刊期
卷 38 ， 期 8 ， 2019
- 摘要：In this paper,a quantitative detection system of cardiac biomarkers was proposed and demonstrated,which could be used in the detection of matrix metallopeptidase 9（MMP9),growth stimulation expressed gene 2（ST2) and pentraxin 3（PTX3).The reaction product of cardiac biomarkers was captured with smartphone camera.The photo was sent to the server side for analysis via the smartphone app.The detection results were displayed on the smartphone screen after the captured photo was analyzed by the server side.Results showed that the calibration curves for of three cardiac biomarkers based on the blue channel agreed well with the four parameters fitted model,and their correlation coefficients（r2 ) were 0999 7,0999 8 and 0999 8 respectively.41,43 and 40 serum samples were detected with MMP9,ST2 and PTX3,respectively.The comparisons between three detection results by the proposed method with those by commercial reader showed that the overall agreements reached up to 9512%,9767% and 9500%,respectively.The proposed method is suitable for the point of care detection and long term monitoring of cardiac biomarkers.关键词：cardiovascular disease;cardiac biomarker;quantitative analysis;smartphone;colorimetric algorithm
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发布时间： - 摘要：A split-type photoelectrochemical（PEC）method was developed for the detection of Escherichia coli O157∶H7（E.coli O157∶H7）with antibacterial peptide as a recognizer.Firstly,water soluble thioglycolic acid capped lead selenide quantum dots（PbSe QDs）were synthesized by a simple water bath method,then PbSe QDs were assembled on surface of indium tin oxide（ITO）electrode through electrostatic interaction,and the Pb2+ on surface of PbSe QDs could be exchanged with Zn2+ to form a ZnSe/PbSe/ZnSe quantum well（QW）,which could promote the electron-hole separation and improve the cathode photocurrent on the ITO/PbSe electrode.This method avoided the immobilized biomolecules on the electrodes to retard the PEC signal,and showed a highly efficient detection.The detection range of the method for E.coli O157∶H7 ranged from 10.0 CFU/mL to 5.0×106 CFU/mL with a detection limit of 4.0 CFU/mL.The recoveries varied from 94.7% to 104% with relative standard deviations of 1.9%-2.8%.关键词：photoelectrochemical sensor;ZnSe/PbSe/ZnSe quantum well;Escherichia coli O157∶H7
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发布时间： - 摘要：An ultra performance liquid chromatography-quadrupole-exactive orbitrap mass spectrometry(UPLC-Q-Exactive Orbitrap) was developed for the rapid screening and confirmation of 74 antibiotics and other compounds in swine urine.The samples were high speedily centrifuged,then diluted with solvent,and finally separated on an Agilent SB C18 (3.0 mm×100 mm，1.8 μm) column using a binary solvent system composed of 0.1% formic acid aqueous solution and 0.1%formic acid acetonitrile solution by gradient elution.Under the optimal conditions,the analytes were precisely screened and confirmed with the precision mass,retention time and two stage ion mass spectra．There were good linear relationships for 74 analytes in their respective concentration ranges with correlation coefficients(r2) larger than 0.99 and limits of detection(LOD) of 10 ng/mL.The recoveries for 74 compounds in swine urine at LOD spiked level mainly ranged from 55.8%to 120%,with relative standard deviations(RSD) of 1.3%-21%.The method was convenient，rapid，sensitive and accurate,and was quite effective for the screening and confirmation of 74 antibiotics and other compounds in swine urine,which was beneficial to the investigation on drugs situation in husbandry.关键词：ultra performance liquid chromatography-quadrupole-exactive orbitrap mass spectrometry(UPLC-Q-Exactive Orbitrap);swine urine;antibiotics and other compounds;rapid screening
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发布时间： - 摘要：A microarray protein chip method was established for the simultaneous detection of clenbuterol and ractopamine residues in food.Results showed that the linear ranges for clenbuterol and ractopamine were 0.07-1.2 ng/g and 0.05-0.8 ng/g,respectively.The recoveries for the two substances in pork and pig liver were in the range of 74%-132%,with relative standard deviations all less than 10%.The established method was compared with HPLC-MS,and the results obtained were identical.This method was simple,rapid and high throughput,and could be used in the detection of clenbuterol and ractopamine residues in actual samples.关键词：protein chip;clenbuterol;ractopamine;artificial antigen
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发布时间： - 摘要：A high sensitivity and throughput method was developed for the simultaneous determination of 152 pesticide residues in vegetables and fruits by gas chromatography tandem mass spectrometry(GC-MS/MS) with QuEChERS-dispersed liquid-liquid microextraction(DLLME).Pesticide residues in vegetables and fruits samples were extracted by QuEChERS method with acetonitrile.Then after centrifugation,the acetonitrile supernatant was added with trace chloroform(CHCl3) for DLLME.The extract was analyzed by(GC-MS/MS) with electron impact ion source(EI) in selective reaction monitoring mode(SRM).Results showed that there were good linear relationships for 152 pesticides including isomers in the range of 5.0-200 μg/L with correlation coefficients above 0.995.The recoveries for the analytes at low,medium and high levels were in the range of 60.6%-119%,with relative standard deviations(RSD,n=6) of 1.5%-20%.The limits of detection and the limits of quantitation were in the ranges of 0.14-2.3 μg/kg and 0.45-7.7 μg/kg,respectively.The method is simple,accurate and sensitive.It is suitable for the high throughput and rapid detection of multi residues in fresh agricultural products such as vegetables and fruits.关键词：QuEChERS;dispersive liquid-liquid micro extraction(DLLME);gas chromatography tandem mass spectrometry(GC-MS/MS);multi pesticide residues;vegetables and fruits
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发布时间： - 摘要：A method was developed for the rapid screening and analysis of 32 banned and restricted components in hair dyes by ultra performance liquid chromatography-quadrupole/electrostatic field obitrap high resolution mass spectrometry.The samples were extracted using a mixed solution of methanol and 2 g/L aqueous ascorbic acid,and purified with n hexane.The separation was carried out on an ZORBAX Eclipse Plus C18 column（3.0 mm×100 mm，1.8 μm）by gradient elution with methanol and 5 mmol/L ammonium acetate as mobile phases.The 32 components were simultaneously analyzed in switching positive and negative modes.The retention time,accurate mass of parent ion and relative isotope abundance in full scan mode were used for fast screening of multi components in hair dyes,while accurate mass of fragment ions in two stage threshold triggered full mass scan mode were used for confirmation.Under the optimal conditions,good linearities（r2>0.99）were obtained in their respective concentration ranges.The limits of quantitation（LOQ）for 32 compounds were in the range of 0.2-40 μg/g.The recoveries ranged from 81.0% to 110% with relative standard deviations（RSDs）of 3.3%-9.9%.The method was simple,sensitive and accurate,and was suitable for the rapid screening and confirmation of 32 kinds of banned and restricted component in hair dyes.关键词：ultra-performance liquid chromatography;obitrap high resolution mass spectrometry;hair dyes;dye;rapid screening
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发布时间： - 摘要：A comprehensive structural analysis on reference monoclonal antibody(IgG1) was conducted,which provides a reference for further in depth research of quality and future quality controling.Exactive plus EMR mass spectrometry was used to detect the precise molecular weight(MW) before and after PNGaseF digestion,then calculating the N glycan content.The MW of the reference antibody ranged from 148 285.0 to 149 020.8,which was 145 810.4 after PNGaseF digestion,and the N glycan content ranged from 1.67% to 2.15%.The WCID-cIEF results showed that the isoelectric point(pI) of the antibody ranged from 8.21 to 8.74,in which the pI of the main component was 8.61 and the relative content was 6143%.Then,the charge heterogeneity was detected by ion exchange chromatography.The contents for basic peak,acid peak and main peak were 4.1%,23.9% and 72.0%,respectively,which were consistent with the pI distribution by WCID-cIEF analysis.Furthermore,the glycopeptide distribution and the glycosylated sites were analyzed by peptide mapping before and after PNGaseF digestion,as well as the complementary determinant region(CDR) of the heavy and light chains,and the oxidation sites and oxidation ratio of methionine.The disulfide bonds were also analyzed by peptide mapping before and after antibody reduction.Finally,the glycation of the C-terminal of the antibody was detected.Results showed that there was no glycation occured in the C-terminal of the reference antibody.关键词：reference antibody;molecular weight;isoelectric point(pI);charge heterogeneity;peptide mapping
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发布时间： - 摘要：A two dimensional correlation spectroscopy(2DCOS) was presented to optimize the characteristic variables for pesticide residues in rice,in order to improve the accuracy for the rapid detection of pesticide residues in rice based on surface enhanced Raman spectroscopy(SERS).Firstly,the original spectra were pretreated using standard normal variable transformation(SNV),then the two dimensional correlation spectrum and diagnosis spectrum were analyzed with chlorpyrifos methyl concentration as the disturbance.The characteristic peaks of chlorpyrifos methyl were optimized based on the two dimensional correlation spectroscopy and diagnosis spectroscopy.A support vector machine(SVM) model for analyzing chlorpyrifos methyl residues in rice was developed,and was compared with the PLS model.Results showed that 2DCOS was a wonderful way for screening out the characteristic peaks related to the chlorpyrifos methyl.The performance of SVM model based on 4 chlorpyrifos methyl characteristic peaks selected by 2DCOS was better than that of the PLS model.The correlation coefficient(Rp) in the prediction set was 0.96,the root mean square error of prediction(RMSEP) was 521,and the relative prediction deviation(RPD) was 3.66,which indicated that the developed model could be used for the actual estimation of chlorpyrifos methyl pesticide residues in rice.Results showed that 2DCOS is feasible for screening characteristic peaks related to chlorpyrifos methyl in rice by simplifying the model and improve the prediction accuracy.It provides a new idea for the rapid detection of food and agricultural products by Raman spectroscopy for quality and safety.关键词：surface enhanced Raman spectroscopy(SERS);two dimensional correlation spectroscopy(2DCOS);characteristic variable optimization;rapid detection;rice;chlorpyrifos methyl
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发布时间： - 摘要：A kind of nitrogen doped carbon quantum dots(N-CDs) with high stability,good water solubility were prepared by one-step microwave method with citric acid as carbon source and urea as nitrogen source.The prepared N-CDs were characterized by transmission electron microscopy(TEM),atomic force microscopy(AFM),X-ray photoelectron spectroscopy(XPS) and infrared spectroscopy(IR).Results showed that the N-CDs contained a particle size ranging from 0.5 nm to 5 nm with an average particle size of 2.6 nm,which were rich in hydroxyl,carboxyl and amino groups and other functional groups.The N-CDs were used in the detection of dopamine.Under the selected experimental conditions,there was a good linear relationship for the fluorescence quenching efficiency(IF/IF0) of N-CDs with dopamine within the concentration range of 25-375 μmol/L,and the method detection limit was 0.08 μmol/L.This method was applied in the detection of dopamine in urine of normal people with high accuracy and satisfactory results.The average recoveries ranged from 995% to 106% with relative standard deviations(RSDs) of 1.8%-2.3%.关键词：microwave one step method;nitrogen doped carbon quantum dots;dopamine;detection
- 713
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发布时间： - 摘要：A novel IL@PPPy-TiO2/NiOCNSs solid phase microextraction fiber was successfully fabricated by using 1-butyl-3-methylimidazolium hexafluorophosphate ionic liquid(IL) doped with polyphenylpyrrole(PPPy) onto the hydrothermally treated NiTi substrate with electrochemical deposition.The uniform and porous nanoparticles were coated on the surface of NiTi alloy.The extraction performance of the fiber was estimated by the combination of high performance liquid chromatography(HPLC)and itself using polychlorinated biphenyls(PCBs),phthalic acid ester(PAEs),polycyclic aromatic hydrocarbon(PAHs) and ultraviolet(UV) absorbent as model analytes.The novel IL@PPPy-TiO2/NiOCNSs fiber showed good extraction selectivity and high extraction capability toward PCBs in water samples.The effect factors including extraction temperature,stirring rate,extraction time and ionic strength on the extraction efficiency of PCBs were optimized.Under the optimized condition,there were linear relationships for the analytes in certain mass concentration range with correlation coefficients(r) not less than 0.998 6.The limits of detection(LOD) were in the range of 0.015-0.11 μg/L.The intra-day and inter-day relative standard deviations(RSD) for a single fiber were in the ranges of 4.7%-6.1% and 5.4%-7.0%,respectively.The fiber-to-fiber reproducibility(n=5) varied from 6.5% to 7.7%.Recoveries for 5 PCBs in real water samples ranged from 83.0% to 104% with RSD not more than 86%.The proposed SPME/HPLC method was successfully applied in the extraction and detection of trace PCBs in different water samples.关键词：ionic liquid;solid phase microextraction(SPME);high performance liquid chromatography(HPLC);polychlorinated biphenyls(PCBs)
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发布时间： - 摘要：An ultra performance liquid chromatography-tandem mass spectrometric（UPLC-MS/MS) method was developed for the determination of carbofuran and aldicarb,as well as their metabolites carbofuran 3-hydroxy,aldicarb sulfone and aldicarb sulfoxide in cucumber,tomato and cowpea.The samples were extracted with acetonitrile and QuEChERS salt packets containing 0.5 g sodium sesquihydrate,1 g sodium citrate,1 g NaCl and 4 g MgSO4,and purified by pass through solid phase extraction using an Oasis PRiME HLB column,then analyzed by UPLC-MS/MS.The matrix effects were observed in the analysis of the analytes in sample.The quantitations were performed by the external standard method with matrix matched calibration standards.There were linear relationships for carbofuran,carbofuran 3 hydroxy,aldicarb,aldicarb sulfone and aldicarb sulfoxide in the range of 0.001-0.5 mg/L with their correlation coefficients（r) larger than 0.996 0.Recoveries for cucumber,tomato and cowpea at spiked levels of 0.02-0.2 mg/kg ranged from 80.4% to 110%,with relative standard deviations（RSDs) of 1.1%-4.8%.The limits of detection（LOD,S/N=3) for carbofuran,carbofuran 3-hydroxy,aldicarb,aldicarb sulfone and aldicarb sulfoxide were 0.07,0.3,1.0,4.0 and 13 μg/kg,respectively,and the limits of quantitation（LOQ,S/N=10) were 0.2,1.0,2.0,13 and 42 μg/kg,respectively关键词：pass through solid phase extraction;ultra performance liquid chromatography-tandem mass spectrometry;cucumber;tomato;cowpea;carbofuran;aldicarb;metabolites
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发布时间： - 摘要：An ultra high performance liquid chromatographic(UPLC) method was established for the rapid determination of sulfamethoxazole(SMZ),N acetyl sulfamethoxazole(N-ac-SMZ) and trimethoprim(TMP) in fish tissues,including muscle and skin in natural proportions,liver,kidney,gill and plasma.Samples of muscle and skin in natural proportions,liver,kidney and gill tissues of fish were prepared using the modified QuEChERS,and plasma sample was prepared by a liquid-liquid extraction procedure.The analytes were separated on an Acquity UPLC-BEH C18 column(2.1 mm×100 mm，1.7 μm) with methanol and water containing 0.1%acetic acid as mobile phases,at a detection wavelength of 270 nm,using an absorbent minus median baseline filter(MBF) in data acquisition mode.The external standard method was used for quantitation.Results showed that there were good linear relationships for SMZ,N ac-SMZ and TMP in the range of 0.05-10 mg/L with correlation coefficients(r2) not less than 0.998 9.The detection limits and quantitation limits for the analytes in fish tissues were 25 μg/kg and 50 μg/kg,respectively.Recoveries for the target compounds at spiked levels of 0.05-2.00 mg/kg were between 68.2%and 97.3%with relative standard deviations of 1.7%-13%.The method is simple,accurate and highly sensitive,and is suitable for the residue determination,pharmacokinetic and tissue distribution study of SMZ,N-ac-SMZ and TMP in fish.关键词：modified QuEChERS;sulfamethoxazole;metabolite;trimethoprim;fish tissue;ultra high performance liquid chromatography(UPLC)
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发布时间： - 摘要：A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) with supercritical fluid carbon dioxide extraction(SFE) was established for the determination of 11 common psychotropic drugs in human hair.The sheared hair samples were extracted by SFE under optimized conditions.The concentrated extract was reconstituted to 100 μL with methanol,then analyzed by HPLC-MS/MS.Results showed that there existed good linear relationships for 11 common psychotropic drugs in the range of 2-200 ng/mL,with correlation coefficients(r2) greater than 0.999.The detection limits and the quantitation limits were in the ranges of 0.01-0.05 ng/mg and 0.03-0.10 ng/mg,respectively.Recoveries at the spiked levels of 0.05,0.20 and 0.40 ng/mg ranged from 816% to 94.8% with relative standard deviations(RSD) of 0.50%-3.4%.The method is rapid,sensitive and accurate,and could be used in simultaneous detection of 11 common psychotropic drugs in human hair.关键词：supercritical fluid carbon dioxide extraction(SFE);human hair;psychotropic drugs;high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)
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发布时间： - 摘要：A high performance liquid chromatographic（HPLC）method was developed for the determination of 4 banned phenols,i.e.phloroglucinol,4-nitroguaiacol,phenolphthalein and dinoseb in water-based,emulsions,creams,powder and waxy based cosmetics.After a clean up process of vortex extraction and nitrogen blowing concentration,the analytes were redissolved with optimized solvent.The qualitative analysis was based on retention time and ultraviolet absorbance,while quantitative analysis was performed by the external standard method.There existed good linear relationships for four analytes in the certain concentration range，with correlation coefficients（r2） more than 0.99.The limits of detection（LOD）and limits of quantitation（LOQ）for 4 banned phenols were in the ranges of 1.5-6.0 mg/kg and 5.0-20.0 mg/kg,respectively.The spiked recoveries for four analytes were in the range of 81.3%-100% with relative standard deviations（RSD）of 1.0%-8.2%.The developed method was applicable for the determination of 4 banned phenols in cosmetic with simple pretreatment and easy operation.关键词：high performance liquid chromatography（HPLC）;cosmetic;banned phenols
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发布时间： - 摘要：A high performance liquid chromatographic method was developed for the simultaneous determination of 11 benzimidazoles metabolites residues in fat.Samples were firstly dissolved with n hexane,then extracted with antioxidant and 0.1 mol/L hydrochloric acid-acetonitrile(1∶1,by volume),followed by treatments with n hexane for defatting,antioxidant again and further clean-up on a MCX solid phase extraction(SPE) column.After concentration,the chromatographic separation was performed on an Atlantis T3 column by gradient elution with a mixed solution of methanol and 1%acetic acid at a flow rate of 1.0 mL/min.The detection wavelength was set at 292 nm,and the external standard method was used for quantitation.The calibration curves for 11 analytes were linear in the range of 25.0-1 000 μg/L with quantitation limits of 50 μg/kg.The recoveries at three spiked levels ranged from 82.0%to 109%with relative standard deviations(RSD) of 0.71%-9.9%.The developed method could meet the requirements for determination of 11 benzimidazoles metabolites residues in fat.关键词：benzimidazoles metabolites residues;fat;solid phase extraction;high performance liquid chromatography
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发布时间： - 摘要：A surface enhanced Raman spectroscopy（SERS）with in situ synthesized silver colloid substrate was developed for the rapid detection of amiloride hydrochloride in tablets.The silver colloid substrate for surface enhanced Raman scattering was prepared using heating paster（warm baby）as heating source,and the SERS performance was evaluated with rhodamine 6G（R6G）as a SERS probe.Results indicated that the synthesis method for silver colloid was simple and rapid,and the substrate could be fabricated within 15 min and keep for 4 h with satisfactory stability and good SERS enhancement effect.It was applied in the SERS detection of amiloride hydrochloride in tablets.There was a linear relationship between SERS intensity and amiloride hydrochloride in the concentration range of 0.8-8 mg/L,with a curve equation of y=1 395ρ-76.40（r2 =0.999 2）.The limit of detection was 0.2 mg/L,and the spiked recoveries from tablet samples were in the range of 104%-106% with relative standard deviations of 0.35%-3.5%.With the advantages of simpleness,rapidness and good stability,the developed method provides a new appraoch for the identification and rapid detection of amiloride hydrochloride in tablets.关键词：surface enhanced Raman spectroscopy（SERS）;amiloride hydrochloride;tablets;silver colloid
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发布时间： - 摘要：A novel electrochemical luminescence method was established for the detection of ribavirin based on a TiO2-CdTe glassy carbon electrode(GCE).The TiO2-CdTe/GCE electrochemical luminescence(ECL) sensor platform was constructed by immobilizing a CdTe-TiO2 complex onto the surface of glassy carbon electrode,which ECL properties were studied.The TiO2-CdTe/GCE exhibited an efficient and stable ECL signal in alkaline buffer solution containing Ru(bpy)2+3 and trinpropylamine(TprA).The ECL signal was obviously quenched when a certain amount of ribavirin was added.Thus,a new detection method for ribavirin was established.Under the optimized conditions,the ECL signal intensity depends linearly on the logarithm of ribavirin concentration in the range of 3.9×10-4-3.9 μmol·L-1,and the detection limit(S/N=3) was 1.3×10-10 mol·L-1.The method was successfully applied in the detection of ribavirin in injection with recoveries of 96.6%-101%.关键词：TiO2-CdTe complex;Ru(bpy)2+3;electrochemical luminescence;ribavirin
- 666
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发布时间： - 摘要：An ion chromatographic method was established for the determination of sodium gluconate in soap noodle.Sample was separated on a METROSEP CARB 1 column by isocratic elution using 150 mmol·L-1 NaOH+20 mmol·L-1 NaAc water solution as mobile phase at a flow rate of 1.0 mL/min,and detected by Metrohm 850 ion chromatography with pulsed amperometric detector,finally quantified by external standard method.A good linear relationship was obtained for sodium gluconate in the range of 0.5-200 mg/L with a correlation coefficient（r2）of 0.999 6.The detection limit and the quantitation limit were 0.25 mg·L-1 and 0.63 mg·L-1,respectively.The recoveries at spiked levels of 1-20 mg/g ranged from 80.7% to 104%.This method was suitable for the determination of sodium gluconate in soap noodle for its derivization free procedure,simplicity and sensitivity.关键词：sodium gluconate;soap noodle;ion chromatography method
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发布时间： - 摘要：Microplastics refer to those plastic fibers,fragments or particles less than 5 mm in diameter,which have a wide range of sources and stable properties in the environment.They are ideal carriers for hydrophobic organic pollutants and heavy metals.Microplastics are easily ingested by plankton,fish and lower organisms,and transferred and enriched between trophic levels in the food web.As a new type of environmental pollutants,microplastics have posed a serious threat to the ecological environment,resulting in potential risks to food safety.Microplastics analysis techniques are the basis for research of microplastics distribution,migration,transformation,fate and ecological toxicological effects in the environment.The research progress of microplastics collection,separation,extraction and qualitative identification in environmental samples at home and abroad is reviewed in this paper,and the advantages and disadvantages of each method are discussed.Finally,aiming at the problems and shortcomings of microplastics analysis methods at present,the future development trend of analysis techniques for environmental microplastics is forecasted.关键词：microplastics;emerging environmental pollutants;separation and extraction;spectral analysis;thermal analysis
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发布时间： - 摘要：Capillary electrophoresis(CE),a highly mature and versatile technique,has been continually evolving in the last three decades.Capillary electrophoresis has important applications in the field of biological analysis such as protein separation due to its advantages of short separation time,high separation efficiency and low sample consumption,etc.However,many drawbacks have been caused by dissociation of silicon hydroxyl on inner wall of capillary in CE separation process.To overcome these drawbacks associated with CE,modification of capillary inner surfaces by antifouling polymer coatings are chosen.The antifouling polymer modified capillary method could not only regulate the electroosmotic flow,but also benefit the proteins separation.This method could also effectively improve the separation efficiency and separation stability for proteins in CE process.The paper presents a review on the latest research progress of capillary coatings,like dynamic and static polymer coating for protein separation.It also summarizes the research progress of polymer coating capillary based on dopamine/polydopamine anchored.And finally,the prospects of the future development trend of polymer coatings of capillary are discussed.关键词：capillary electrophoresis;polymer coatings;protein separation;electroosmotic flow
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