最新刊期
卷 39 ， 期 5 ， 2020
- 摘要：Digital PCR is a newly developed absolute quantitative analysis technique after real-time quantitative PCR,which is widely used in early detection and diagnosis of diseases and microbial detection.However,in the detection of digital PCR microreactors,conventional optical detection methods require complex optical equipments while the application environment is restricted and the cost is high.Therefore,a kind of PCR droplet detection chip based on contactless conductivity detection was developed by replacing the traditional optical detection with conductivity detection,which could effectively reduce the cost of the digital PCR result readout system.By optimizing the electrode structure and arrangement,a 3D electrode structure composed of three parallel electrodes is adopted to reduce the relative error and improve the sensitivity,and the detection on ratio of negative to positive PCR reaction droplets is achieved.The detecting throughput of the chip reaches up to 100 pcs per second,with a good relativity(r2=0.998) in the DNA template concentration range of 0.5×104-3×104 copies/μL.关键词：digital PCR;droplets;label-free;contactless conductivity detection
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发布时间：2023-04-18 - 摘要：An online liquid chromatography-gas chromatography-mass spectrometric(LC-GC-MS) method was developed for the detection of mineral oil components in recycled and virgin papers.Meanwhile,combined with multivariate statistical analysis,the differences between recycled and virgin papers were analyzed and identified.The mineral oil components in paper samples were extracted with n-hexane-ethanol(1∶1) solution,then analyzed by LC-GC-MS.The chromatograms were subjected to convolution and retention time alignment processing.Principal component analysis(PCA) and orthogonal partial least squares discriminant analysis(OPLS-DA) were used to discriminate the recycled and virgin papers,and screen the differential components.Results showed that recycled and virgin papers could be clearly distinguished by multivariate statistical analysis.Compounds including diisopropyl naphthalene isomers,tetramethyl biphenyl isomers,dimethyl biphenyl isomers,isopropylbiphenyl isomers in mineral oil aromatic hydrocarbons(MOAH) fraction,and the compounds containing n-alkanes with carbon atom numbers from 25 to 33 in mineral oil saturated hydrocarbons(MOSH) fraction,were responsible for the chemical difference between recycled and virgin papers.关键词：recycled paper;virgin paper;online liquid chromatography-gas chromatography-mass spectrometry;principal component analysis;mineral oil
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发布时间：2023-04-18 - 摘要：Benzopyrene(BaP) is a common polycyclic aromatic hydrocarbon compound,which has attracted wide attention due to its strong carcinogenicity to the human body.In this paper,an electrochemical luminescence sensor for the detection of BaP was constructed based on a covalent organic framework modified electrode.Firstly,the covalent organic framework material,CTpPa-2 formed by the condensation reaction of 1,3,5-triformylphloroglucinol(CTp) and 2,5-dimethyl-p-phenylenediamine (Pa-2),was modified on the electrode surface by drop coating method,then a simple and rapid BaP electrochemical luminescence sensor with good stability was constructed by combining the modified electrode with a luminol-hydrogen peroxide system.The morphology and electrochemical properties of CTpPa-2 modified carbon electrode were characterized by scanning electron microscopy,differential pulse voltammetry,cyclic voltammetry,galvanostatic charge/discharge and electrochemical luminescence.The feasibility for the determination of BaP was also investigated.Under the optimized experimental conditions,there was a good linear relationship between luminescent intensity and BaP concentration in the range of 50-600 nmol/L with a correlation coefficient(r2) of 0.995 1,and the limit of detection(S/N=3) was 5.60 nmol/L.The proposed sensor was applied in the detection of BaP in roasted meat sample,and the results obtained were similar to those of HPLC method,indicating that this method has a good application prospect.关键词：covalent organic framework;benzopyrene(BaP);luminol;electrochemical luminescence;sensor
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发布时间：2023-04-18 - 摘要：A high performance liquid chromatography with magnetic zeolitic imidazolate framework (ZIF-8@Fe3O4) solid phase extraction was developed for the determination of three benzoylurea insecticides)(BUs),ie.penfluron,clofentezine and chlorfluazuron in fruit juice samples.The prepared ZIF-8@Fe3O4 sorbent was characterized by X-ray diffraction,Fourier transform infrared spectrometry,scanning electron microscopy and vibrating sample magnetometry.The extraction parameters were optimized,including pH value of solution,amount of sorbent,extraction time,eluting solvent type and volume(single elution volume×elution times).Under the optimized conditions,there were good linear relationships in the range of 2.0-200 ng/mL for penfluron and clofentezine and 3.5-350 ng/mL for chlorfluazuron,with correlation coefficients(r) of 0.999.The limits of detection(S/N=3) for three analytes were in the range of 0.6-1.0 ng/mL,and the limits of quantitation(S/N=10) were 2.0-35 ng/mL.The recoveries for all targets at three spiked levels in fruit juice samples ranged from 82.7% to 98.6%,with intra-day and inter-day relative standard deviations(RSD) of 1.2%-6.1% and 1.3%-9.0%,respectively.The enhancement factors ranged from 43.4 to 48.1 for all the analytes when 10 mL juice sample was used as loading solution.The reusability of the fabricated ZIF-8@Fe3O4 adsorbent was investigated,and the RSD for recoveries of benzoylurea insecticides for 10 consecutive adsorption-desorption cycles in sample solutions were not more than 8.8%.The proposed method is sensitive and effective,and could be applied in the determination of benzoylurea insecticides in fruit juice samples.关键词：ZIF-8@Fe3O4;magnetic solid phase extraction;benzoylurea insecticides;fruit juice;high performance liquid chromatography
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发布时间：2023-04-18 - 摘要：To develop a rapid and highly selective method for detection of citric acid is a must as citric acid is an important marker for a variety of diseases.A water soluble hydroxypyridine functionalized spiropyran probe was designed and synthesized by introducing hydroxypyridine group into spiropyran skeleton,as to improve its binding ability to citric acid through the synergy effect between spiropyran carbon and hydroxyl group.Results showed that the probe responded to citric acid with high selectivity,accompanying with significant color change and fluorescence quenching.Based on this,a rapid and sensitive fluorescence method for detection of citric acid was established.The probe was applied in the detection of citric acid in urine sample,with a linear range of 20-120 μmol/L and a detection limit of 1.0 μmol/L.Moreover,the probe was used for the detection of citric acid in 2.5% artificial urine.The recoveries ranged from 85.7% to 92.2%,with relation standard deviations of 3.0%-9.2%.The method is facile,accurate and selective,and is potential in the determination of citric acid in urine.关键词：water-soluble spiropyran;hydroxypyridine functionalized;citric acid;urine;fluorescence spectra
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发布时间：2023-04-18 - 摘要：In this paper,two new quinoline derivatives were synthesized by combining 2-methyl-8-hydroxyquinoline with tetrastyrene or tristyrene moieties,and their photophysical properties were studied.It was found that the quinoline derivatives with tetrastyrene attached exhibited a characteristics of aggregation induced emission(AIE),while the quinoline derivatives with tristyrene attached showed a mild aggregation induced quenching(ACQ) effect.Therefore,the aggregation induced effect of the target molecules could be adjusted through the regulation of functional groups.The overall planarities of the molecules in different systems were different,the fluorescence lifetime of tristyrene-modified derivatives in solution is 0.55 ns higher than the solid fluorescence lifetime of 0.43 ns.Cyclic voltammetry(CV) proves that the compounds have excellent electrochemical stability, and the LUMO energy levels of 4-Br-TPE-8HQ and TriPE-8HQ were calculated to be -2.40 eV and -2.43 eV, respectively, indicating that the two compounds can be injected with electrons.关键词：2-methyl-8-hydroxyquinoline;tetrastyrene;tristyrene;aggregation induced emission;crystal structure
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发布时间：2023-04-18 - 摘要：In order to investigate the variation of aroma components in cut tobacco in the heating and humidifying process(SIROX process) and drying process on primary processing line,samples were collected on the primary processing line at three time points:before SIROX,after SIROX(before drying) and after drying.Samples were ultrasonically extracted with solvent,then analyzed by GC-MS and quantified with C17 as internal standard.Results showed that:Firstly,the contents of 18 aroma components such as acetic acid and benzyl alcohol,etc.decreased during SIROX process,while those of 6 aroma components increased,including 2-furanmethanol,2,4-dihydroxy-2,5-dimethyl-3(2H)-furan-3-one,etc.Secondly,the contents of 14 aroma components such as acetic acid and maltol,etc.decreased during drying process,while those of 6 aroma components increased,including 2-furanmethanol and 2-furancarboxaldehyde,etc.Thirdly,the contents of 23 aroma components such as acetic acid and 2,3-butanediol,etc.decreased during SIROX and drying process,while those of 4 aroma components increased，including 2-furanmethanol and 2,4-dihydroxy-2,5-dimethyl-3(2H)-furan-3-one,etc.Fourthly,the variations of temperature and humility in SIROX and drying process on primary processing line may result in Maillard reaction,degradation and volatilization inside the cut tobacco,leading to the changes of the aroma components.This investigation provides a scientific basis for the development of cigarette products with high quality.关键词：cut tobacco;heating and humidifying process;drying process;aroma components
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发布时间：2023-04-18 - 摘要：An electrochemical method was developed for the detection of hesperetin(HSP) using a three dimensional potassium sorbate derived interconnected porous carbon(PSIPC) modified electrode.The PSIPC material was synthesized by pyrolyzing method,using organic salt potassium sorbate(PS) as template via heating treatment in nitrogen atmosphere,and was characterized by scanning electron microscopy(SEM),transmission electron microscopy(TEM),X ray powder diffraction(XRD),X photoelectron spectroscopy(XPS),thermogravimetric analysis(TGA) and N2 adsorption and desorption tests.PSIPC-700,PSIPC-800 and PSIPC-900 obtained in different temperatures were directly dropped onto the surface of a glassy carbon electrode to obtain PSIPC modified electrodes(PSIPC-700/GCE,PSIPC-800/GCE and PSIPC-900/GCE).The electrochemical behaviors of HSP on PSIPC-900/GCE were investigated by cyclic voltammetry(CV) and differential pulse voltammetry(DPV).Under the optimized conditions,the linear range for HSP was in the range of 0.05-15.0 μmol/L.The limit of detection was as low as 0.021 μmol/L.With high sensitivity and wide detection range,this method could be applied in the detection of HSP in real samples.关键词：potassium sorbate(PS);porous carbon;hesperetin(HSP);electrochemical detection
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发布时间：2023-04-18 - 摘要：An electrochemiluminescence(ECL) biosensor based on carboxyl functionalized poly［(9,9-dioctylfluorene-2,7-diyl)-co-(1,4-benzo-｛2,1′-3｝-thiadiazole)］polymer dots(PFBT-COOH) was constructed for the detection of glucose.The PFBT-COOH emitted a strong ECL signal without any exogenous coreactants,which could be effectively quenched by H2O2.In this work,PFBT-COOH was modified onto surface of glassy carbon electrode(GCE),and further cross linked with glucose oxidase(GOD) to obtain the biosensor,GOD/PFBT-COOH/GCE.With increase of glucose concentration in detection solution,amount of H2O2 generated by glucose in situ under the catalysis of GOD would increase,leading to a gradual weakening of ECL signal at the biosensor,thus achieving an accurate,quick and sensitive detection of glucose.The linear range of glucose was in the range of 1.0×10-7-3.0×10-3 mol/L,and the detection limit was 3.0×10-8 mol/L.The method was applid in the detection of glucose in serum samples with spiked recoveries of 985%-106%.Such a strategy provides a new idea for construction of enzyme sensor and a new method for glucose detection.关键词：glucose;biosensor;electrochemiluminescence(ECL);PFBT-COOH
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发布时间：2023-04-18 - 摘要：A single particle inductively coupled plasma mass spectrometric(SP-ICP-MS) method was developed for simultaneous determination of the particle concentration,mass concentration and particle size distribution of nano silver particles(AgNPs) in environmental water samples.Effects of pH,dissolved organic matter(DOM) concentration and ionic strength of the solution on AgNPs were also investigated.A 60 nm AgNPs standard solution was determined by SP-ICP-MS with good accuracy,which results were consistent with the certified values.Impacts on the determine results were low in the conditions of pH value within 5 to 7,ionic strength not more than mmol/L and DOM concentration not larger than 30 mg/L.When pH value of the solution was not more than 5 or the ionic strength was larger than 1,the particle concentration and the particle size decreased with decreasing pH or increasing ionic strength.The method was applied to the detection of AgNPs in three actual water samples of river water,dye wastewater,and aquaculture wastewater,with the spiked recoveries for AgNPs of 98.1%,83.3% and 93.3%,respectively.Results indicated that the SP-ICP-MS method could be used for quick and accurate determination of the particle concentration,mass concentration,and particle size distribution of AgNPs in environmental water samples under appropriate matrix conditions.关键词：silver nanoparticle;inductively coupled plasma mass spectrometry;environmental water sample;matrix effect
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发布时间：2023-04-18 - 摘要：An analytical method was established for the determination of 88 pesticide residues in Pericarpium citri reticulatae by improved QuEChERS pretreatment combined with gas chromatography tandem mass spectrometry(GC-MS/MS) in dynamic multi reaction monitoring mode.Screening and optimizing of sample extraction methods,acetonitrile as extraction solvent,then added with 40 g anhydrous magnesium sulfate and 1.0 g anhydrous sodium acetate,followed by ceramic proton extraction,200 mg PSA,100 mg C18 and 30 mg GCB purification,and finally corrected by matrix matching external standard method.Influences of matrix effect on the quantification accuracy for target compounds in Pericarpium citri reticulatae were significantly weakened.The calibration curves for 88 pesticides exhibited good linearity in a certain concentration range,with their correlation coefficients(r2) not less than 0.996 3.The limits of detection(S/N=3) and the limits of quantification(S/N=10) were 0.001 0-0.050 0 mg/kg and 0.002-0.100 0 mg/kg,respectively.Moreover,the average recoveries at low,medium and high spiked levels ranged from 60.1% to 118% with the relative standard deviations(RSDs,n=6) ranged from 0.30% to 13%.The method was fast,efficient,sensitive and reliable,and was suitable for the rapid screening and routine detection of pesticide residues in Pericarpium citri reticulatae.关键词：Pericarpium citri reticulatae;QuEChERS;rapid screening;ceramic homoproton
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发布时间：2023-04-18 - 摘要：An ultra high performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was established for the determination of two tetrodotoxins(TTXs),eg TTX and 4,9 anhTTX,in puffer fish and nassarius with a direct dilution technique.Samples were extracted with acetic acid-methanol(1∶99,by volume).After centrifuged and diluted by 80% methanol solution，the extract was separated on an ACQUITY BEH Amide(100 mm×2.1 mm，1.7 μm) column by gradient elution,with 0.1% formic acid solution containing 05 mmol/L ammonium formate-0.1% formic acid acetonitrile solution as mobile phases,analyzed in ESI+ mode under multiple reaction monitoring(MRM) mode and quantified by external standard method.There were good linear relationships in the range of 0.5-100 μg/L for TTX and 0.5-50 μg/L for 4,9 anhTTX,with their correlation coefficients(r2) larger than 0.99.The limits of detection(LOD) and limits of quantitation(LOQ) were in the ranges of 100-150 μg/kg and 300-450 μg/kg,respectively.Recoveries at three spiked levels ranged from 75.4% to 96.8%,with intra-day relative standard deviations(RSD) and inter-day RSD of 2.3%-9.5% and 5.3%-9.2%,respectively.The method was simple and high sensitive,and was suitable for the determination of two TTXs in puffer fish and nassarius.关键词：direct dilution;tetrodotoxin;ultra high performance liquid chromatography-tandem mass spectrometry;puffer fish;nassarius
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发布时间：2023-04-18 - 摘要：A method of solid phase extraction/gas chromatography-mass spectrometry was developed for the simultaneous determination of 23 organochlorine pesticides in soil.And different matrix effect compensation approaches were studied.Soil samples were extracted with n hexane-acetone(1∶1,by volume),then purified with a florisil column,and finally detected by GC-MS.Medium or strong matrix effects existed in 7 organic chlorines,which was controlled within 20% for all the 23 organochlorines when 10 mL dichloromethane∶n-hexane(1∶9,by volume) and 10 mL acetone∶n hexane(1∶9,by volume) were selected as the eluents of solid phase extraction,and the pulse pressure was set at 275.8 kPa.Results showed that there was a good linear relationship of the method in the concentration range of 04-10 μg·mL-1 with correlation coefficients(r2) no less than 0.999 2.The limits of detection and limits of quantitation were in the ranges of 1.0-8.6 μg·kg-1 and 4.0-34.4 μg·kg-1,respectively.The average recoveries for blank soil at spiked levels of 20,60 and 100 μg·kg-1 ranged from 46.3% to 109%,with relative standard deviations(RSDs,n=6) of 0.68%-15%.Five organochlorine pesticides,including α-BHC,γ-BHC,p,p′-DDE,endrin aldehyde,p,p′-DDT were detected in a soil sample.关键词：soil;organochlorine;clean-up;injection condition;matrix effect
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发布时间：2023-04-18 - 摘要：An ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) with isotope dilution was developed for the analysis of progesterone in human serum.The serum samples were extracted by liquid-liquid extraction(LLE) with ethyl acetate and n-hexane,then separated on an Acquity UPLC BEH C18 column(2.1 mm×100 mm,1.7 μm) by gradient elution in 5 min,and finally analyzed by UPLC-MS/MS with electrospray ionization in positive ion mode under multiple reaction monitoring(MRM) mode and quantified by isotope internal standard.Impact of the two step LLE extraction on progesterone was investigated.Higher separation performance was observed when methanol-water containing 0.1% aqueous ammonia was used as mobile phase.The stability of serum extracts was also investigated.Results showed that the calibration curves for progesterone were linear in the concentration range of 10-10 000 pg/mL with correlation coefficients(r2) of 0.999 8．The limit of detection(LOD,S/N=3) and limit of quantitation(LOQ,S/N=10) were 5 pg/mL and 10 pg/mL,respectively.Recoveries for progesterone ranged from 91.5% to 106% with the intra relative standard deviations(RSD) and inter RSD of 1.2%-8.2% and 4.1%-9.1%,respectively.This method was applied in the determination of progesterone in serum samples from thirty individual donors with the progesterone concentrations ranging from 0.050 2 ng/mL to 1.363 5 ng/mL.With the characteristics of high sensitivity,good accuracy and reliability,this method could be used in the detection of progesterone in clinical serum samples.关键词：progesterone;isotope dilution;ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS);liquid-liquid extraction(LLE);serum
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发布时间：2023-04-18 - 摘要：A high performance liquid chromatography with evaporative light scattering detector was developed for the determination of main components in polymyxin B and polymyxin E crude drugs.Analytes were separated on a Phenomenex Kinetex Biphenyl column(50 mm×4.6 mm id,5 μm) by gradient elution with methanol and 20 mmol/L ammonium acetate aqueous solution containing 0.6% formic acid as mobile phases at a flow rate of 0.5 mL/min.The parameters for evaporative light scattering detector were as follows:drift tube temperature:55 ℃,carrier gas pressure:20 psi,and the gain:250.Results showed that there were good linear relationships for the analytes in polymyxin B and polymyxin E in the concentration range of 10-200 μg/mL with their detection limits of 0.8 μg/mL and 1.2 μg/mL,and their quantitation limits of 2.6 μg/mL and 4.0 μg/mL,respectively.The intra batch recoveries for polymyxin B and polymyxin E were in the ranges of 100%-104% and 101%-103%,with intra batch relative standard deviations of 0.90%-2.4% and 0.90%-2.6%,respectively.The inter batch recoveries were in the ranges of 101%-103% and 101%-102%,with inter-batch relative standard deviations of 1.1%-1.9% and 1.3%-1.7%,respectively.Compared with microbiological detection method,the developed method is simpler,more precise and more accurate in the detection of analytes in crude drugs,and could be applied to the quality control of polymyxin B and polymyxin E crude drugs.关键词：polymyxin B;polymyxin E;high performance liquid chromatography-evaporative light scattering detector;crude drugs;content
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发布时间：2023-04-18 - 摘要：In this paper,a new luminol electrochemiluminescence signal enhancement technique based on tetraphenylethylene(TPE) modified electrode was developed for the determination of dissolved oxygen in solution.TPE molecules were modified on the surface of gold electrode to form porous and amorphous self assembled films at room temperature.Oxygen molecules and superoxide radical O·-2 were efficiently captured due to the synergistic effect between the enlarged specific surface area of the electrode and the pores,thus the electrochemiluminescence intensity of luminol solution was enhanced.TPE modified electrode exhibited high stability and good reproducibility.The ECL intensity of luminol was changed by adding nitrogen to remove oxygen at different times,then the concentration of dissolved oxygen in the solution could be calculated quantitatively.Results showed that there was a good linear relationship between nitrogen duration(1-6 min) and concentration of dissolved oxygen in the range of 1.63-0.190 mg/L with a correlation coefficient(r2) of 0.990 9.The detection limit for initial concentration of dissolved oxygen was 1.89 mg/L.With the advantages of convenience,rapidness,sensitivity,the method provides a new approach for the detection of dissolved oxygen.关键词：luminol;tetraphenylethylene(TPE);dissolved oxygen detection;electrochemiluminescence(ECL)
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发布时间：2023-04-18 - 摘要：A solid phase microextraction(SPME) probe based on graphene self assembly was prepared in situ,which was combined with GC-MS to develop a method for determination of toluene,ethylbenzene and o xylene in water.SEM characterization results showed that graphene on the probe prepared was uniformly and firmly bonded to the quartz fiber.The effects of extraction mode,extraction temperature,extraction time and salinity were optimized.Under the optimum conditions,three benzenes showed good linearity in the concentration range of 0.2-200 μg/L,with their linear coefficients(r2) of 0.998 7-0.999 6.The limits of detection of this method ranged from 0.001 2 μg/L to 0.004 2 μg/L with relative standard deviations less than 5%.Three collected samples were detected to observe benzene series pollution with different concentrations.The spiked recoveries ranged from 90.3% to 111%.This method could be used for the determination of benzene series in environmental water samples.关键词：solid phase microextraction;graphene;in situ self assembly;benzene series;water
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发布时间：2023-04-18 - 摘要：Polymerase chain reaction(PCR) has become a more and more important detection technique for identification of animal sources,plant sources,genetically modified organisms(GMOs) and microorganisms in food safety detection field.The PCR technique evolving from conventional PCR(cPCR) to fluorescent PCR(qPCR) and digital PCR(dPCR),has gradually been applied in the qualitative,relative quantification and absolute quantification due to its ability to detect small amounts of nucleic acid in raw food materials,while dPCR,is especially of great advantage both in efficiency and accuracy compared with other methods.The latest research progresses of dPCR in food safety detection in recent five years are summarized in this paper,the relevant standards of cPCR,qPCR and dPCR in food analysis are compared,and the technical advances and problems of dPCR in different food safety fields are discussed.Finally,The future development of dPCR technique is anticipate.关键词：polymerase chain reaction(PCR);fluorescent PCR(qPCR);digital PCR(dPCR);food safety detection
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发布时间：2023-04-18 - 摘要：Sulfonamides(SAs) residues are closely related to food safety level.Development of rapid,efficient and highly selective pretreatment methods is the key point for determination of SAs owing to the presence of complicated matrices.Solid phase extraction(SPE),featuring with low solvent consumption,environmental friendliness,high selectivity,high sensitivity,timesaving,low cost and compatibility with different detection methods,has been widely applied in the sample pretreatment for SAs.In this review,advances of SPE application in the analysis of SAs are summarized,mainly including pipette tip SPE,magnetic SPE,molecularly imprinted SPE,in tube SPE and other SPE.关键词：solid phase extraction;sulfonamides;residue analysis;review
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发布时间：2023-04-18 - 摘要：The usage amount of organic pesticides has increased significantly with the development of agriculture,forestry,animal husbandry and aquaculture in China.The increasing level of organic pesticide contaminations to natural waters has posed a potential adverse effect to aquatic ecosystem and human health.The mechanisms,advantages and disadvantages of detection methods for organic pesticides in water,including pretreatment methods and detection methods,are summarized in this paper,and the development trends for these methods are prospected.Results of review and comparative analysis show that gas chromatography and liquid chromatography are the most effective methods for detection of organic pesticide residues in water.This paper provides an important reference for the detection of organic pesticides in water.关键词：organic pesticide;pesticides pollution;pretreatment method;detection method
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发布时间：2023-04-18
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