最新刊期
卷 39 ， 期 6 ， 2020
- 摘要：Aiming at the scientific problem that oil crops contain a variety of lipid molecules which structures are difficult to identify,an ultra high performance liquid chromatography-high resolution mass spectrometry was developed for the analysis of lipids in five kinds of oilseeds,i.e.rapeseed,soybean,peanut,sunflower seed and corn.Lipids were separated by using reversed phase chromatographic column ACQUITY UPLC BEH C18(2.1 mm×100 mm,1.7 μm).In UPLC-Orbitrap Fusion Mass positive or negative ion mode,Data Dependent MS2 data were collected,and lipid molecules were characterized by using secondary mass spectrometry fragment characteristics,accurate molecular mass,retention time and database matching,then the unique structural formulas of the lipid molecules were obtained.A total of 132 lipid molecules in oil crops were identified in this research,including 8 diglyceride(DG）,5 lysophosphatidylcholine(LPC）,2 lysophosphatidyl ethanolamine(LPE）,24 phosphatidylcholine(PC）,18 phosphatidyl ethanolamine(PE）,8 phosphatidyl inositol(PI）,1 phosphatidyl glycerol(PG）,1 phosphatidyl serine(PS） and 65 triglyceride(TG）,then peak area ratio was used to compare their relative contents.This method could well realize the separation of lipid components and improve the analysis of lipid components in oil crops from the level of fatty acid analysis to the level of lipid molecules,and it provides a research basis for better application of lipid components in oil crops and promotes the development of lipidomics.关键词：oil crops;lipid;ultra high performance liquid chromatography-high resolution mass spectrometry
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发布时间：2023-04-18 - 摘要：In this work,an ultra high performance liquid chromatography-quadrupole-orbitrap mass spectrometry was developed for non directional screening of mycotoxins in dairy products.Under the mass spectrometry data dependent scanning mode,the molecular ion mass to charge ratios,secondary fragmented fragments mass to charge ratios and retention times of 38 typical mycotoxins reference materials were collected.A standard database for mycotoxins was established,and the analysis on fragmentation path was completed.The characteristic fragment fragments were combined with the standard database for mycotoxins in a mass spectrum independent scanning mode to finally achieve a non-directional screening of mycotoxins in dairy products.The detection limit(CCα) and the detection capacity(CCβ) of this method were in the ranges of 0.01-0.36 μg/kg and 0.03-0.57 μg/kg,respectively.and the recoveries ranged from 81.9% to 111% with relative standard deviations of 1.1%-6.1%.The established method was used to screen 40 batches of pasteurized milk,ultra high temperature instant sterilized milk,milk containing beverages and infant formula milk powder.Results showed that the method was simple and rapid,and could meet the requirements for accurate determination and quantitation of mycotoxins in dairy products.关键词：dairy products;mycotoxin;ultra high performance liquid chromatography-quadrupole-orbitrap mass spectrometry;non directional screening
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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 developed for the simultaneous determination of 23 bisphenol analogs and their halogenated derivatives(BPs） in urine and serum based on derivatization of pyridine-3-sulfonyl chloride.Urine samples were extracted by liquid-liquid extraction with ethyl acetate,while serum samples were extracted with acetonitrile and followed by PRiME HLB cartridge purification.After derivatization with pyridine-3-sulfonyl chloride,the extracts were separated on an ACQUITY UPLC BEH C18(2.1 mm×100 mm，1.7 μm） column with acetonitrile and water containing 0.1% formic acid as mobile phases,and determined by UPLC-MS/MS with electrospray ionization(ESI） in positive ion mode.There were good linear relationships for 23 BPs in both urine and serum samples in the range of 0.005-100 μg/L,with their limits of detection between 0.002 μg/L and 0.030 μg/L ，limits of quantitation between 0.005 μg/L and 0.100 μg/L.Average recoveries ranged from 76.6% to 122%,with relative standard deviations(RSD） of 0.60%-14%.The method was applied in the analysis of BPs in 20 urine samples and 20 serum samples.The method could meet the requirements for simultaneous determination of 23 BPs in urine and serum samples with low sample consumption and high sensitivity.关键词：bisphenol analogs and their halogenated derivatives;urine;serum;pyridine 3 sulfonyl chloride;ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS）
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发布时间：2023-04-18 - 摘要：Acrylamide(AA) and 5-hydroxymethylfurfural(5-HMF) are mainly formed by Maillard reaction,which have attracted much attention due to their widespread existence in foods and their significant toxicological effects.In this paper,a new method was developed for the determination of AA and 5-HMF in edible oils by micellar electrokinetic chromatography with microwave-assisted ionic liquid dispersive liquid-liquid microextraction without dispersant.Factors affecting the recovery were optimized in the experiments,including type and volume of ionic liquid,microwave assisted extraction conditions,sample volume and separation conditions of micellar electrokinetic chromatography.Under the optimized conditions,the method exhibited a good linearity in the range of 0.5-50 μg/mL with correlation coefficients(r2) not less than 0.997 1.The limits of detections(S/N=3) for AA and 5-HMF were 0.11 μg/mL and 0.70 μg/mL,respectively.The spiked recoveries were in the range of 77.9%-96.2% with relative standard deviations(RSDs) of 1.3%-5.2%.5-HMF was found in three kinds of sesame oils and a pepper oil with concentrations of 1.1-3.3 μg/mL.The proposed method was simple,efficient,inexpensive and ecofriendly,and it was applicable for the analysis of AA and 5-HMF in edible oils.
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发布时间：2023-04-18 - 摘要：A method of inductively coupled plasma mass spectrometry(ICP-MS） with Au solvent trapping was established for the simultaneous determination of 7 kinds of heavy metal elements,i.e.chromium,nickel,arsenic,lead,cadmium,antimony and mercury in e-cigarette aerosols.The trapping conditions for e-cigarette aerosols were optimized.The aerosols were trapped with dilute nitric acid solution(5.0%,by volume） containing 2.0 mg/L Au solution.Two impingers were tandemly connected,in which each contained 25.0 mL trapping solution,and the puffing number was 100.Results showed that,seven elements in e cigarette aerosols were trapped effectively.Under the optimal conditions,the calibration curves were linear in the range of 0.3-80 μg/L for Cr,Ni, As,Pb,Cd,and 0.3-10 μg/L for Sb,Hg,with their correlation coefficients(r2) larger than 0.999.The limits of detection(LODs） for seven elements were in the range of 0.69-1.19 ng/100 puffs,and the limits of quantitation were 2.29-3.97 ng/100 puffs.The recoveries ranged from 96.5% to 103% with relative standard deviations(RSD） of 6.6%-14%10 commercial e-cigarettes were determined by this method and the French Standardization,respectively,and the detection results were consistent.Therefore,this method was accurate,reliable,efficient and low-consumption,which could be used for the detection of heavy metals in e cigarette aerosols.关键词：e-cigarette;aerosols;heavy metals;Au nitric solution;inductively coupled plasma mass spectrometry(ICP-MS）
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发布时间：2023-04-18 - 摘要：A method was developed for the simultaneous determination of bisphenol substances in drug and food homologous products by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS） combined with accelerated solvent extraction(ASE） and QuEChERS.The samples were extracted at 80 ℃ via two cycles of ASE,with acetonitrile-acetic acid-water(89∶1∶10,by volume） for 6 min,then purified by QuEChERS.11 bisphenol substances were separated on an ACQUITY UPLC HSS T3 column(2.1 mm×100 mm,1.8 μm） by gradient elution using methanol containing 0.1% formic acid and 5 mmol/L ammonium acetate containing 0.1% formic acid as mobile phases,then analyzed by MS/MS with electrospray ionization in positive and negative mode under multiple reaction monitoring(MRM） mode,finally quantified by internal standard method.There were good linear relationships for 11 bisphenol substances in the concentration range of 0.5-50.0 μg/L,with correlation coefficients(r2） not less than 0.996 0.The limits of detection(LOD） and limits of quantitation(LOQ） for 11 bisphenol substances were in the ranges of 0.1-0.5 μg/kg and 0.3-1.5 μg/kg,respectively.The recoveries at three spiked levels ranged from 72.4% to 108% with relative standard deviations(RSD） of 1.7%-15%.The proposed method was simple,rapid,high sensitive and reproducible,and it was suitable for the rapid determination of 11 bisphenol substances in drug and food homologous products.关键词：accelerated solvent extraction(ASE）;QuEChERS;ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS）;bisphenol substances;drug and food homologous products
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发布时间：2023-04-18 - 摘要：In this article,a surface enhanced Raman spectroscopy(SERS） based on filter paper substrate was developed for the recyclable detection of chlorpyrifos in water.The substrate was prepared by loading the filter paper with Ag nanoparticles(AgNPs） and ZnO nanoparticles,which has a uniform distribution of hot spot and a good detection stability,and exhibits a high performance in the detection of chlorpyrifos,with a limit of detection(LOD） of 48.53 μg/L and a linear range of 50-500 μg/L.Stability for cycle detection of the substrate was investigated under UV irradiation,and Results showed that chlorpyrifos pesticide could be degraded with ZnO nanoparticles as photocatalyst under the circular irradiation of UV light.Meanwhile,the substrate remained a high Raman activity in each detection.The detection substrate combined with SERS was applied to the detection of chlorpyrifos in real surface water.The spiked recoveries were in the range of 111%-139% with relative standard deviations(RSDs） not more than 12%.The detection limit for chlorpyrifos residues in water based on the fabricated substrate in this paper could meet the limit requirements for groundwater quality standard towards chlorpyrifos in agricultural water and the maximum residue limit value for chlorpyrifos in fruits and vegetables in the pesticide residue limit standard towards food.With the advantages of simple operation,short time consumption and low cost,this method has a great potential in the rapid detection of pesticide residues.关键词：paper-based Raman spectroscopy;photocatalysis;water;chlorpyrifos
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发布时间：2023-04-18 - 摘要：A novel high performance liquid chromatography(HPLC) with magnetic solid phase extraction(MSPE) based on multi template molecularly imprinted polymer(MIP) was developed for the detection of tetracyclines in environmental water samples.The multi template MIP was prepared by sol-gel method,with mesoporous silicon magnetic graphene oxide as carrier,tetracycline,oxytetracycline,chlortetracycline and doxycycline as templates,and N-［3-(trimethoxysilyl)propyl］ethylenedi amine(KH-792) and anilinomethyl triethoxysilane(KH-42) as functional monomers,which was characterized by field emission scanning electron microscopy(SEM),infrared spectroscopy(IR) and vibrating sample magnetometry(VSM).The method was applied in the detection of tetracycline,oxytetracycline,chlortetracycline and doxycycline in water samples.Results showed that the calibration curves for 4 tetracyclines were linear in the range of 5-50 μg/L,with their detection limits and quantitation limits of 0.67-0.95 μg/L and 2.13-3.50 μg/L,respectively.The spiked recoveries ranged from 82.7% to 103% with relative standard deviations(RSD) of 1.0%-8.8%.The proposed method could be used for the simultaneous and selective detection of these four tetracyclines in real environmental water samples.关键词：tetracyclines;multi template molecularly imprinted polymers(MIP);magnetic solid phase extraction;high performance liquid chromatography(HPLC)
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发布时间：2023-04-18 - 摘要：A method was established for screening and quantitative determination of cimetidine and ranitidine in cosmetics by high performance liquid chromatography-quadrupole/time of flight high resolution mass spectrometry.In addition,the tandem MS fragment pathways of cimetidine and ranitidine were studied.Samples were ultrasonically extracted with methanol and filtered,then separated on a Zorbax SB-Aq column(3.0 mm×100 mm,1.8 μm) with acetonitrile and water containing 0.1% formic acid as mobile phases by gradient elution,finally analyzed with double spray electrospray ion source in positive mode.Data were acquired in full mass scan and target mass/mass scan modes.In different cosmetic matrixes,there were good linear relationships for cimetidine and ranitidine in concentration ranges of 5.65-113 ng/mL and 4.95-99.0 ng/mL,respectively,with their correlation coefficients(r) larger than 0.999.The limits of detection for cimetidine and ranitidine were 1.1 ng/mL and 0.99 ng/mL,and the limits of quantitation were 5.6 ng/mL and 5.0 ng/mL,respectively.The recoveries of two analytes at three spiked levels varied from 86.7% to 110% with relative standard deviations(RSD) of 0.90%-6.0%,and the repeatability was satisfactory(RSD<10%).The proposed method is simple,rapid and sensitive,and could be applied in quick screening and quantitative analysis of cimetidine and ranitidine in cosmetics.关键词：high performance liquid chromatography-quadrupole/time of flight mass spectrometry;cosmetics;cimetidine;ranitidine
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发布时间：2023-04-18 - 摘要：Nitrogen fluoride co-doped carbon dots(NFCDs) were synthesized by hydrothermal method using citric acid,L-lysine and sodium fluoride as raw material.The structures of carbon dots were characterized by transmission electron microscopy(TEM),Fourier transform infrared spectroscopy(FT-IR),ultraviolet visible spectroscopy(UV-Vis) and fluorescence spectroscopy.Based on the fluorescence resonance energy transfer between riboflavin and NFCDs,a NFCDs fluorescent probe was constructed for the detection of riboflavin.Under the optimized experimental conditions,the detection linearity of this method for riboflavin ranged from 3.0 μmol/L to 66.5 μmol/L with a detection limit of 0.26 μmol/L,calculated by 3 times of the signal-to-noise ratio.The probe was successfully applied to the determination of riboflavin in milk and milk powder with recoveries of 96.7%-103%.In addition,the low toxicity of NFCDs on HeLa cells was determined by the MTT assay,and they were also applied to fluorescence imaging of cells,and the presence of riboflavin in cells was successfully confirmed by laser scanning confocal microscopy.关键词：nitrogen fluoride co doped carbon dots(NFCDs);fluorescent probes;fluorescence resonance energy transfer;riboflavin
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发布时间：2023-04-18 - 摘要：A pyrolysis gas chromatography-mass spectrometry with silica as dispersant for sample preparatio was developed for the quantitative analysis of blend ratio of polycarbonate(PC) to acrylonitrile-butadiene-styrene copolymer(ABS).The samples were dispersed with silica after freeze fracturing,then weighed carefully and injected.The pyrograms of the samples were obtained at a pyrolysis temperature of 600 ℃.The characteristic peak of styrene in thermally decomposed polyester was selected as the quantitative peak for determination of the blending ration of PC and ABS in PC/ABS blend.A series of content known PC/ABS blend standards were prepared using silica as dispersant.Results showed that there were good linear relationships between styrene peak area and ABS concentration in the range of 0.06-20 g/kg(corresponding to PC∶ABS ratio of 99.7∶0.30-0∶100),with their correlation coefficient(r2) of 0.994.The detection limit(S/N=5) of the method for ABS was 0.06 g/kg(corresponding a PC to ABS ratio of 99.7∶0.30).The method was applied to the PC/ABS blend samples with known bending ratios.The recoveries ranged from 95.3% to 103% with relative standard deviations(RSDs,n=3) of 1.1%-3.8%.The method is simple,convenient and accurate,ant it is suitable for the analysis of PC/ABS blending ratio in the full range.关键词：pyrolysis gas chromatography-mass spectrometry;PC/ABS blend;solid dispersant;quantitative analysis
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发布时间：2023-04-18 - 摘要：In this study,a DNA biosensor was constructed for the sensitive detection of target DNA by chain reaction,with a specially designed DNA sequence as capture probe and a G-quadruplex-hemin complex as signal molecule.In the presence of target DNA,the capture DNA and the target DNA could recognize each other,while the target DNA could have a continuous chain reaction with the assistant probe,leading to the formation of a large number of G-quadruplex on the electrode surface.In the presence of hemin,the G-quadruplex combines with the hemin to form a G-quadruplex-hemin complex,which emits a strong electrochemical signal.Therefore, the detection of target DNA could be realized as the electrochemical signal obtained by differential pulse voltammetry(DPV) has a corresponding relationship with concentration of the target DNA in the system.Under the optimal conditions for the concentration of each component,the DPV current response has a good linear relationship with the target DNA concentration in the range of 0.01-10 pmol/L,and the minimum detection limit reaches to 8 fmol/L.With the advantages of high sensitivity and good specificity,the sensor has a good application prospect.关键词：DNA biosensor;G-quadruplex;hemin;gene detection
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发布时间：2023-04-18 - 摘要：In this paper,a method of surface enhanced Raman spectroscopy(SERS) based on core shell Au@Ag nanoparticles(Au@AgNPs) was developed for the rapid detection of famotidine(FMD).The Au@AgNPs were synthesized by seed growth method,and then characterized by SEM,TEM,UV-Vis spectrometry and XRD.Rhodamine 6(RG6) was used as the molecular probe to evaluate the SERS performance of Au@AgNPs.The synthesized Au@AgNPs has a uniform morphology and a good enhancement effect,with an enhancement factor of 6.66×105.The Au@AgNPs were used for SERS detection of FMD standard solution.Results showed that there was a good linear relationship between logarithm of concentration and logarithm of FMD peak intensity at 1 540 cm-1 in the range of 0.5-50 μmol/L,with a correlation coefficient(r2) of 0.978 and a detection limit(LOD) of 4.18×10-8 mol/L.Under the same conditions,Au@AgNPs were used for SERS detection of FMD in diluted plasma,with a LOD as low as 1.11×10-7 mol/L.The spiked recoveries were in the range of 91.6%-122% with relation standard deviations of 6.6%-12%.The experimental results demonstrated that this method is fast and sensitive,and has a potential application value in detection of biological sample.关键词：surface enhanced Raman spectroscopy(SERS);core shell Au@Ag nanoparticles;famotidine;plasma
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发布时间：2023-04-18 - 摘要：It is very meaningful for the detection and imaging of H2S in living systems due to its important role in many biological processes.In this work,a novel fluorescent probe,DHCD was designed and synthesized for the detection of H2S based on an excited state intramolecular proton transfer(ESIPT） fluorophore.The free probe showed relatively weak fluorescence as the protection of the OH group on a 2,4-dinitrophenyl group in the fluorophore blocked the ESIPT process.However,in presence of H2S,the sensing system displayed a remarkable fluorescence enhancement accompanying with a large Stokes shift(~165 nm） due to the recovery of the ESIPT process resulting from the thiolysis of the 2,4-dinitrophenyl ether in probe DHCD triggered by HS-.The detecting mechanism of probe DHCD for H2S was confirmed by high resolution mass spectrometry.In PBS-DMSO buffer(pH 7.45,99∶1,by volume）,the normalized fluorescence intensity increased linearly with the concentration of HS- within the range of 0-10 μmol/L,and the detection limit of the probe DHCD for HS- was calculated to be 0.84 μmol/L.In addition,the synthesized probe had not only a high selectivity to H2S other than other biologically related analytes,but also a high anti interference ability against other coexisting species,which could satisfy the requirements for the selective detection of H2S in real samples from different origins.Most importantly,this probe possessed excellent cell permeation and low toxicity,and could be used for fluorescent imaging of H2S in HeLa cells.It thus provides a promising approach for studying the effects of H2S in biological systems,and exhibits a great potential in biological applications.关键词：fluorescent probe;H2S;Stokes shift;fluorescent imaging
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发布时间：2023-04-18 - 摘要：A method was established for the quantitative analysis of protein based on electrospray-differential electromigration-particle counting.Effects of factors such as electrospray voltage,liquid solution flow rate and gas flow rate on particle size distribution were systematically investigated and optimized,and common silica capillaries with an inner diameter of 25 μm and a length of 4.07 cm were used.The method was applied to the quantitative analysis of bovine serum albumin reference materials.Results showed that,under the condition of Taylor cone,a bovine serum albumin reference material and a bovine serum albumin solution reference material could both be accurately quantified at a sample solution flow rate of 300 nL/min,an air flow rate of 1.0 L/min and a carbon dioxide flow rate of 0.1 L/min,with the determined results of 20.05 g/L and 69.52 g/L,respectively.The relative errors were within ±5%,which were consistent with the quantitative values of standard materials.With no need of internal and external standards,the method is fast,accurate and sensitive,and it provides a new analytical approach for absolute protein quantification.关键词：electrospray-differential mobility analysis-condensation particle counter(ES-DMA-CPC);sucrose;bovine serum albumin(BSA);absolute protein quantification
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发布时间：2023-04-18 - 摘要：In this work,a near infrared(NIR) spectroscopy was developed for detection of the chemical composition of flax fiber,as it had become a development trend to rapidly and accurately analyze the chemical composition of flax fiber used for spinning in the process of promoting the preparation and industrial production.Compared with the determination value by chemical analysis,a NIR model for the chemical composition was set up by partial least square method,which could be used in rapid and efficient quantitative analysis of the composition.Results showed that the correction correlation coefficient(RC) and the verification correlation coefficient(RCV) of the established NIR model for cellulose,hemicellulose,lignin and pectin were all above 0.9.The corrected root mean square error(RMSEC) was less than the predicted root mean square error(RESEP),and they both were smaller than 1.External verification and double tailed t test showed that the model prediction results were relatively accurate,and there was no significant difference between the predicted values and the measured values obtained by chemical analysis.Therefore,the NIR based model could be used for rapid prediction of the chemical composition of flax fiber.关键词：flax fiber;chemical composition;near infrared spectroscopy;quantitative analysis
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发布时间：2023-04-18 - 摘要：A high performance liquid chromatography-inductively coupled plasma-mass spectrometric(HPLC-ICP-MS) method was established for the detection of two lead compounds,i.e.trimethyllead and triethyllead in blood and urine.The samples were extracted with benzene as solvent,followed by baci extraction with sodium thiosulfate after sonication and centrifugation.The extracts were separated by HPLC using an Agilent Zorbax Plus C18 column(4.6 mm×100 mm,3.5 μm),with 0.1 mol/L ammonium acetate-0.1 mol/L acetic acid and methanol as mobile phases by isocratic elution,and then detected by ICP-MSResults showed that there were good linear relationships for two lead compounds in blood and urine samples in the ranges of 3-200 ng/mL and 5-400 ng/mL,with their limits of detection and limits of quantitation of 0.85-1.31 ng/mL and 3.00-5.00 ng/mL,respectively.The recoveries ranged from 85.3% to 104% with intra-day and inter-day relative standard deviations(RSD) of 1.8%-10%,and the matrix effects of 88.3%-117%.The developed method was simple,sensitive and accurate,and it was suitable for the determination of trimethyllead and triethyllead in human blood and urine.关键词：high-performance liquid chromatography-inductively coupled plasma-mass spectrometry(HPLC-ICP-MS);trimethyllead;triethyllead;blood;urine
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发布时间：2023-04-18 - 摘要：Ionic liquids were proposed as the potential replacement to the traditional organic solvents and widely used in the formation of aqueous biphasic systems,due to their unique properties,including non-volatility,low toxicity,non flammability,high chemical and thermal stability.The aqueous biphasic systems based on ionic liquids offered their extensive benefits on the extraction of biomolecules and organic compounds,such as fast extraction,simple operation,easy scale and high biocompatibility without using the harmful organic solvents and complicated apparatus.In the paper,the phase separation mechanisms of aqueous biphasic systems and their applications in separation and purification of small organic molecules and biological samples were reviewed.The advantages,drawbacks and future development of the aqueous biphasic systems were also presented.关键词：ionic liquid;aqueous biphasic system;separation mechanism;salting out effect
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发布时间：2023-04-18 - 摘要：A T-Hg(Ⅱ）-T structure with base mismatch was formed based on the proton-substitution reaction between mercury ions and thymine,which could be used as a good recognition component for novel mercury ion sensors.Compared with the traditional detection methods,the new mercury ion sensors with T-Hg(Ⅱ）-T mismatch structure as recognizer had some advantages in efficiency and precision.In this paper,research progress and trend of this mercury ion sensors with T-Hg(Ⅱ）-T structure as recognizer based on different types of reporter groups were summarized,thus providing a reference for the development of mercury ion sensors.关键词：mercury ion sensor;T-Hg(Ⅱ）-T structure;recognition group;reporter group
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发布时间：2023-04-18
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