最新刊期
卷 36 ， 期 12 ， 2017
- 摘要：In this study,the ultra high performance liquid chromatography-Q exactive hybrid quadrupole-orbitrap high-resolution accurate mass spectrometry(UHPLC-Q-Orbitrap-HRMS) was firstly applied in the analysis of the plasma from the glioma patients and the normal control group to find the differential metabolites,which could provide the scientific evidence for clinical diagnosis and pathogenesis research.The spectra obtained by UHPLC-Q-Orbitrap HRMS were conducted to peak identification,peak matching and denoising.The data of metabolomics were statistically analyzed by using principal component analysis and orthogonal partial least-squares-discriminant analysis method to screen the differential metabolites with VIP>10 and P<005,which were investigated to further evaluate the diagnostic ability.The results showed that the plasma metabolic profiles of glioma patients were dramatically altered,and ten potential biomarkers were identified.The metabolites of leucine,valine,tryptophan,choline and taurine were significantly reduced in glioma patients,while histidine,citric acid,lactic acid,creatine and pyruvic acid were obviously increased compared with the normal controls(P<005),which suggested that amino acid and energy metabolism might play an important role in the development of glioma.In addition,the different metabolites showed good diagnostic ability toward gliomas(AUC>08),which could be used as potential diagnostic biomarkers.关键词：glioma;ultra high performance liquid chromatography-Q exactive hybrid quadrupole-orbitrap high-resolution accurate mass spectrometry;metabolomics;diagnosis biomarker
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发布时间： - 摘要：Based on cryogenic treatment and QuEChERS method,an ultra performance liquid chromatography-high resolution benchtop Q-Exactive mass spectrometry method for the determination of fipronil and its metabolites in animal derived foods was established.The samples were extracted with acetonitrile,and cleaned up by the cryogenic treatment and dispersive solid phase extraction(d-SPE)with the N-propylethlene diamine(PSA)and C18.The chromatographic analysis was performed on a BEH C18 column with 0.1% acetic acid and acetonitrile as mobile phase by gradient elution,and the external standard calibration was used for quantification.The negative ion acquisition mode was applied,and the quantitative analysis was carried out by high resolution mass spectrometry using parallel reaction monitoring(PRM)mode.Fipronil and its metabolites showed good linearities in the concentration ranges of 0.02-2 μg/L and 0.2-20 μg/L,with the correlation coefficients(r2)above 0.992.For liquid or semi-liquid samples(such as milk and eggs)and the solid samples(such as chicken)，the limits of quantification(LOQs)for 4 analytes were between 0.1 μg/kg and 0.2 μg/kg.At different spiked levels,the average recoveries of fipronil and its metabolites in eggs,chicken and milk were in the ranges of 81.6%-96.9%,81.2%-96.0% and 79.1%-100.1%,with the relative standard deviations(RSDs)of 1.3%-11.5%,3.4%-11.4% and 1.5%-10.7%,respectively.The method was simple,sensitive and accurate,and was suitable for the rapid screening and quantitative analysis of fipronil and its metabolites in animal derived foods,and the sensitivity of the method could meet the requirement for residual limitation of EU.关键词：fipronil;animal derived food;QuEChERS;high resolution mass spectrometry;metabolites
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发布时间： - 摘要：In this study,an analytical method was established for the determination of thiamethoxam and its metabolites clothianidin,spirotetramat and its four metabolites such as BYI08330-enol-glucoside,BYI08330-ketohydroxy,BYI08330-enol and BYI08330-mono-hydroxy residues in tomatoes using QuEChERS cleanup with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The residues in samples were extracted with acetonitrile,dehydrated with anhydrous magnesium sulfate and sodium chloride,then purified with primary secondary amine (PSA) sorbent and C18,finally detected by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) under the multi-reactive ion monitoring mode(MRM) and quantified by external standard method.The results showed that good linearities for the seven analytes i.e.thiamethoxam,clothianidin,spirotetramat,BYI08330-enol-glucoside,BYI08330-mono-hydroxy,BYI08330-enol and BYI08330-ketohydroxy were observed in the concentration range of 0.2-2 000 μg/L with the correlation coefficients(r2) not less than 0.999 2. The limits of quantification(LOQs) were 0.002 mg/kg.The average recoveries at the fortified levels of 0.002,0.02,0.20 and 2.00 mg/kg were in the range of 79.9%-104% with the relative standard deviations of 0.94%-6.4%.With the advantages of rapidness,simplicity,high sensitivity and good reproducibility,the method is suitable for the determination of thiamethoxam,clothianidin,spirotetramat and their four metabolites residues in tomatoes.关键词：QuEChERS;UPLC-MS/MS;pesticide residues;tomato
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发布时间： - 摘要：Chiral metal-organic frameworks(MOFs),as a novel type of porous material with many properties such as large surface area,diverse structure,adjustable pore size and good chemical stability,have aroused much attention in the field of chromatographic separation.In this paper,a homochiral MOF［Cu3(HL)2(L)2(bpy)3］·4H2O with 2D chiral network was synthesized through the reaction of two kinds of ligands((1R,2R)-1,2-cyclohexanedicarboxylic acid(H2L) and 4,4′-bipyridine(bpy)) with copper ion via a solvothermal approach.The homochiral MOF ［Cu3(HL)2(L)2(bpy)3］·4H2O was used as chiral stationary phase to fabricate a packed column for high performance liquid chromatography.To investigate the MOF′s chiral recognition ability,a series of racemates were separated on the homochiral MOF column under normal phase condition using n hexane-isopropanol as mobile phase.The homochiral MOF column exhibited a good resolving ability towards 10 kinds of chiral compounds,including alcohols,ketones,acids,epoxy compounds and ethers,etc.The reproducibility and stability of the homochiral MOF column were evaluated.The effect of the injected mass of chiral compound on separation was also investigated.Results indicated that the homochiral MOF column has a good reproducibility and stability for enantioseparation.关键词：metal-organic framework;high-performance liquid chromatography;chiral stationary phase;chiral separation
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发布时间： - 摘要：A rapid method was developed for the screening and quantification of 28 pesticides endocrine disruptors in aquatic products by ultrahigh performance liquid chromatography-quadrupole/electrostatic field obitrap high-resolution mass spectrometry.The samples were extracted with ethyl acetate,and purified with a Captiva ND Lipids column.The separation was carried out on an ACQUITY UPLC@BEN C18 column(2.1 mm×50 mm,1.7 μm) with methanol-water as mobile phases by gradient elution.The 28 pesticides endocrine disruptors were simultaneously analyzed in switching positive and negative modes.The retention time,accurate mass of parent ion and relative isotope abundance were used for fast screening in full scan mode,while accurate mass of fragment ions were used for comfirmation in two-stage threshold-triggered full mass scan mode.Under the optimal conditions,good linearities(r2>0.99) were obtained in their respective linear ranges.The limits of detections(LODs) for most compounds were not more than 10 μg/kg except for acetochlor,procymidone and fenitrothion.The recoveries were in the range of 65.7%-98.9% and the relative standard deviations(RSDs) were 6.2%-11.3%.The method was simple,sensitive and accurate,and was suitable for the rapid screening and confirmation of multiple pesticides endocrine disruptors in aquatic products.关键词：ultra-performance liquid chromatography;obitrap high-resolution mass spectrometry;pesticides;endocrine disruptors;rapid screening
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发布时间： - 摘要：The self-assembly inclusion complexes of β-cyclodextrin(β-CD) and 4-aminoantipyrine(4-AAP) were respectively prepared by the solution method at a constant magnetic field and a non-magnetic field.The β-CD inclusion complexes were characterized by Fourier transform infrared spectroscopy(FT-IR),differential scanning calorimetry(DSC),atomic fluorescence spectrometry(AFS),X-ray powder diffraction(XRD) and scanning electronic microscopy(SEM).The results indicated that the constant magnetic field could influence the self-assembly clathration of β-CD inclusion complexes and improve the bonding effect between the host and the guest.The self-assembly inclusion complexes were easier to be composed.The cavity structures of the β-CD inclusion complexes arranged more orderly,and the crystallinities of the formed inclusion complexes at a constant magnetic field had an even more improvement.关键词：constant magnetic field;β-cyclodextrin;inclusion complex;self-assembly clathration
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发布时间： - 摘要：The relative contents of four kinds of glycan forms in the inovator and biosimilar products of recombinant human thromboplastin(rhTPO) were accurately determined using matrix assisted laser desorption ionization time of flight mass spectrometry(MALDI-TOF MS) with quasi-internal calibration,the consistencies between products and among batches were evaluated.The N-glycan,sialic acid and O-glycan of rhTPO were removed off with different endoglycosidase,respectively.bovine serum albumin(BSA)used as the standard was pointed target separate with the sample.The molecular weights of the intact glycoproteins and the different forms of deglycosylated proteins were determined by MALDI-TOF MS with quasi-internal calibration.The glycan contents in samples were calculated by the molecular weight differences among different deglycosylated samples.Finally,the consistency of the inovator and biosimilar products were evaluated.The multi-charge peaks of BSA were used for the quasi-internal calibration of MALDI-TOF MS.And their calibration relative standard deviations(RSDs) were all no more than 0.075%,and the RSDs among different calibrations were among 0.001%-0.004%.The method deviations away from the sequence molecular weight were less than 0.01%.For the biosimilar drug,the relative contents of N-glycan,sialic acid,O-glycan,and glycation were 24.6%,2.9%，9.0%and 5.1%,respectively,and the batch-to-batch consistency was quite good.The total glycan contents were consistent with those reported in the literature.For the innovator drug,the relative contents of N-glycan,sialic acid,O-glycan and glycation were 25.6%,2.9%,7.9%and 3.5%,respectively.The total glycan content was lower than that reported in the literature.The relative contents of glycosylation between the innoventor products and the biosimilar products were almost the same but the relative contents of glycation showed some differences.Glycation of rhTPO has not been reported up-to-now,the differences of the relative contents of glycation might be the important factors for the different rhTPO-manufacturers,the glycation differences were mainly caused by the differences of fermentation process.关键词：recombinant human thrombopoietin(rhTPO);matrix assisted laser desorption ionization time of flight mass spectrometry(MALDI-TOF MS);quasi-internal calibration;glycan contents;glycation
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发布时间： - 摘要：A rapid method was developed for the determination of 10 organophosphate esters(OPEs) in the Arctic waters by liquid chromatography-mass spectrometry(LC-MS/MS) combined with C18membrane disk extraction.By the optimized pretreatment and instrumental methods,10 OPEs were collected with C18membrane disk from 4 L water,and extracted with dichloromethane in ultrasonic extraction apparatus.After purification and concentration,the OPEs were analyzed by LC-MS/MS under positive electrospray ionization in selective reaction monitoring(SRM) mode.The linear correlation coefficients are in the range of 0.994 4-0.999 9.The recoveries of 10 OPEs in water samples ranged from 64.1% to 115% with the method detection limits of 0.08-0.55 ng/L.Furthermore,10 OPEs compounds in the Arctic waters samples were analyzed by this method,and the OPEs concentrations in the river and seawater were in the ranges of 0.64-6.64 ng/L and 0.09-2.03 ng/L,respectively.关键词：organophosphate esters;C18membrane disk extraction;LC-MS/MS;polar water
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发布时间： - 摘要：A method was developed for the determination of 15 triazole pesticides in vegetables and fruits by gas chromatography(GC) and gas chromatography-mass spectrometry(GC-MS) with ion exchange column.The samples were pretreated quickly,then extracted with acetonitrile after sodium chloride homogenization，separated by liquid-liquid partition．The clear supernatant purified by solid phase extraction with ion exchange column was ready for GC-ECD and GC-MS analysis．Determinations were performed by using selected ion monitoring(SIM) mode,and external standard method was used for quantification．After optimizing the conditions for pretreatment and determination，the method was convenient and rapid．Under the optimal conditions,the quantitation limits of the method(S/N≥10) were 0.01 mg/kg.The recoveries at spiked levels of 0.01，0.05,0.10 mg/kg were in the range of 68%-102% with the relative standard deviations of 2.4%-16.2%.Besides,the pretreatment has a good purification effect in GC-ECD chromatogram.The method is easy，rapid and sensitive,and could meet the requirements for the analysis of 15 triazole pesticides in vegetables and fruits.关键词：solid phase extraction(SPE);gas chromatography;gas chromatography-mass spectrometry;triazole fungicides;triazole plant growth mediations;vegetables and fruits
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发布时间： - 摘要：A homemade LC-MS interface was developed.The interface included atmospheric interface,ion source and electronic communication interface which connected to high-performance liquid chromatography and mass spectrometry′s software.The team self-developed API-TOFMS 10000 was successfully linked to Thermo Fisher Scientific Diana U3000.Experimental results showed that the self-built LC-MS was operated with a good stability(RSD=5.6%),the linear correlation coefficient(r2) was 0.995 8,the detection range: 2-2 000 pg,the limit of quantitation: 2 pg,and the detection limit: 0.5 pg.Piroxicam,theophylline and prednisone could be obviously detected.The experimental data showed that the self-developed LC-MS interface could meet the testing requirements,and the self-built LC-MS has an application potential in biochemistry,pharmaceutical analysis,food safety,environmental detection etc.关键词：LC-MS;interface technology;atmospheric pressure interface;ion source
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发布时间： - 摘要：An analytical method was developed for the simultaneous determination of 24 insecticide residues in cucumber and tomato by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The samples were firstly extracted with acetonitrile,then purified by QuEChERS method and centrifuged at a high speed,finally filtered with a 0.22 μm membrane filter before UPLC-MS/MS determination.The results indicated that there were good linear relationships for 24 kinds of insecticides in the concentration range of 0.1-50 μg/L with the linear correlation coefficients(r2) more than 0.99.The average recoveries for the target compounds at four spiked levels of 0.002,0.01,0.1,1.0 mg/kg were in the range of 70.3%-110% with the relative standard deviations less than 15%.The limits of quantitation(LOQs) and the limits of detection(LODs) of the method were in the ranges of 0.05-5 μg/kg and 0.01-1.82 μg/kg,respectively,which could meet the detection requirements.This method is suitable for the simultaneous detection on 24 insecticides in cucumber and tomato with the advantages of high sensitivity,accuracy and efficiency.关键词：QuEChERS;ultra performance liquid chromatography tandem mass spectrometry;insecticide;tomato;cucumber;residues
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发布时间： - 摘要：A method of solid-phase extraction(SPE) and high performance liquid chromatography-tandem mass spectrometry(SPE/HPLC-MS/MS) was developed for the simultaneous determination of 24 pesticides in water.The samples were extracted with acetonitrile,then enriched and purified with solid-phase extraction cartridges.Acetonitrile and 0.1%(by volume) formic acid aqueous solution were used as mobile phases.Target pesticides were analyzed by HPLC-MS/MS in positive electrospray ionization(ESI+) under multiple reaction monitoring(MRM) mode.Results showed that 24 pesticides were separated in 25 min with excellent linear relationships(r2≥0.998).The recoveries at spiked levels of 5,20,100 μg/L in water samples ranged from 65.9%-127.8% with relative standard deviations(RSDs) of 0.7%-14.2%.The limits of detection were in the range of 0.05-0.71 ng/L.This method was applied in the detection of the water samples from 10 estuaries and 2 reservoirs in Dalian，and 10 pesticides were detected in the concentration range of 0.2-558.3 ng/L.The proposed SPE/HPLC-MS/MS method is efficient and sensitive,and is suitable for the determination of various pesticides in actual water samples.关键词：solid-phase extraction(SPE);high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS);pesticides;water detection
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发布时间： - 摘要：The methylene blue(MB)solution was determined by mobile phone colorimetric method based on standard deviation transfer law.Through the relationship between the color primary color value RGB and the gray value Gr,calculated by the standard deviation transfer formula,the feasibility of the indirect measurement method was proved theoratically.The influences of three kinds of lighting environment on the quality of photos were analyzed,and three types of mobile phones were used as sampling tools.Results showed that the precision of indirect measurement method was significantly improved.The indirect measurement values XR,XG,XB of phone picture color showed a similar changing trend with methylene blue concentration.XB was proportional to the concentration C.A new method for the determination of methylene blue concentration was established.The recoveries for the method were between 91.3% and 101% with the relative standard deviations of 2.7%-4.8%.The stability,precision and accuracy meet the requirements for determination.关键词：standard deviation;phone colorimetric method;methylene blue
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发布时间： - 摘要：In this study,a method for the preparation of high purity hesperetin based on reversed-phase silica gel purification was established.The factors such as loading volume,flow rate and eluent polarity were optimized.Structure of the product was identified by infrared spectroscopy and nuclear magnetic resonance,and the purity of the analyte was 99.87%.The daily preparation efficiency of the method could reach to gram-grade.With the advantages of high efficiency,large preparation and high separation efficiency,the method could provide a technical support for the preparation of certified reference material of hesperetin.关键词：hesperetin;reverse phase silica gel;purification;qualitative analysis;high performance liquid chromatography
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发布时间： - 摘要：Cadmium ion imprinted polymers(Cd(Ⅱ)-IIP) were prepared by microwave-assisted inverse emulsion polymerization method with β-cyclodextrin and acrylamide as functional monomers,epichlorohydrin as crosslinking agent and ammonium persulfate as initiator.The Cd(Ⅱ)-IIP was characterized by scanning electron microscopy(SEM).Results showed that the Cd(Ⅱ)-IIP became uneven after elution,and had a complex pore structure on the surface.These specific recognition sites benifited the Cd(Ⅱ)-IIP to recognize and adsorb Cd(Ⅱ).The result of adsorption isotherm showed that the adsorption process of the Cd(Ⅱ)-IIP followed the Langmuir adsorption model(r2>0.99).The adsorption process obeyed Scatchard model,and the dissociation constant KD and the maximum apparent adsorption binding capacity Qmax were 72.99 mg/L and 130 mg/g,respectively.The optimum extraction condition was listed as follows:eluent:methanol-acetic acid(7∶1),the Cd(Ⅱ) concentration:10 μg/L and pH 7.0.The extraction efficiency of Cd(Ⅱ)-IIP was more than 70%when it was used five times.In the presence of the competition ions,the extraction efficiency of Cd(Ⅱ),Cu(Ⅱ),Zn(Ⅱ) and Pb(Ⅱ) was 97.58%,15.07%,5.28%and 40.2%,respectively.The relative standard deviation(RSD) and the detection limit(3σ) of the method were about 2.7%and 0.809 4 μg/L,respectively.The recoveries for Cd(Ⅱ) in waste water samples were between 93.6%and 101%.关键词：microwave-assisted;inverse emulsion polymerization;Cd(Ⅱ) ion imprinted polymers;solid phase extraction
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发布时间： - 摘要：In this paper,an octaethylporphyrin film/K+ exchanged glass optical waveguide sensor was fabricated by spin-coating method immobilizing the octaethylporphyrin compound on K+ glass optical waveguide surface.The sensor was used to detect different volatile gases in optical waveguide detection system.Besides,the preparation conditions for the sensor were optimized.The experimental results showed that the sensor has a high sensitivity to methylamine.The detection limit was 1.0×10-8 V/V0(S/N=5.1),and the response time and recovery time was 1.2 s and 2.3 s,respectively.There also existed a good linear relationship for the results obtained in the parallel experiment with the relative standard deviation of 1.1%,which proved the accuracy of the sensor in methylamine gas detection.关键词：octaethylporphyrin;optical waveguide sensor;methylamine;spin-coating
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发布时间： - 摘要：A capillary electrophoresis with laser induced fluorescence detection(CE-LIF) method was developed for the determinations of polysaccharides in traditional Chinese medicines(TCMs) and N-glycome in human serum glycoprotein in this paper.After pre column derivatized with 9-aminopyrene-1,4,6-trisulfonate(APTS) by reductive amination,the seven monosaccharides were sufficiently separated within 15 min.In the analysis of real samples,the average recoveries for the analytes were all in the range of 88.0%-102% with relative standard deviations(RSDs) lower than 3.0%.The method is sensitive,accurate and reliable,and is suitable for the determination of monosaccharide composition in Chinese medicinal preparation.Meanwhile,fingerprints of N-glycome in human serum were established based on capillary gel electrophoresis(CGE).A poly(vinly alcohol) neutrally coated column was used to suppress the electroosmotic flow which would increase the analysis time,and the excellent separation of glycan isomers was realized.5 μL human sera was analyzed and a total of 17 fractions were isolated(RFU>0.2).The analysis of N-glycan profile has made it possible to research the glycosylation alterations of complex biological fluid.关键词：capillary electrophoresis with laser-induced fluorescence;polysaccharides from traditional Chinese medicines;N-glycosylation;glycoprotein
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发布时间： - 摘要：In this paper,a method was established for the analysis of 11 heavy metal elements(Cu，Mn，Cr，Pb，Cd，Ni，Sb，Hg，Co，Ag，As) in grain and vegetables using inductively coupled plasma mass spectrometry(ICP-MS) with microwave digestion.The instrumental parameters and microwave digestion conditions were optimized.Samples were digested completely using HNO3-HF-H2O2 and HNO3-H2O2.And the results showed that the linear correlation cofficients of eleven elements(r) were not less than 0.999 5,the limits of detection were in the range of 0.001-10.00 μg/L and the relative standard deviations(RSD，n=5) were not more than 5.0%.This method has the advantages of rapidness,simplicity,high sensitivity,good stability and accuracy.关键词：microwave digestion;inductively coupled plasma mass spectrometry;heavy metals elements;grain and vegetable
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发布时间： - 摘要：Synthetic musks(SMs) are widely used as a substitute of natural musks in consumer products for their low price,special and long-lasting fragrance.They are divided into nitro musks,polycyclic musks and macro musks according to their chemical structures.With the mass production and extensive usage,SMs are continuely released into the environment via direct or indirect ways,and becoming emerging pollutants.Numerous reports have shown that SMs,especially galaxolide(HHCB),tonalide(AHTN),musk xylene(MX) and musk ketone(MK),are available in aquatic environment,soil,air and organisms.Due to their high lipophilicity and persistency,synthetic musks accumulate and produce toxic effect in biotas,thus having increasing impact on ecology and giving rise to public concern.In this paper,the characteristics,exact classification,environmental occurrences and the analysis of SMs are introduced.The main focus is on the analytical methods such as GC and GC-MS,the most common detection methods for SMs.Mass spectrometry is firstly preferred among the analytical methods because of its high selectivity,accuracy and sensitivy in qualitative and quantitative analyses.The preparation techniques for samples with different matrix(eg.water,sewage sluge,sediment,air and biotas) to reduce interference are also discussed,which may still be a notable problem in the near future.关键词：synthetic musks(SMs);analytical methods;sample preparation;environmental occurrences;review
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发布时间： - 摘要：Dynamic light scattering(DLS),as a conventional analysis method by particle size,has the advantages of free separation,easy operation,low test costs and easy data processing etc.Functionalized AuNPs,in addition to thier own particle properties,could also specifically identify the target,significantly amplify the light scattering signals from the target,and ultimately achieve a fast,specific and sensitive detection on the target through the DLS technique.In this paper,research progresses on the application of DLS with gold nanoparticles in detection on the target were reviewed.Some problems in the application process of DLS technique were discussed,which was intended to provide some reference for its practical application.关键词：AuNPs;dynamic light scattering;limit of detection;sample detection;review
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