最新刊期
卷 37 ， 期 6 ， 2018
- 摘要：Based on salting-out assisted liquid-liquid extraction(LLE) and polyvinylpolypyrrolidone(PVPP) cleanup,a method was developed for the determination of seven neonicotinoid pesticides in honey by target single ion monitoring(TSIM)/high-resolution mass spectrometry.The samples were extracted and cleaned up with acetonitrile by salting-out assisted LLE-PVPP method.The chromatographic separation was conducted on a BEH C18 column using methanol-water containing 0.1%formic acid and 5 mmol/L ammonium formate in two phases,as mobile phase by gradient elution.The analysis was performed by high resolution mass spectrometry in TSIM mode,and the quantitation was carried out by the internal standard method.The result showed that salting-out assisted LLE-PPVP cleanup method allowed one-step sample preparation,while TSIM mode showed a wide linear dynamic range with higher sensitivity and accuracy.There existed good linearities(r2>0.999) for seven neonicotinoid pesticides in the concentration ranges of 0.01-100 μg/L or 0.02-100 μg/L.The limits of detection(LODs) and quantitation(LOQs) were in the ranges of 0.03-0.07 μg/kg and 0.1-0.2 μg/kg,respectively.At three spiked levels of 0.2,2,20 μg/kg,the average recoveries for the analytes in honey were between 84.8%and 112.7%,with the intra-day precision(RSDr) and the inter-day precision(RSDR) of 0.9%-5.7%and 3.7%-9.7%,respectively.With the advantages of a rapid and simple pretreatment,low-cost,high sensitivity and good reproducibility,this method was suitable for the determination of neonicotinoid pesticides in honey.关键词：neonicotinoid pesticides;polyvinylpolypyrrolidone(PVPP);target single ion monitoring (TSIM);high resolution mass spectrometry;honey;salting out assisted liquid liquid extraction
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发布时间： - 摘要：An ultra-performance liquid chromatography-Q exactive orbitrap high resolution mass spectrometric（UPLC Orbitrap HRMS） method was utilized for the analysis of ginsenosides compositions in different processd Panax quinquefoliums L.roots.The electrospray ionization（ESI） ion source and orbitrap mass analyzer were equipped，and negative ion mode was used for data collection.On the basis of accurate mass to charge in MS，the accurate molecular weights of ginsenosides were acquired.Based on the second stage of tandem MS data，the fragmentations of ginsenosides were obtained.The characteristic MS fragmentation pathways of different types of ginsenosides were summarized.According to these fragmentation rules，55 ginsenosides in Panax quinquefoliums L.roots were identified，among which protopanaxdiol（PPD） type ginsenosides were 28，protopanaxtriol（PPT） type ginsenosides were 17，oleanane（OLE） type ginsenosides and ocotillol（OCO） type ginsenosides were both 5.The ginsenosides compositions of PPD，PPT，OCO and OLE types in different processd Panax quinquefoliums L.roots were compared.The results obtained provided the information for influences of different processing on ginsenosides composition of Panax quinquefoliums L.roots.The research also provided a reference for the exploitation and utilization of Panax quinquefoliums L.roots，and a clarification for its bio-effectiveness material basis.关键词：ultra-performance liquid chromatography-Q exactive orbitrap high resolution mass spectrometry（UPLC Orbitrap HRMS）;Panax quinquefoliums L.roots;process;ginsenosides
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发布时间： - 摘要：A gas chromatography-triple quadrupole mass spectrometric（GC-MS/MS） method for the determination of 48 pesticide residues in high-acidity fruits was developed using solid-phase extraction as sample preparation method.The samples were extracted with acetonitrile containing 1% acetic acid，purified with a CarbonNH2 and ProElutNH2 solid phase extraction column,and analyzed by GC-MS/MS.Effects of different kinds of extractants，extraction times and types of SPE column on the extraction efficiency were investigated by using pomelo,orange,pineapple and hawthorn matrixes.The results showed that the calibration curves of 48 pesticides were linear in the range of 1.0-100.0 μg/kg with limits of quantitation of 1.0-10.0 μg/kg.The average recoveries for 48 pesticides in four kinds of fruits（pomelo,orange,pineapple and hawthorn） ranged from 70.7% to 118.0% with relative standard deviations（RSD,n=5） not more than 9.7%.With wide detection range,high precision and low detection limit,the method was successfully applied in the detection of commercially available fruit samples.关键词：solid-phase extraction（SPE）;gas chromatography-triple quadrupole mass spectrometry（GC-MS/MS）;pesticide residue;fruit
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发布时间： - 摘要：A rapid method was developed for the simultaneous determinaion of 23 plant growth regulators in vegetables by ultra high performance liquid chromatography-tandem mass spectrometry（UHPLC-MS/MS）.The vegetable samples were extracted with acetonitrile containing 1% acetic acid，followed by salting out with 6 g magnesium sulfate and 1 g sodium chloride，then the solvent extracts were analyzed by UHPLC-MS/MS without further purification.The positive and negative modes and multiple reaction monitoring（MRM） mode were used for identification while the matrix-matched external standard calibration curves were used for quantification.The results showed that there existed good linearities for 23 plant growth regulators in corresponding concentration ranges with their correlation coefficients（r2） higher than 0.98.The average recoveries for 21 plant growth regulators at three spiked levels ranged from 70.2% to 125.6% except that those for chlormequat and mepiquat chloride were from 50.5% to 73.7%，with their relative standard deviations（RSDs） of 0.7%-22.5%.The limits of quantitation of this method were in the range of 1-50 μg/kg.The method is simple，rapid，sensitive and accurate，and is suitable for the rapid qualitation and quantitation for 23 plant growth regulators in vegetables.关键词：ultra high performance liquid chromatography-tandem mass spectrometry（UHPLC-MS/MS）;plant growth regulators;vegetables
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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 six alkaloids,e.g.colchicine,raubasine,veratridine,cevadine,ergotamine and ergocristine in cosmetics.The samples were ultrasonically extracted with a mixed solvent of 0.1% formic acid-acetonitrile,then cleaned up with a Cleanert PCX solid phase extraction column.After separated on a Thermo Hypersil GOLD column,the analytes were detected in multiple reaction monitoring(MRM) mode.Six alkaloids showed good linearities(r2>0.999 0) in the range of 0.2-20 μg/L.The limits of quantitation(LOQs) of the method for six alkaloids were in the range of 2.0-5.3 μg/kg.The average recoveries for six alkaloids at three spiked levels ranged from 83.9% to 101.1% with relative standard deviations of 0.7%-6.6%.The method was rapid,accurate and sensitive,and could be applied in the safety evaluation on alkaloids in cosmetics.关键词：ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS);cosmetics;alkaloids;solid phase extraction(SPE)
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发布时间： - 摘要：A label-free self-enhanced electrochemiluminescence（ECL） immunosensor was fabricated for the ultrasensitive detection of tetrodotoxin（TTX） based on immobilizing tris（2,2′-bipyridyl） ruthenium（Ⅱ）-Au nanoparticles（Ru（bpy）2+3-AuNPs） composites to glassy carbon electrode（GCE） with Nafion.In this strategy,an anti-TTX was able to fix on the electrode surface via Au-N chemical bond for realizing the specific capture toward the target.Meanwhile,TTX could be used as the co-reactant of Ru（bpy）2+3 to promote the ECL intensity.The advantage of this approach is that the electron transfer distance between the emitter and the co reactant is shorter,and the ECL efficiency is improved and the experimental cost is reduced compared with that in the presence of co-reactant in solution or labeling of second antibody.Under the optimum conditions,the change of ECL intensity demonstrated a linear relationship with TTX concentration in the range of 0.01-1 000 μg·L-1,with a limit of detection（LOD） down to 0.01 μg·L-1.This label-free self-enhanced ECL immunosensor exhibited an excellent performance with good stability,reproducibility and sensitivity.The recoveries for TTX in real samples were in the range of 98.0%-104.0%,indicated it has good practical value.关键词：electrochemiluminescence;immunosensor;tetrodotoxin;Nafion-Ru（bpy）2+3-Au composite
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发布时间： - 摘要：A method of two-dimensional liquid chromatography with online enrichment was established for the determination of trace ginkgolic acids in Ginkgo biloba extract（EGB） and their preparations.The liquid chromatography system was composed of two LC pumps,an UV detector,a manual sampling valve,a switching valve and two columns.The ginkgolic acids were enriched on the first dimensional column of ZORBAX Eclipse Plus-C18（2.1 mm×12.5 mm,5 μm） using a methanol-water-trifluoroacetic acid mixture（80∶20∶0.01） as mobile phase at a flow rate of 0.25 mL/min,then separated on the second dimensional column of ZORBAX Eclipse Plus-C18（2.1 mm×150 mm,5 μm） using a methanol-water-trifluoroacetic acid mixture（90∶10∶0.01） as mobile phase at a flow rate of 0.25 mL/min,finally detected with a UV detector at 310 nm.The effects of sample solvent and sample volume on the enrichment were investigated.When the sample solvent was consistent with the first dimension mobile phase,the enrichment on 300 μL sample could be achieved.There existed good linear responses for 5 kinds of ginkgolic acids in the range of 0.200-100.0 mg/kg,with correlation coefficients greater than 0.998 and detection limits of 0.02-0.06 mg/kg.The recoveries at two spiked levels of 5 mg/kg and 10 mg/kg were between 94.0% and 101.3% with relative standard deviations not more than 5.0%.关键词：extract of Ginkgo biloba;ginkgolic acids;two-dimensional liquid chromatography;online enrichment;column switching
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发布时间： -
Determination of Aflatoxin B1 by Lateral Flow Assay Based on Molecule Beacon/Fluorescent Microsphere
摘要：A new method was proposed for the determination of aflatoxin B1（AFB1） by lateral flow assay based on molecule beacon（MB）/fluorescent microsphere（FM）.A MB containing AFB1 aptamer conjugated with FM,which was coated on the conjugate pad of a strip.A sequence containing adenine（A） was coated on the nitrocellulose membrane（NCM） at the test line,and another sequence complementing with AFB1 aptamer was coated on the control line.In the presence of AFB1,the specific combination of AFB1 and aptamer-FM led to the broken off of the double strand in MB.Then,the complex of AFB1/aptamer-FM was captured at the test line,and the excess MB/FM were captured at the control line.The fluorescence was observed with a fluorescence detector,and the content of AFB1 was estimated by the ratio of fluorescence peaks of the test line（T） and the control line（C）.The results showed that there existed a good linear relationship between the ratio of fluorescence peaks and AFB1 in the range of 0.1-50 μg/L with a limit of detection（S/N=3） approximately 0.05 μg/L.With a light signal “off-on” procedure,this proposed method could provide a new way for the accurate determination of AFB1.关键词：aflatoxin B1;molecule beacon（MB）;fluorescent microsphere（FM）;lateral flow assay;quantitative analysis- 711
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发布时间： - 摘要：A high performance liquid chromatography-quadrupole/electrostatic field Orbitrap high resolution mass spectrometry（HPLC-Q/Orbitrap HRMS） was developed for the determination of aflatoxins in feeds.The IMMUNOPREP- ONLINE AFLATOXIN（Part Code:P900） was used as an online solid phase extraction column,and DiamonsilPlus C18（150 mm×4.6 mm,5 μm） as an analytical column.The feed samples were dissolved with a certain amount of NaCl and acetonitrile-water（80∶20）.After ultrasonic extraction,the supernatant was injected into an online solid phase extraction column,then the target was transferred to the analysis column by valve switching technique and HPD confocal elution mode for separation.The external standard method was used for quantitation.The analysis was performed by MS under Full scanning mode in positive mode.Under the optimal conditions,the calibration curves were linear in the range of 0.5-50.0 μg/L for four aflatoxin,the limits of detection and quantitation were 0.2 μg/kg and 0.5 μg/kg,respectively.The average recoveries at three spiked levels（0.5,1.0,5.0 μg/kg） were in the range of 94.6%-114.3% with relative standard deviations（RSDs） not more than 8.3%.With the advantages of rapidness,high automation,high-throughput detection and low cost,the proposed method could be used in the rapid detection on aflatoxins in feed samples.关键词：aflatoxins;online solid phase extraction;high performance liquid chromatography-quadrupole/electrostatic field Orbitrap mass spectrometry（HPLC-Q/Orbitrap MS）;feed
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发布时间： - 摘要：A high performance liquid chromatography-tandem mass spectrometric(HPLC-MS/MS) method was established for the simultaneous determination of 4 kinds of optional components(choline,L-carnitine,taurine and inositol) in infant formula milk powder.After dissolution with warm water,the protein in sample was precipitated with zinc acetate and potassium ferrocyanide.The supernatant was separated on an HSS T3 column,then detected by MS/MS under MRM mode,and quantified by the internal and external standard methods.Under the optimized conditions,the calibration curves were linear in the ranges of 0.01-2.0 mg/L for choline and L-carnitine,and 0.1-2.0 mg/L for taurine and inositol,with correlation coefficients larger than 0.997.The detection limits of the method were 1.5 mg/kg for choline and L-carnitine,and 15 mg/kg for taurine and inositol,respectively.The mean recoveries were in the range of 87.5%-102.4%with relative standard deviations(RSDs,n=6) of 3.0%-7.3%.The method,with the advantages of high sensitivity,good purification effect and quantitative accuracy,is applicable for the detection of choline,L-carnitine,taurine and inositol in infant formula milk powder.关键词：high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS);infant formula milk powder;choline;L-carnitine;taurine;inositol
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发布时间： - 摘要：A closed loop dynamic needle sampling method was developed for the determination of volatile components in cigarette tobacco by gas chromatography-mass spectrometry（GC-MS）.The collection mode,trapping and desorption conditions were optimized,and the desorption rate of dynamic needle trap（NT） was investigated,which was compared with that of solid phase microextraction（SPME）.The optimal conditions were as follows:a needle filled with Carboxen1000 material was used to trap the sample at a heating temperature of 80 ℃,with a velocity of 3 mL/min,a capturing time of 30 min,a desorption temperature of 250 ℃ and a desorption time of 5 min.Under the optimized conditions,45 compounds including tobacco organic acids,esters,aldehydes,alcohols etc.were detected,among which 27 species,accounting for 60% of total compounds,had the relative standard deviations less than 5%.The NT method,with better sensitivity and repeatability,is more suitable than solid phase microextraction method for the analysis of volatile components in cigarette tobacco.关键词：dynamic needle trap（NT）;solid phase microextraction（SPME）;gas chromatography-mass spectrometry（GC-MS）;tobacco products
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发布时间： - 摘要：A method was developed for the determination of hexabromocyclododecanes（HBCDs） in marine organisms by high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS） coupled with LC-Si SPE clean up.The samples were extracted with n-hexane,cleaned up by LC-Si SPE,and analyzed by LC-MS/MS.The major parameters affecting LC-Si SPE eluting conditions were also investigated.The chromatographic separation was performed on an ACQUITY UPLC BEH C18 column by gradient elution with water and methanol-acetonitrile solution（methanol∶acetonitrile=4∶6） as mobile phase.The detection of analyte was carried out by electrospray mass spectrometry in negative ionization under multiple reaction monitoring mode,and the internal standard method was used for quantification.There existed good linear relationships for HBCDs in the range of 0.50-100.0 μg/L with correlation coefficients（r2） more than 0.995.The quantitation limits of the method were 0.20 μg/kg.The recoveries for HBCDs were in the range of 85.6%-97.3%,with relative standard deviations of 3.9%-8.8%.Therefore,the method could be applied in the identification and quantitation of HBCDs in marine organisms with low matrix interference and good reproducibility.关键词：solid phase extraction(SPE);UPLC-MS/MS;marine organisms;hexabromocyclododecanes（HBCDs）
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发布时间： - 摘要：A gas chromatography-mass spectrometric(GC-MS) method was developed for the determination of 16 organotin compounds in textile materials and their products.Samples were ultrasonically extracted with a mixture of methanol and sodium acetate,then the extract was derived with sodium tetraethyl borate,and extracted with n-hexane.The target ingredients were separated on a DB-5MS(30 m×0.25 mm×0.25 μm) column.The 16 organotin compounds were analyzed in selective ion mode(SIM).Under the optimal conditions,the calibration curves for 16 organotin compounds were linear in the range of 50-500 μg/L,with limit of quantitation of 0.05 mg/L(0.15 mg/kg).The recoveries ranged from 77.6%to 106.0%,with relative standard deviations(RSDs,n=6) not more than 8.3%.This method was rapid,reliable,accurate and convenient to operate,and it was appropriate for the determination of organotin compounds in textile materials and their products in routine tests.关键词：textile;organotin;gas chromatography-mass spectrometry(GC-MS);ultrasonic extraction
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发布时间： - 摘要：Carbon quantum dots（CDs） with green fluorescence were synthesized by nitric acid oxidation and hydrothermal method with Taixi coal as carbon source.The CDs had good stability and water dispersibility with an average diameter of 3.64 nm.The structures and optical properties of the CDs were characterized by transmission electron microscopy（TEM）,X-ray photoelectron spectroscopy（XPS）,Fourier transform infrared spectroscopy（FTIR）,UV-Vis spectroscopy and fluorescence spectroscopy.Based on the fluorescence quenching principle,the fluorescence intensity of CDs decreased with the increase of Fe3+ concentration under the optimal detection conditions.The fluorescence quenching efficiency of CDs was in good linearity with Fe3+ in the concentration ranges of 0.6×10-6-2.5×10-6 mol/L and 3.0×10-6-21.0×10-6 mol/L,and the detection limit for Fe3+ was 6.7×10-7 mol/L.关键词：carbon quantum dots（CDs）;Taixi coal;fluorescence quenching;Fe3+
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发布时间： - 摘要：A method was developed for the determination of fumonisin B1，fumonisin B2 and fumonisin B3 in feeds by high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）.The samples were extracted with acetonitrile-water-formic acid（50∶49∶1,by volume）,and cleaned up with a PRIME HLB solid phase extraction column.The analytes were separated on an Agilent Zorbax SB-C18 column（150 mm×2.1 mm,3.5 μm） and gradiently eluted with acetonitrile and 5 mmol/L ammonium acetate solution containing 0.1% formic acid as mobile phases.The target compounds were detected with electrospray ionization（ESI） in positive mode under multiple reaction monitoring mode,and quantified by the external standard method with matrix correction standard curves.The results indicated that the linear ranges for 3 compounds ranged from 5.0 μg/L to 250.0 μg/L with correlation coefficients（r2） more than 0.995.The limits of detection（LODs） and quantitation（LOQs） were 3 μg/kg and 10 μg/kg，respectively.The average recoveries at three spiked levels of 10，20 and 50 μg/kg were in the range of 80.3%-93.7%,with relative standard deviations（RSDs） of 7.5%-13.4%.The method is simple,rapid and stable,and could be used for the detection of fumonisins in feeds.关键词：high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）;solid phase extraction（SPE）;fumonisins;feeds
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发布时间： - 摘要：The microstructure and composition of ethylene and methyl methacrylate copolymer（EMMA-a）,obtained with bis ［N-（2,6-diisopropylphenyl）-3-isopropylsalicylaldiminate］ nickel（Ⅱ）/methylaluminoxane（MAO）,were fully characterized by 1H NMR and 13C NMR techniques.The copolymer（EMMA-b） of ethylene and methyl methacrylate,produced by radical polymerization,also experienced the corresponding characterization.According to the 1H NMR data,the corporations of the co-unit MMA in the two copolymers were calculated to be 14.10% and 10.26%,respectively.Based on the 13C NMR data,the microstructures of the two copolymers were compared.The results showed that in the ethylene co-units,methyl type branches mainly appeared in the EMMA-a,while long-chain branches were found in the EMMA-b.Besides,in the MMA co-units,the chemical shift of carbon in carbonyl（C‖O） of EMMA-a was found as 177.27,while the chemical shift of carbon in carbonyl（C‖O） of EMMA-b was 175.96.关键词：nuclear magnetic resonance（NMR）;ethylene and methyl methacrylate copolymer（EMMA）;microstructures;characterization
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发布时间： - 摘要：A fluorescent method was developed for the quantitative analysis of iodine by synthesizing BSA-protected AuNCs（AuNCs@BSA） as fluorescent probe.Under the optimum conditions,the decrease of the fluorescent intensity of AuNCs@BSA had a good linear relationship with iodine concentration in the range of 2.0 nmol/L-35 μmol/L,and the detection limit for iodine was 1.8 nmol/L.The proposed method was used to detect iodine in water,and the results were consistent with those obtained by ICP-MS method,which indicated that this method was a rapid and reliable technique for detection of iodine in real samples.The quenching mechanism of iodine with AuNCs@BSA was studied by the modified Stern-Volmer equation and thermodynamic calculation,and CD and IR results revealed that the secondary-structure change of the capping ligand BSA played an important role in the fluorecent quenching of AuNCs@BSA.In conclusion,the accurate and full data would make a significant contribution to understanding of the action mechanism and relationship between inorganic small molecules and protein protected metal nanoclusters.关键词：gold nanoclusters;fluorescent probe;quenching mechanism;thermodynamic calculation;iodine
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发布时间： - 摘要：A high field asymmetrical waveform ion migration spectrometric(FAIMS) method was developed for the determination of benzene in water.The benzene standard spectra in different dispersion voltages(DV) were studied,and the second-order α2 and the fourth-order α4 coefficients of non-linear function for benzene identification were calculated to be -3.8×10-5 Td-2 and 5.1×10-8 Td-4,respectively.The optimum dispersion voltage for benzene identification was obtained to be 800 V by balancing the sensitivity and resolution.The detection limit of FAIMS for benzene in water,through the relationship between benzene signal intensity and different benzene concentrations(0.08-0.64 mg/L),was determined to be 0.89 μg/L,which was far superior to the national concentration limit(10 μg/L) for benzene in drinking water.This study provides a rapid and sensitive method for the detection of benzene in water.关键词：high field asymmetrical waveform ion migration spectrometry(FAIMS);field detection;benzene;water
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发布时间： - 摘要：A method based on UV absorption spectroscopy with polyethylenimine（PEI） solution was proposed for the rapid and accurate detection of H2S gas in oil and gas fields.The amino groups in PEI reacted with H2S gas while it was bubbled into PEI solution，which could be utilized in the detection of H2S concentration.The UV absorption spectra of PEI solution were measured before and after bubbling H2S gas，and the absorbance near absorption line 230 nm and 365 nm of UV absorption spectra was analyzed.H2S gas samples with standard concentration were prepared for concentration calibration tests，and the relationship between gas concentration and UV absorbance was studied.The experimental results showed that a good linear relationship between H2S gas concentration and UV absorbance of PEI solution was obtained，with a correlation coefficient（r2） of 0.970 6.Meanwhile，the limit of detection for H2S gas reached to 15.39 mg/m3.UV absorbance analysis on PEI solution could be used for the rapid determination of H2S gas in oil and gas fields.关键词：polyethylenimine;ultraviolet absorption spectrum;hydrogen sulfide;organic polymer;accurate measurement
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发布时间： - 摘要：A method was developed for the determination of hydroxylamine residues in candesartan cilexetil drugs by ion chromatography with electrochemical detection.After dissolved with dichlomethane,extracted with 30 mmol/L methanesulfonic acid solution and filtrated on an OnGuard Ⅱ RP column,the samples were injected into the instrument.The separation was performed on an Ionpac CS16（250 mm×5 mm） column using 30 mmol/L methanesulfonic acid as eluting solution at a flow rate of 1.0 mL/min.Then,a 300 mmol/L sodium hydroxide solution was added into the instrument at a flow rate of 0.3 mL/min.An integrated pulsed electrochemical detector was used for the detection,in which the electrode material is made of gold,the reference electrode is pH-Ag/AgCl composite electrode,the potential waveform is composed of six potentials of amino acid,the column temperature is 40 ℃,and the injection volume is 25 μL.The calibration curve for hydroxylamine showed a good linearity（r=0.999） in the range of 0.014 47-0.289 4 mg/L,with a limit of detection（LOD,S/N=3） of 0.007 24 mg/L and a limit of quantitation（LOQ,S/N=10） of 0.014 47 mg/L.There was a good resolution between hydroxylamine and ammonium ion.With the advantages of simple operation,high sensitivity and good reproducibility,the method could be used for the detection of hydroxylamine residues in candesartan cilexetil drugs.关键词：ion chromatography with electrochemical detection;candesartan cilexetil;hydroxylamine
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