最新刊期

    33 5 2014
    • Vol. 33, Issue 5, Pages: 489-498(2014)
      摘要:A fast and easy method for the screening and quantification of 111 pesticides residues in wines by liquid chromatography-Quadrupole/Orbitrap high-resolution mass spectrometry was developed.The wine samples were extracted with acetonitrile (containing 0.1% acetic acid),and salted out with anhydrous magnesium sulphate and anhydrous sodium acetate.After concentration,the analyte was dissolved with methanol and water,then cleaned up with primary secondary amine (PSA) to reduce matrix interference.Chromatographic analysis was carried out using a C18 column with acetonitrile-5 mmol/L ammonium acetate solution as mobile phase by gradient elution.111 pesticides residues were analyzed by high-resolution mass spectrometry in positive mode.Accurate mass extraction of the target pesticide compounds and data dependence threshold-triggered MS/MS minimized the matrices interference during the analysis.The linearities of all 111 pesticides ranged from 1 μg/L to 100 μg/L with correlation coefficients greater than 0.99.By detecting spiked samples,the limits of detection of the method were 5 μg/kg for all the pesticides residues and the recoveries were in the range of 63.3%-123.7% with RSDs of 3.2%-18.8%.This method could be used for high-throughput screening and confirmation of multiple pesticide residues in wines.  
      关键词:high performance liquid chromatography;orbitrap;high-resolution mass spectrometry;pesticide residues;wine;high-throughput   
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    • Vol. 33, Issue 5, Pages: 499-505(2014)
      摘要:A high sensitivity and throughput method was developed for the simultaneous determination of 167 pesticide residues in soybean by liquid chromatography-electrospray tandem mass spectrometry(LC-MS/MS).Sample was soaked with water and extracted with acetonitrile,followed by salting out with anhydrous MgSO4,NaCl,Na3Citrate dihydrate and Na2HCitrat sesquihydrate mixture.The extract was added to C18 and PSA solid phase extraction columns,and eluted with 2% formic acid methanol solution.The eluent was concentrated to a constant volume and separated on an Atlantis C18 column(100 mm×2.1 mm,3 μm) .The analyte was analyzed by HPLC-MS/MS with a positive and negative ions switching mechanism under multiple reaction monitoring mode.The results were quantified with matrix-matched standard solutions as the external standard.The average recoveries of the pesticides at three spiked concentration levels of 0.01,0.02,0.05 mg/kg were in the range of 67.3%-123.5%,with RSDs of 4.7%-13.9%.All the pesticides in matrix-matched standard solutions were linear in the range of 0-50.0 μg/L with correlation coefficients more than 0.99.The limits of quantitation(S/N>10) for all pesticides were 0.01 mg/kg.The proposed method was suitable for the screening of multi-pesticide residues in soybean for its high sample throughput,low LOQ,good accuracy and precision.  
      关键词:liquid chromatography-electrospray tandem mass spectrometry(LC-MS/MS);soybean;multi-pesticide residues;high-throughput   
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    • Vol. 33, Issue 5, Pages: 506-511(2014)
      摘要:A total of 84 Perilla frutescens(L.) Britt.samples from three main geographical origins in China were collected and investigated by using high performance liquid chromatography(HPLC) incorporated with chemometrics method.Prior to investigation,the measured liquid chromatographic data were subjected to pretreatments,including baseline correction and retention time alignment.Principal component analysis(PCA) was then applied in the aligned and compressed data sets,respectively,to evaluate the data quality,and three sample groups were observed in the PCA score plots.Moreover,partial least squares-discriminant analysis (PLS-DA) was applied to classify these herbal samples,providing better abilities of recognition(92.8%) and prediction(89.6%).  
      关键词:Perilla frutescens(L.) Britt.;HPLC;fingerprints;chemometrics;discrimination   
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    • Vol. 33, Issue 5, Pages: 512-519(2014)
      摘要:A poly(2-oxygen amino methyl-2-(2-amino thiazole)-4-acetic acid(PAMTA)modified glassy carbon electrode(PAMTA/GCE) was fabricated by CV method.In 0.1 mol/L pH 7.0 PBS buffer,PAMTA/GCE not only improved the oxidations of DA,UA and NO-2,but also resolved the weak and overlapped voltammetric responses of DA,UA and NO-2 into three sensitive oxidation peaks.Thus,the modified electrode can be used for the simultaneous determination of these species.Under the optimum conditions,the linear concentration dependences of DPV current responses were observed for DA,UA and NO-2 in the concentration ranges of 0.3-75 μmol/L,1-480 μmol/L and 20-1 680 μmol/L,with correlation coefficients of 0.989 9,0.957 1 and 0.992 7,respectively.The detection-limits(3δ) were 0.05,0.10,0.30 μmol/L for DA,UA and NO-2,respectively.The modified electrode was used for simultaneous determination of DA,UA and NO-2 in human urine and serum samples with satisfactory results.  
      关键词:dopamine;uric acid;nitrite;2-oxygen amino methyl-2-(2-amino thiazole)-4-acetic acid   
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    • Vol. 33, Issue 5, Pages: 520-526(2014)
      摘要:The application of near infrared spectrum technology in rapid detection of Monascus biomass in solid-state fermentation was studied in this paper. Four batches of 80 samples′s spectra were collected,and glucosamine method was used to estimate the biomass. In order to reduce the complexity of the model and improve the prediction performance, the application of the genetic algorithm (GA) to selected wavelenths region was studied,and partial least squares regression was constructed for the prediction of biomass value in solid state fermentation of Monascus with effective wavelengths selected by GA. To illustrate the feasibility of GA to optimize spectral variables,partial least squares regression (PLSR) was constructed with full-spectrum and the wavelengths were selected by the correlation coefficient method,respectively. The prediction ability of the three models were comparatively analyzed,and the correlation between the spectral bands information selected by GA algorithm and the corresponding absorption generated by hydrogen groups of bacteria′s composition was explained. The results showed that GA could reduce the complexity of the model and improve the model′s prediction performance,with Rc=0.998 3,RMSECV=3.580 2,Rp=0.993 1,RMSEP=3.643 7,data points participate in modeling decreasing from the original 1 457 to 585,and the model predict-tion accuracy is improved by 11.55% compared with that of the full spectrum′s PLS model. The result showed that the PLS model built by using near infrared spectroscopy combined with GA could realize the rapid detection of biomass of Monascus in solid state fermentation. The method provided the technical foundation to further realize online fermentation process optimization control.  
      关键词:NIR;genetic algorithm(GA);Monascus;solid-state fermentation;biomass   
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    • Vol. 33, Issue 5, Pages: 527-532(2014)
      摘要:A solid phase extraction combined with ultra performance liquid chromatography-tandem mass spectrometric(SPE/UPLC-MS/MS) method was developed for the simultaneous determination of 12 synthetic colorants,including Acid Violet 49,Pigment Red 57,Pigment Red 53∶1,Acid Yellow 36,Rhodamine B,Basic Violet 3,Disperse Yellow 3,Pigment Orange 5,Sudan Ⅰ,Sudan Ⅱ,Sudan Ⅳ,Solvent Blue 35,in lip gloss,eye shadow,lipstick and other cosmetics.The cosmetics were extracted sequentially by ultrasonic technique with tetrahydrofuran(THF),dimethyl sulfoxide(DMSO) and methanol,cleaned up with HLB solid phase extraction column.The separation was performed on an Acquity UPLC BEH-C18(2.1 mm×50 mm,1.7 μm) column by gradient elution using acetonitrile-0.05% formic acid as mobile phase,then the isolates were analyzed under multiple reaction monitoring(MRM) mode,and quantified by the matrix matched external standard method.The results showed that the 12 investigated colorants displayed good peak shapes within 6 min.The calibration curves of 12 colorants were linear in the range of 0.5-800 μg?L-1,with correlation coefficients more than 0.99.The limits of quantitation(LOQ,S/N>10) were in the range of 1.4-2 000 μg?kg-1.The recoveries of 12 colorants in spiked lip gloss,eye shadow and lipstick samples ranged from 60.8% to 118.0% with relative standard deviations(RSD) of 2.3%-10.8%.The method was rapid,simple and sensitive,and was suitable for the determination and confirmation of the colorants in oil cosmetics,cream cosmetics and powder cosmetics.  
      关键词:SPE;UPLC-MS/MS;colorants;cosmetic   
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    • Vol. 33, Issue 5, Pages: 533-538(2014)
      摘要:A reversed-phase high performance liquid chromatographic method was developed for the determination of six aromatic carboxylic acids including p-amino benzoic acid,phthalic acid,p-hydroxy benzoic acid,salicylate acid,benzoic acid and o-methyl benzoic acid,by using ionic liquids as mobile phase additives.The chromatographic separation of aromatic carboxylic acids was performed on a RP-C18 column.The detection of aromatic carboxylic acids was carried out by ultraviolet(UV) detection.The comparison of three different mobile phases was performed.When the ionic liquids were chosen as mobile phase additives,the chromatogram was improved with better chromatographic peak shape and higher sensitivity.Effects of experimental conditions,e.g.detection wavelength,methanol content,pH value,concentrations and alkyl chain length of ionic liquids on separation and determination of aromatic carboxylic acids were investigated.The optimum chromatographic conditions were as follows:mobile phase:methanol-1.0 mmol/L 1-butyl-3-methylimidazolium tetrafluoroborate aqueous solution(pH 3.0)(40∶60),UV detection wavelength:240 nm,flow rate:1.0 mL/min,column temperature:30 ℃.The six aromatic carboxylic acids were successfully separated within 16.5 min under the optimal conditions.The calibration curves showed good linearities over the range of 5-120 mg/L for aromatic carboxylic acids with correlation coefficients more than 0.999.The average recoveries of spiked components were in the range of 98.3%-103.8%,with relative standard deviations not more than 0.63%.The method was successfully used to determine the content of aromatic carboxylic acids in pharmaceuticals,Compound Redbud Bark and Salicylic Acid solution and the Zujunqing Tinctura.  
      关键词:ionic liquid;high performance liquid chromatography(HPLC);aromatic carboxylic acids;ultraviolet detection;pharmaceutical   
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    • Vol. 33, Issue 5, Pages: 539-544(2014)
      摘要:A gas chromatography-mass spectrometric(GC-MS) method was established for the simultaneous determination of 42 semivolatile organic compounds,including polycyclic aromatic hydrocarbons(PAHs),polychlorinated biphenyls(PCBs),organochlorine pesticides(OCPs) and organophosphorus pesticides(OPPs)in groundwater.The preparation and analytical conditions,such as solid phase extraction(SPE),liquid-liquid extraction(LLE),extraction solvent and chromatographic column,were optimized.The 42 pollutants in groundwater were extracted by liquid-liquid extraction with ethyl acetate-hexane(1∶4),then determined by gas chromatography-mass spectrometry under selected ion monitoring(GC-MS/SIM) mode.Isotope labled acenaphthene-d10,phenanthrene-d10,chrysene-d12 and perylene-d12 were used as the internal standard for the quantitation analysis.Under the proposed conditions,the calibration curves of the compounds were linear in the range of 0.5-1 000 μg/L with correlation coefficients higher than 0.995.The method detection limits(MDL) were in the range of 0.05-3.08 ng/L.The accuracy and precision of the method were determined by analyzing water samples spiked with three concentration levels of 10,40,400 ng/L target compounds.The recoveries were in the range of 73.0%-107%,with RSDs(n=5) of 1.4%-11.3%.The method is sensitive,accurate and simple,which could significantly improve the efficiency in the analysis of main organic pollutants in groundwater.The method was successfully applied in the analysis of trace organic contaminants in groundwater samples collected from the surrounding area of Shijiazhuang,China.  
      关键词:gas chromatography-mass spectrometry(GC-MS);groundwater;polycyclic aromatic hydrocarbons(PAHs);polychlorinated biphenyls(PCBs);organochlorine pesticides(OCPs);organophosphorus pesticides(OPPs)   
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    • Vol. 33, Issue 5, Pages: 545-550(2014)
      摘要:A new method for the determination of 9 organic acids in tobacco was developed by derivatization,solid phase extraction and gas chromatography(GC).The tobacco samples were methylated with methanol and sulfuric acid.The organic acid ester was firstly extracted using solid-phase extraction in strong acidic medium,and then enriched with MCI-GEL and eluted with methanol.The eluent was determined by GC with a DB 5 capillary column and a splitless injection volume of 1.0 μL at a detector temperature of 250 ℃.This method was applied in the determination of lactic acid,oxalic acid,propandioic acid,acetylpropionic acid,malic acid,citric acid,palmic acid,linoleic acid and stearic acid in tobacco samples.The recoveries were in the range of 92.2%-102.6% with relative standard deviations(RSD) of 2.4%-3.2%.The limits of quantitation(LOQ) for all analytes were between 0.20 mg/L and 0.36 mg/L.The method was accurate and sensitive,and could meet the actual requirements for the analysis of tobacco samples.  
      关键词:solid phase extraction;enrichment;gas chromatography(GC);tobacco;organic acids   
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    • Vol. 33, Issue 5, Pages: 551-556(2014)
      摘要:A new method for rapid determination of pesticide was developed.Each of the optical sensors utilized in the liquid arrays was comprised of 7 dyes and gold nanoparticle to yield a different response to each pesticide sample.The experimental data were recorded by a 96-well plate reader and analyzed by principal component analysis(PCA),hierarchical clustering analysis(HCA)and linear discriminant analysis(LDA).The experimental results of PCA showed that the first three principal components reflect 92.69% of the total information and exhibit good recognition capabilities for 5 pesticides.HCA results showed that the classification for 25 samples was correct.LDA suggested that the classification accuracy was 100%.These results demonstrated that the developed visual liquid array system could offer an excellent sensing platform for the identification of pesticide samples,and has an application potential in the detection of pesticide residue.  
      关键词:pesticide;visual liquid array;dye;nano gold   
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    • Vol. 33, Issue 5, Pages: 557-560(2014)
      摘要:A novel method for the determination of methimazole was proposed,based on its enhancement effect on the luminol-silver nitrate-gold nanoparticles(AuNPs) chemiluminescence(CL) system in alkaline medium.The experimental conditions were studied.Under the optimal experimental conditions,methimazole could be detected in 3 sectional linear ranges of 1.0×10-9-1.0×10-8,1.0×10-8-1.0×10-7,1.0×10-7-1.0×10-6 g/mL with a detection limit of 3.0×10-10g/mL,and relative standard deviation was 1.2%(n=11,ρ=1.0×10-8 g/mL).The method was successfully applied in the determination of methimazole in pharmaceutical formulations.In addition,the mechanism of gold nanoparticles-luminol-AgNO3 system was also explored by the CL spectrum.  
      关键词:methimazole;chemiluminescence;gold nanoparticles   
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    • Vol. 33, Issue 5, Pages: 561-565(2014)
      摘要:A novel microfluidic chip system with simplified amperometric detector was manufactured and used to determine nicotinamide in commercially available nicotinamide tablets.The integrated two electrode in the simplified amperometric detector was comprised of a carbon-nanotubes electrode and a titanium tube.The carbon-nanotubes electrode in the middle of the electrode was used as the working electrode,and the titanium tube was used not only as a counter electrode of amperometric detection but also as the ground electrode of power source in separation.The structure of microfluidic chip system was more simplified and miniaturized.The experimental conditions,such as type and concentration of buffer solution,separation voltage and injection time etc,were optimized.The results showed that nicotinamide was separated and detected within 2 min in the buffer of 10 mmol?L-1 phosphate solution(pH 7.8) at a separation voltage of 2.0 kV and an injection time of 10 s.The calibration curve of nicotinamide was linear in the range of 10-600 μmol?L-1.The limit of detection(LOD,S/N=3) reached to 5 μmol?L-1 and the relative standard deviation(RSD) was 3.0% for nicotinamide.The average spiked recovery was 99.1%.This device has realized miniaturization and integration with high sensitivity,good selectivity and low cost,and could be used for the quality control of medicines.  
      关键词:microfluidic chip;simplified amperometric detector;integrated two-electrode;nicotinamide   
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    • Vol. 33, Issue 5, Pages: 566-571(2014)
      摘要:A new symmetrical 1,3-dihexylimidazolium bis[(trifluoromethyl)sulfonyl]imide([HHIM][Tf2N]) was synthesized and characterized,and was for the first time employed as extraction solvent in dispersive liquid-liquid microextraction(DLLME) for enrichment and determination of four polycyclic aromatic hydrocarbons(PAHs) including chloronaphthalene,fluorene,anthracene and chrysene in environmental water sample by high-performance liquid chromatography(HPLC).The extraction conditions influencing extraction efficiency,such as kind of extraction and disperser solvent,volume of extraction and disperser solvent,salt concentration,extraction and centrifugal time were investigated in detailed.Under the optimal conditions,the proposed method provided good linearities for all analytes with correlation coefficients(r2) of 0.999 0- 0.999 8.The relative standard deviations(RSDs,n=5) for four analytes varied between 1.5% and 5.0%.The limits of detection for the method(S/N=3) ranged from 0.002 5 μg?L-1 to 1.0 μg?L-1 and the enrichment factors were in the range of 183-372.This developed method was convenient,speedy,highly sensitive,environment friendly,and was successfully applied in the detection of 4 real water samples(e.g.tap water,ground water,rain water and river water) with recoveries of 84.7%-115.2% and RSDs of 1.6%-6.4%.  
      关键词:1,3-dihexylimidazolium bis[(trifluoromethyl)sulfonyl]imide ionic liquid;dispersive liquid-liquid microextraction;high-performance liquid chromatography(HPLC);polycyclic aromatic hydrocarbons   
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    • Vol. 33, Issue 5, Pages: 572-577(2014)
      摘要:A MWCNTs loading cobalt-iron mixed oxide modified electrode was fabricated by using cyclic voltammetry.The electrocatalytic activity of the modified electrode for the oxidation of glucose was investigated by cyclic voltammetry and amperometric method.The results showed that the modified electrode exhibited a high electrocatalytic activity for the oxidation of glucose.Based on this,an amperometric method for the determination of glucose was established.Under the optimum conditions,the oxidation peak current had linear relationships with concentrations of glucose over the ranges of 2.0×10-7-4.2×10-5 mol?L-1 and 4.2×10-5-4.9×10-4 mol?L-1,with sensitivities of 242.7 μA?(mmol?L-1)-1 and 114.8 μA?(mmol?L-1)-1,respectively.The detection limit(3sb) was 5.0×10-8 mol?L-1.The proposed method was successfully applied in the detection of glucose in serum.  
      关键词:cobalt-iron mixed oxide;multi-wall carbon nanotubes;glucose;electrocatalytic oxidation   
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    • Vol. 33, Issue 5, Pages: 578-582(2014)
      摘要:A method was developed for the determination of sulfur dioxide in chrysanthemum by ion chromatography(IC).The crushed sample was extracted with alkaline solution by accelerated solvent extraction(ASE),and purified with C18 solid phase extraction(SPE)cartridge.The analyte was separated with IonPac AS9-HC ion chromatographic column using carbonate as eluent and detected with conductivity detector.A good linear relationship(r2=0.999 7) was obtained in the range of 0.5-50 mg?L-1 with a limit of detection(LOD)of 0.05 mg?L-1 and a limit of quantitation(LOQ)of 0.17 mg?L-1.The method was validated at three different spiked levels,and the average recoveries were in the range of 82.9% - 92.6% with relative standard deviations(RSDs,n=6) less than 5.0%.The results indicated that the method had a high degree of automation and efficiency of extraction,and was suitable for rapid and accurate analysis of sulfur dioxide residue in chrysanthemum samples in batch.  
      关键词:sulfur dioxide;chrysanthemum;alkaline solution;accelerated solvent extraction(ASE);ion chromatography(IC)   
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    • Vol. 33, Issue 5, Pages: 583-587(2014)
      摘要:The structure of fullerenols was directly characterized by combining detection of positive and negative ion mode of laser desorption ionization time-of-flight mass spectrometry.Compared to that of the fullerene,the carbon cage of fullerenol was found to more easily show regular fragmentation peaks in the positive ion mode.However,in the negative ion mode,both fullerene and fullerenol retain the characteristic peaks of carbon cage.This method can be used for the identification and selection of the alkali reaction condition for the synthesis of fullerenols,and the optimal reaction alkali concentration of 1.0 g/mL was obtained.At the same time,this method was also approved that fullereols could be stable in the solvent of DMSO.  
      关键词:fullerenols;laser desorption ionization;time-of-flight mass spectrometry   
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    • Vol. 33, Issue 5, Pages: 588-593(2014)
      摘要:A simple,rapid,sensitive and cheap high performance liquid chromatography-tandem quadrupole mass spectrometric(HPLC-MS/MS) method was developed for the determination of tetrodotoxin(TTX)that is one of the most toxic non protein small biotoxin in Fugu rubripes muscle.The analytes were ultrasonically extracted from homogeneous fugu muscle samples with 1% acetic acid methanol solution at 50 ℃,purified by freezing high speed centrifugation,and succeeded cleaned by QuEChERS(Quick,Easy,Cheap,Effective,Rugged and Safe) method using a mixture of Cleanert PestiCarb and C18 as sorbent.The analyte was determined by HPLC-MS/MS using acetonitrile and 0.15% acetic acid(containing 10 mmol/L ammonium acetate)as mobile phase by gradient elution.The quantitation of TTX was performed using matrix-matched calibration curve by the external standard method.Recoveries of TTX at spiked levels of 30,50,100 μg/kg were between 74.0% and 105.0% with relative standard deviations(RSD,n=6) not more than 11.0%.The limit of detection and limit of quantitation were 10 μg/kg and 30 μg/kg,respectively.With the advantages of good accuracy,repeatability,sensitivity,simplicity,economy and environment friendiness,this method could meet the requirements of practical analysis of TTX in fugu flesh samples.  
      关键词:tetrodotoxin(TTX);Fugu rubripes flesh;QuEChERS;high performance liquid chromatograph-tandem quadrupole mass spectrometry(HPLC-MS/MS);quick extraction   
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    • Vol. 33, Issue 5, Pages: 594-597(2014)
      摘要:A new method was established for the separation and enrichment of niclosamide in environmental water by cloud point extraction coupled with high performance liquid chromatography(HPLC).With Triton X-114 as solvent,some factors affecting the cloud point extraction,such as surfactant concentration,pH value of sample solution,equilibration time and equilibration temperature on extraction efficiencies were studied and optimized.In the conditions of adding 3% Triton X-114 at pH 3.5,an equilibrium temperature of 45 ℃,an equilibrium time of 30 min and sodium chloride amount of 200 mg,the average recoveries were in the range of 95.6%-97.5%,and the limit of detection was 0.021 2 mg/L.With the advantages of high efficiency,environment friendliness and low cost,the method is suitalbe for the determination of drug residue in water samples of environment.  
      关键词:cloud point extraction;niclosamide;high performance liquid chromatography   
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    • Vol. 33, Issue 5, Pages: 598-601(2014)
      摘要:A rapid and sensitive analytical method for the determination of thifluzamide residues in rice,corn and potato samples was established based on QuEChERS(Quick,Easy,Cheap,Effective,Rugged and Safe) and ultra performance liquid chromatography coupled with tandem mass spectrometry(UPLC-MS/MS).The sample was extracted with acetonitrile,and then purified with primary secondary amine(PSA).The mass spectrometer was operated with electrospray in the negative ion mode(ESI-).The thifluzamide residues were quantified by the external standard method using the matched standard solution to compensate for matrix effect.Under the optimal conditions,the calibration curve showed a good linearity in the range of 1.0-1 000 μg?L-1 with a correlation coefficient of 0.999 0.The average recoveries of thifluzamide in rice,corn and potato at three spiked levels of 0.01,0.1,1.0 mg?kg-1 ranged from 89.1% to 109.3% with relative standard deviations(RSDs,n=5) of 3.5%-8.7%.The limits of detection(LODs) of thifluzamide were in the range of 0.009-0.015 μg?kg-1,and the limits of quantitation(LOQs) were 0.032-0.049 μg?kg-1.The method is simple,rapid and accurate,and could be adapted for the confirmation of thifluzamide residues in rice,corn and potato samples.  
      关键词:thifluzamide;UPLC-MS/MS;rice;corn;potato   
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    • Vol. 33, Issue 5, Pages: 602-605(2014)
      摘要:A liquid chromatography-tandem mass spectrometric(LC-MS/MS)method was developed for the determination of gossypol in feed.The sample was extracted with acetone-water(7∶3).The compound was separated on a C18 column(100 mm×2.1 mm,3.5 μm)with acetonitrile – 0.1% formic acid as mobile phase by gradient elution.The detection of gossypol was carried out by LC-MS/MS with positive electrospray ionization under the multiple reaction monitoring mode and quantified the external standard method.The limits of quantitation(S/N>10)was 1 mg/kg.Under the optimal conditions,the calibration curve was linear in the range of 10-100 μg/L with correlation coefficient of 0.993.The recoveries of gossypol at the spiked levels of 1,20,40 mg/kg in feed ranged from 83.8% to 97.5% with relative standard deviations(RSDs)of 1.3%-5.2%.With the advantages of easy operation,higher recoveries and good precision,the method was suitable for the confirmation and quantification of gossypol residue in feed.  
      关键词:feed;gossypol;liquid chromatography-tandem mass spectrometry(LC-MS/MS)   
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    • Vol. 33, Issue 5, Pages: 606-614(2014)
      摘要:Dispersive liquid-liquid microextraction(DLLME) is novel microextraction technique with a great potential in sample pretreatment,which has been increasingly used for preconcentration of diverse analytes.DLLME enjoys the advantages of simplicity,rapidity,low cost,high recovery and enrichment factor,and environmental benignity.Recently,as a viable sample-preparation approach,DLLME has been receiving rising concerns and achieving wide applications.In this paper,the research progress and applications of DLLME in preconcentration and separation of pollutants in different media are reviewed.  
      关键词:dispersive liquid-liquid microextraction;research progress;pollutants analysis;review   
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    • Vol. 33, Issue 5, Pages: 615-620(2014)
      摘要:Chirality is the intrinsic attribute of the nature.It is of great importance to develop new,rapid,efficient and sensitive chiral separation and analysis methods for enantioselective synthesis,chiral drugs pharmacological research,enantiomeric purity analysis and environmental monitoring.Metal nanoparticles can be used as ideal supporting materials for chiral chromatography due to their large surface area,good stability and easy post-functionalization.Furthermore,some kinds of metal nanoparticles own unique properties for surface plasmon resonance resulting from the collective oscillations of conduction band electrons,fluorescence and catalysis,so the practical applications and theoretical studies of metal nanoparticles in the area of chiral sensors are going deep.In this review,the recent applications of different metal nanoparticles (gold nanoparticles,silver nanoparticles,quantum dots,magnetic nanoparticles,etc.) in chiral separation and recognition are reviewed,and the future developments in this field are also prospected.  
      关键词:metal nanoparticles;chiral recognition;chiral separation;review   
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