最新刊期
卷 37 ， 期 7 ， 2018
- 摘要：A rapid method for the identification of constituents in Yangxinshi tablets was established by high performance liquid chromatography-time of flight mass spectrometry(HPLC-TOF/MS).Simultaneously,the quantitation on the sample was performed by high performance liquid chromatography-triple quadrupole mass spectrometry(HPLC-MS/MS).30 kinds of constituents in Yangxinshi tablets were identified by HPLC-TOF/MS in the running conditions as follows:chromatographic column:an Agilent ZORBAX Eclipse Plus C18 column(100 mm×30 mm,18 μm),mobile phase:acetonitrile-01% formic acid solution,elution type:gradient elution,flow rate:02 mL·min-1,column temperature:30 ℃,MS scanning mode:electrospray in both positive and negative ion.The HPLC-MS/MS method was operated under the following conditions:chromatographic column:a Waters XBridge BEH C18 column(150 mm×46 mm,25 μm),mobile phase:acetonitrile-01% formic acid solution,elution type:gradient elution,flow rate:04 mL·min-1,column temperature:30 ℃,MS scanning mode:multiple reaction monitoring(MRM) mode with electrospray ion source in both positive and negative ion.16 main constituents in Yangxinshi tablets were determined by HPLC-MS/MS.There were excellent linear responses for the peak areas of the analytes to their concentrations with the correlation coefficients(r) not less than 0997.The limits of detection(LODs) and quantitation(LOQs) for 16 constituents were in the range of 0039 1-781 μg/L and 0156-312 μg/L,respectively.The average recoveries were in the range of 968%-1038% with the relative standard deviations of 10%-35%.With the advantages of simple operation,accuracy and acceptable reproducibility,the developed method could be applied in the qualitation and quantitation of constituents in Yangxinshi tablets.Therefore,it could provide a reference for the quality control,further study and application of Yangxinshi tablets.关键词：Yangxinshi tablets;constituents;HPLC-TOF/MS;HPLC-MS/MS;quantitative analysis
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发布时间： - 摘要：To resolve the chromatographic column capacity of gas chromatography-mass spectrometry（GC-MS）,a GC-MS method with supercritical fluid chromatography（SFC） was developed for the determination of carbonyl compounds in mainstream cigarette smoke.The total particulate matter in mainstream cigarette smoke was collected with a Cambridge filter pad,and the carbonyl compounds were extracted with a supercritical fluid extractor,then the extract was separated and divided into 3 fractions by SFC method,and each fraction was analyzed by GC-MS.The results showed that the overlapping chromatographic peaks were avoided,and the chromatographic column capacity of GC-MS was improved.Therefore,the kinds of aldehydes and ketones aromatic components in mainstream cigarette smoke determined by the developed method were far more than that without SFC separation.Only 29 kinds of aldehydes and ketones compounds,including 7 kinds of aldehydes and 22 kinds of ketones,were identified without SFC separation,while 57 kinds of aldehydes and ketones compounds,including 13 kinds of aldehydes and 44 kinds of ketones,were determined using the developed method.There were great differences in the species and contents of aldehydes and ketones in mainstream smoke of three cigarettes.Each cigarette contained different specific aldehydes and ketones in mainstream cigarette smoke.This study provided a new method for the determination of aldehydes and ketones in cigarette mainstream smoke.关键词：supercritical fluid chromatography（SFC）;gas chromatography-mass spectrometry（GC-MS）;mainstream cigarette smoke;aromatic components;aldehydes and ketones compounds
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发布时间： - 摘要：A gas chromatography-mass spectrometry(GC-MS) with solid phase microextraction(SPME) was developed for the determination of 18 polycyclic aromatic hydrocarbons(PAHs) migrated from asphalt based waterproof coating.Influences of fibers species,extraction time,mixing speed and temperature on extraction efficiency were investigated.Under the optimized experimental conditions,good linearities were obtained for 18 PAHs in the range of 1-100 μg/L with their correlation coefficients(r) of 0992 8-0998 9 and the detection limits of 003-009 μg/L.The average recoveries at three spiked levels of 1,10,100 μg/L were in the range of 71%-94% with the relative standard deviations(RSD,n=6) of 28%-86%.The proposed method was applied in the migration analysis on five asphalt based waterproof coatings.Results showed that the PAHs in migratory fluid were detected,in which most were those with 4 rings below.The method is suitable for the determination of 18 PAHs migrated from asphalt based waterproof coating.关键词：solid phase microextraction(SPME);gas chromatography-mass spectrometry(GC-MS);polycyclic aromatic hydrocarbons(PAHs);asphalt based waterproof coating;migration
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发布时间： - 摘要：A novel variable selection method based on sampling error profile analysis frame and least angel regression（SEPA-LAR） was proposed in order to build a robust NIR model.Based on SEPA-LAR,more models were obtained by Monte Carlo sampling（MCS）,and the LAR regression coefficients at each wavelength were statistically analyzed,which were sorted by the sum sequence of their absolute values.Wavelengths containing larger sums of the absolute values of regression coefficients were selected,and a model with the wavelengths was built.Samples in the independent validation dataset were applied in the evaluation of the model.NIR datasets of corn moisture,diesel density and cheese fat were used to evaluate the performance of SEPA-LAR.Errors of root mean squared error of prediction（RMSEP） estimated with the validation dataset are 0001 44%（moisture）,0001 58 g/mL（density） and 113 g/100 g（fat content）,respectively.The results showed that,compared with Monte Carlo uninformative variable elimination（MCUVE）,moving window partial least squares regression（MWPLS） and competitive adaptive reweighted sampling（CARS）,SEPA-LAR could select less wavelengths and has smaller prediction error.The calibration model built by SEPA-LAR has good predictive ability,stability and interpretability.关键词：least angle regression;regression coefficient;Monte Carlo sampling;sampling error profile analysis;variable selection;near infrared spectroscopy
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发布时间： - 摘要：A relatively simple and fast phosphorescence method for the detection of baicalein（BAI） was established,based on that baicalein could quench the room temperature phosphorescence（RTP） of PEI-Mn/ZnS quantum dots（QDs） prepared by water phase coprecipitation through electron transfer effect.The experimental results showed that,at pH 80 and a reaction time of 10 min,the phosphorescence quenching degree of QDs had a linear relationship（r=0997） with BAI in the concentration range of 007-060 mg·L-1.The detection limits of the method were 0039 mg·L-1,and the relative standard deviations were 41%.The spiked recoveries for practical samples were in the range of 960%-1007%.The established method,effectively avoiding the interference of common ions and amino acids etc., could be used for the rapid determination of BAI in scutellaria baicalensis georgi and serum,which is expected to be applied in the determination and analysis of BAI in medicine industry.It also provides a technical basis for the detection of other drugs based on the mechanism of QDs electron transfer.关键词：quantum dots（QDs）;room temperature phosphorescence（RTP）;baicalein（BAI）;scutellaria baicalensis georgi;serum;sensor
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发布时间： - 摘要：A three phase hollow fiber membrane microextraction/ultrahigh performance liquid chromatography（HF-LPME/UPLC） was developed for the determination of eight amino acids in Escherichia coli..The three phase hollow fiber membrane micro extraction system was designed.The extraction conditions for HF-LPME were optimized as follows:the supported liquid membrane:n octanol,the concentration for NaOH in receiving phase:030 mol/L,the concentration for hydrochloric acid in sample solution:50 mmol/L,the concentration for NaCl:200 g/L,the extraction temperature:25 ℃,the stirring speed:500 r/min and the extraction time:4 hours.Eight kinds of amino acids were extracted after derivatization,and finally analyzed by UPLC.A baseline separation was achieved within 5 min.The calibration curves for the analytes were linear in range of 020-49×103 μmol/L with their correlation coefficients（r2） more than 0999,the enrichment factors of 110-290 and the detection limits of 00l/L.At a spiked concentration of 10 μmol/L,the recoveries for eight amino acids in Escherichia coli.were 887%-1031% with the relative standard deviations of 32%-43%（n=5）.The proposed method was highly sensitive and reproducible,and could be used for the detection of amino acids in bacteria.关键词：Escherichia coli.;amino acid;ultra high performance liquid chromatography（UHPLC）;hollow fiber membrane phase microextraction
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发布时间： - 摘要：In order to compare the differences between the work function values of materials measured by X ray photoelectron spectroscopy（XPS） and ultraviolet photoelectron spectroscopy（UPS），both techniques were used to respectively measure the Au,Ag film samples and monocrystalline silicon cleaned with argon ions,and the Au,Ag,MoO3 film samples,monocrystalline silicon and ITO without any surface cleaning.The calculation methods of work functions for materials measured by XPS and UPS were provided in this paper,and the influencing factors for the uncertainty of the work function values measured by photoelectron spectroscopy were discussed.Results showed that,in the measurement of the metal samples imposed a surface cleaning,the measurement values obtained by UPS and XPS displayed an obvious coherence with high accuracy,while the surface cleaned Au and Ag samples would be covered by an adsorption layer as soon as they were exposed to the air,and their work functions would change quickly.Therefore,when the intrinsic work functions of metal and semiconductors were measured,the sample surface should avoid being exposed to the atmosphere,and it is recommended that the sample surface should be cleaned with argon ion gun if it has been exposed to the atmosphere.This study showed that it is of a certain guiding significance for researchers to adopt reasonable measuring means according to actual test requirements关键词：work function;ultraviolet photoelectron spectroscopy;X ray photoelectron spectroscopy
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发布时间： - 摘要：A novel molecularly imprinted electrochemical sensor（MIP/rGO@Pd/GCE） for the determination of bisphenol A（BPA） was prepared by molecular imprinting technique based on reduced graphene oxide（rGO） and Pd composite（rGO@Pd） modified glassy carbon electrode（GCE）.BPA and pyrrole were used as template and monomer,respectively.The electrochemical properties of the molecularly imprinted electrochemical sensor were evaluated by cyclic voltammetry（CV）,differential pulse voltammetry（DPV） and electrochemical impedance spectroscopy（EIS）.The morphologies of the sensor were characterized by scanning electron microscopy（SEM） and Fourier transform infrared spectroscopy（FT-IR）.Under the optimum experimental conditions,the peak current intensity at the modified electrode was linear with BPA in the concentration range of 10-100 nmol/L.The limit of detection（LOD） for the sensor was 01 nmol/L and the correlation coefficient（r） was 0997 7.With high sensitivity,excellent selectivity,long term stability and remarkable reproducibility,this novel molecularly imprinted electrochemical sensor was successfully applied in the determination of BPA in water samples with spiked recoveries of 921%-1080%．关键词：bisphenol A;reduced graphene oxide and Pd composite;molecular imprinting technique;electrochemical sensor
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发布时间： - 摘要：A high performance liquid chromatographic（HPLC） method was established for the analysis of formaldehyde and acetaldehyde in cigarette capsules based on a novel extraction tube device integrating extraction，filtering and transfer in one step.The cigarette capsules were extracted with aqueous solution of acetonitrile（50% by volume） for 25 min.After purification，the extracts were allowed to derivatively react with 2,4 dinitrophenylhydrazine in an acidic condition（pH 48）.Then the derivatives of the extracts were analyzed by HPLC.The results indicated that the extraction tube device greatly simplified the sample preparation for HPLC analysis.Furthermore，the formaldehyde and acetaldehyde in the capsules were successfully separated and determined.The calibration curves for them both were linear in the ranges of 8-1 500 μg/L and 10-1 650 μg/L，respectively，with their correlation coefficients（r2） larger than 0999.The limits of detection（LOD） and quantitation（LOQ） for formaldehyde and acetaldehyde were 25 μg/L and 28 μg/L，and 80 μg/L and 95 μg/L，respectively.The mean recoveries for the target compounds were in the range of 969%-1011% with the intra day and inter day precisions both below 4%.The method provides a new strategy for the quantitation on formaldehyde and acetaldehyde in cigarette capsules with unprecedented simplicity，high precision and great reproducibility.关键词：capsule of cigarette;formaldehyde;acetaldehyde;extraction;high performance liquid chromatography（HPLC）
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发布时间： - 摘要：A gas chromatography-mass spectrometric（GC-MS） method was established for the determination of migration quantity of 2,6 dimethylphenol，p tert butylphenol，2,6 di tert butyl 4 methylphenol and butylated hydroxyanisole in food packaging materials，with water，4%（by volume） aqueous acetic acid，50%（by volume） aqueous ethanol and isooctane as the food simulated solution.Samples were soaked with food stimulant，and the water based food simulated soaking solution was extracted with ethyl acetate before analysis，while the isooctane soaking solution was analyzed without any pretreatment.The separation of target compounds was conducted using a DB-1701 capillary（30 m×025 mm×025 μm） column.The determination was performed in selective ion mode，and external standard method was used for quantitation.The results showed that，under optimized conditions，there were good linearities for four phenolic antioxidants between peak areas and concentrations in the range of 01-10 mg/L with correlation coefficients（r） more than 0999.The limits of detection（LOD） of this method were 001 mg/L，and the limits of quantitation（LOQ） were 003 mg/L.The spiked recoveries for four phenolic antioxidants in fruits at three spiked levels of 01，10，100 mg/L ranged from 915% to 110%，with relative standard deviations（RSDs，n=5） of 19%-93%.The method，with the advantages of accuracy，high reliability and sensitivity，was suitable for the determination of migration of four phenolic antioxidants in food packaging materials.关键词：phenolic antioxidants;food simulant;food packaging materials;gas chromatography-mass spectrometry（GC-MS）;migration quantity
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发布时间： - 摘要：A high performance liquid chromatography-tandem mass spectrometric(HPLC-MS/MS) method was developed for the simultaneous analysis of Nisin A and Nisin Z in fresh wet rice noodles.An extraction solution of formic acid(pH 30) was used to extract Nisin A and Nisin Z in fresh wet rice noodles samples.The extract was separated on a Hilic column,and determined with electrospray ionization(ESI) source in positive ion mode under multiple reaction monitoring(MRM) mode.There were good linear relationships for the analytes between their peak area responses and concentrations of 100-2 000 μg/L,with correlative coefficients larger than 0999.The limits of detection for Nisin A and Nisin Z were 001 mg/kg and 002 mg/kg,respectively.The recoveries were in the range of 956%-1070% with RSDs less than 20%.The method was reliable and accurate,and was suitable for the determination of Nisin A and Nisin Z in fresh wet rice noodles.关键词：Nisin A;Nisin Z;HPLC-MS/MS;fresh wet rice noodles
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发布时间： - 摘要：A method based on liquid chromatography-tandem mass spectrometry with accelerated solvent extraction（ASE/LC-MS/MS） was developed for the analysis of niclosamide and its degradation products（5 chlorosalicylic acid and 2 chloro 4 nitroaniline） in sediments.Extraction and cleanup were integrated into one step by accelerated solvent extraction（ASE） with 50 g neutral alumina as within cell adsorbing material,and different temperatures and static times were optimized with acetonitrile-water（3∶1,by volume） as extraction solvents.Under the optimized conditions,the calibration curves for niclosamide and its degradation products were linear in the range of 01-200 μg/L with their correlation coefficients（r） more than 0999.The limits of detection and quantitation of the method were in the ranges of 004-01 μg/kg and 02-05 μg/kg,respectively.The proposed method was applied in the trace analysis of niclosamide and its degradation products in sediments with average recoveries in the range of 935%-1019% at 3 spiked levels of 05,10 and 20 μg/kg,and relative standard deviations of 37%-67%.The method was simple,sensitive and reproducible,and was suitable for the analysis of real sample.关键词：liquid chromatography tandem mass spectrometry（LC-MS/MS）;niclosamide;degradation products;accelerated solvent extraction;sediment
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发布时间： - 摘要：A new method was established for the determination of two kinds of guanidines vulcanization accelerators,1,3 diphenyl guanidine（DPG） and 1,3 di o tolylguanidine（DOTG） in synthetic rubber materials by high performance liquid chromatography（HPLC）.The samples were extracted by soxhlet extraction with methanol,and separated on a C18 column with acetonitrile-phosphate buffer as mobile phase by gradient elution.The UV detection wavelength was set at 235 nm,and the external standard method was used for quantitative analysis.There were good linear relationships for the two componds in the concentration range of 2-50 mg/L with their correlation coefficients both 0999 9.The limits of detection of the method（MLODs） were 30 mg/kg and 40 mg/kg,respectively.The average recoveries for the analytes were in the range of 824%-945%,with the relative standard deviations（RSD,n=5） of 10%-33%.This method was simple,rapid and reliable,and was suitable for the determination of DPG and DOTG residues in synthetic rubber materials．关键词：rubber material;vulcanization accelerator;guanidine;high performance liquid hromatography（HPLC）
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发布时间： - 摘要：An ultra high performance liquid chromatography-tandem mass spectrometric(UHPLC-MS/MS) method was established for the determination of spinetoram residues,XDE-175-J and XDE-175-L in Radix Gotonopsic Tongshen Otiv.The samples were exacted with acetonitrile,and purified with primary secondary amine and graphitized carbon black.The target compounds were quantified by the external standard method.There were good linearities for the peak areas of XDE-175-J and XDE-175-L in the concentration ranges of 0075-75 μg/L and 0025-25 μg/L,respectively.The average recoveries for XDE-175-J and XDE-175-L at the spiked levels of 0375,375,75 μg/kg and 0125,125,25 μg/kg were in the ranges of 884%-1135% and 844%-995%,with relative standard deviations(RSDs) of 20%-42% and 25%-49%,respectively.The limits of quantitation(LOQs) for XDE-175-J and XDE-175-L were 0375 μg/kg and 0125 μg/kg,respectively.With the advantages of simplicity,rapidness and convenience,the method could meet the requirements for pesticide residues analysis,and be applied in the rapid detection of spinetoram residues in Radix Gotonopsic Tongshen Otiv.关键词：spinetoram;ultra high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS);Radix Gotonopsic Tongshen Otiv.;residues determination
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发布时间： - 摘要：In order to achieve the selective adsorption of heavy metal ions in environmental aqueous solution，a thiol groups functionalized gold nanoparticles metal stirring bar（AuNPs-SH-SBSE） was fabricated by self assembling 1,8 octanedithiol on surface of the etched stainless steel deposited with gold nanoparticles（AuNPs）.The extraction and separation properties of the stirring bar were evaluated with Pb（Ⅱ） and Cd（Ⅱ） by ICP-OES.Effects of adsorption time，pH value and desorption solvent on the adsorption were investigated.The results showed that，using equilibrium time of 30 min and an optimum pH of 80，60 mL 15 mol/L HNO3 as eluate，the maximal adsorption capacity of the stirring bar toward Pb（Ⅱ） and Cd（Ⅱ） reached to 985% and 874%，respectively.Under the optimal conditions，the method was successfully applied in the determination of trace Pb（Ⅱ） and Cd（Ⅱ） in real samples.There existed linearities for Pb（Ⅱ） and Cd（Ⅱ） in the ranges of 01-50 mg/L and 02-20 mg/L，with their limits of detection（S/N=3） of 24 ng/L and 36 μg/L，respectively.The recoveries at two spiked levels of 20 μg/L and 50 μg/L were in the ranges of 854%-1050% and 742%-978%，with their RSDs（n=3） of 38%-82% and 42%-106%，respectively.The method was simple，rapid and sensitive，and could be applied in the separation and detection of Pb（Ⅱ） and Cd（Ⅱ） in environmental water.关键词：gold nanoparticles;thiol groups functionalized;stir bar sorption;heavy mental ions
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发布时间： - 摘要：A method based on gas chromatography-triple quadrupole mass spectrometry with headspace（HS/GC-MS/MS） was developed for the determination of three xylene isomers in seafoods.The samples were incubated at 90 ℃ and oscillated for 40 min,then separated on an HP-INNOWax column.The determination of the target compounds were performed by GC-MS/MS under the multiple reaction monitoring（MRM） mode,and the quantification was carried out using the external standard method.The calibration curves for three xylene isomers were linear in the range of 50-1000 μg/kg with their correlation coefficients（r2） larger than 099.The limits of detection（LOD） and quantitation（LOQ） of the method were 25 μg/kg and 50 μg/kg,respectively.The recoveries at three spiked level of 60,150,500 μg/kg were in the range of 896%-1124% with relative standard deviations（RSD） not more than 115%.The method was successfully applied in the determination of xylene isomers in seafoods.With the advantages of simple operation,accuracy and high sensitivity,the method was suitable for the determination of xylene residues in seafoods.关键词：headspace;gas chromatography-triple quadrupole mass spectrometry（GC-MS/MS）;xylene;isomer;seafood
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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 simultaneous analysis of 10 antiviral drugs,eg.valaciclovir,abacavir,entecavir,zidovudine,nevirapine,ganciclovir,telbivudine,lamivudine,acyclovir and amantadine in surface water.The aqueous samples were concentrated and purified on an ISOLUTE ENV+ cartridge,and then separated on a Waters ACQUITY UPLCTM BEH C18 column by gradient elution with 01% formic acid-acetonitrile as mobile phase.The detection of antiviral drugs was performed by tandem mass spectrometry in electrospray ionization under multiple reactions monitoring（MRM） mode.The calibration curves for target compounds were linear over the range of 05-200 ng/L with correlation coefficients（r2） larger than 0993.The average recoveries for antiviral drugs in surface water at three spiked concentration levels ranged from 700% to 1040%,with the limits of quantitation（LOQ） of 02-50 ng/L and the relative standard deviations（RSDs） less than 15%.This method could be applied in the analysis of antiviral drugs in aqueous samples.关键词：ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）;antiviral drugs;surface water;solid phase extraction（SPE）
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发布时间： -
Determination of Acesulfame Potassium in Swimming Pool by High Performance Capillary Electrophoresis
摘要：A high performance capillary electrophoresis method with solid phase extraction was established for the determination of acesulfame potassium(ACE),a urine indicator in swimming pool water.The separation was performed on a fused silica capillary with uncoated inner wall(602 cm×75 μm id.,an effective length of 50 cm),using 10 mmol/L sodium tetraborate(pH 93) as electrophoresis buffer at a separation voltage of 24 kV.The sample was injected for 20 seconds at a detection wavelength of 226 nm.The swimming pool samples were directly analyzed after filtered and enriched by solid phase extraction(SPE).The results showed that,under the optimized conditions,a good linear relationship was obtained for acesulfame potassium in the concentration range of 02-1000 mg/L,with a correlation coefficient(r) of 0999 8,and a detection limit of 500 μg/L.The spiked recoveries were in the range of 960%-1036% with relative standard deviations(RSDs) for migration time and peak height of 073% and 18%,respectively.The method is sensitive,simple and reliable,and is suitable for the detection of acesulfame potassium in swimming pool water.关键词：high performance capillary electrophoresis;solid phase extraction;acesulfame potassium;urine indicator- 791
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发布时间： - 摘要：The pyrolysis behavior of pelargonic acid vanllylamide(PAVA) was investigated by gas chromatography-mass spectmmetry with on line pyrolysis(Py/GC-MS) in the presence of helium.The influence factors of PAVA pyrolysis behavior such as different temperatures and different time were studied.GC-MS was used for the qualitative and semi quantitative analyses on PAVA pyrolysis products.The results indicated that pyrolysis temperature had a significant effect on the types and relative contents of pyrolysis products.14 products were detected when the temperature reached 700 ℃ above,including nonanamide,2 methoxy 4 methylphenol,1 hexene,nonanenitrile,nonaldehyde,etc.The pyrolysis rate of PAVA increased gradually with time increasing.According to the pyrolysis products and their contents,the pyrolysis regulation for PAVA was preliminarily dicussed.关键词：pelargonic acid vanllylamide;pyrolysis;gas chromatography-mass spectrometry(GC-MS)
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发布时间： - 摘要：The detection and traceability technology of characteristic components of agricultural products are powerful tools for government to regulate the market and protect geographical indications products.The recent research progress on the detection of organic chemical compositions and mineral elements,and the traceability of wolfberry are comprehensively reviewed in this paper,including chromatographic techniques（high performance liquid chromatography and gel permeation chromatography）,mass spectrometry and its coupled techniques（gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry）,infrared spectroscopy（fourier transform infrared spectroscopy and near infrared spectroscopy）,inductively coupled plasma atomic emission spectrometry and inductively coupled plasma mass spectrometry.More applications of chemometrics are also briefly introduced.The aim of this paper is to provide a valuable reference for the quality control and origin traceability of wolfberry,and preferably promote the healthy development of consumption market of wolfberry.关键词：wolfberry;characteristic component;analytical technique;traceability;geographical indications;review
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