最新刊期
卷 37 ， 期 12 ， 2018
- 摘要：A gas chromatograph-mass spectrometric（GC-MS） method based on ultrasound assisted extraction and dispersive solid phase extraction was developed for the simultaneous determination of 18 polychlorinated biphenyls（PCBs） in fresh tea leaves.The samples were extracted using a mixture of hexane-acetone（1∶1,by volume） by ultrasonic extraction,and cleaned up with the mixed sorbents of carboxylated multi walled carbon nanotubes（MWCNTs-COOH） and primary secondary amine（PSA） after replacing hexane-acetone by toluene,then detected by GC-MS under selected ion monitoring mode.The PCBs were qualitatively confirmed by retention time and relative abundance ratio of characteristic ions,and quantified by the external standard method with matrix matched standards solution.The chromatographic and MS parameters influencing separation and sensitivity were optimized,and several important factors affecting extraction and purification efficiency such as type and volume of extraction solvent,extraction time,type and amount of cleanup sorbent and cleanup time were investigated.Under the optimum conditions,satisfactory linear relationships for the analytes were observed in the concentration range of 5-500 μg/kg with correlation coefficients not less than 0.999 8.The recoveries for 18 PCBs in fresh tea leaves at spiked levels of 5,10 and 100 μg/kg were in the range of 92.3%-111% with relative standard deviations（n=6） of 1.2%-7.9%.The limits of detection and the limits of quantitation for PCBs were 0.5-1.4 μg/kg and 5 μg/kg,respectively.The method was simple,rapid,accurate,sensitive and effective in purification,and was suitable for the determination of 18 PCBs in fresh tea leaves.关键词：carboxylated multi walled carbon nanotubes;dispersive solid phase extraction;gas chromatography-mass spectrometry（GC-MS）;fresh tea leaves;polychlorinated biphenyls（PCBs）
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发布时间： - 摘要：In this review，the porcine liver esterase（PLE） organic-inorganic hybrid nanoflowers（Ca3（PO4）2-PLE） were prepared in phosphate buffer by biomineralization strategy.The morphology and components of the prepared organic-inorganic hybrid nanoflowers were analyzed by scanning electron microscopy（SEM），energy dispersive spectrometry（EDS） and Fourier transform infrared spectroscopy（FT-IR）.The parameters for the preparation of PLE hybrid nanoflowers were optimized.Results showed that the prepared PLE hybrid nanoflowers had the highest enzyme activity in phosphate buffer solution（pH 74） of 10 mmol/L，PLE concentration of 03 g/L and calcium ion concentration of 500 mmol/L at preparation temperature of 20 ℃，and its enzyme activity was 169% of the free enzyme in the same enzyme concentration.Furthermore，the PLE hybrid nanoflowers were used to study the enzymatic hydrolysis properties toward four pyrethroid pesticides.It was found that under the same conditions，the enzymatic hydrolysis rates of PLE hybrid nanoflowers were better than that of the free enzyme.In addition，the prepared PLE hybrid nanoflowers still remained over 70% of the enzymatic activity after twice uses of the pyrethroid pesticide enzymatic cycle.关键词：hybrid nanoflowers;porcine liver esterase（PLE）;pyrethroid pesticide;enzyme activity;enzymolysis
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发布时间： - 摘要：A method of high performance liquid chromatography with solid phase extraction using covalent organic polymers（COPs） was developed for the analysis of three fluorescent whitening agents（FWAs） in flour.The COPs with satisfactory adsorption performance were successfully synthesized by the Schiff base reaction of 1,3,5 triformylphloroglucinol and 2,6 diaminopyridine at room temperature,using BiCl3 as catalyst,then characterized by Fourier transform infrared spectroscopy（FT-IR） and nitrogen adsorption experiment.Results showed that the imine linked COPs with good specific surface area were successfully constructed.The synthesized COPs were used as the SPE sorbent in the extraction of three FWAs in flour,and finally the three FWAs were determined by high performance liquid chromatography（HPLC）.Under the optimum conditions,the method exhibited good linear relationships for the analytes in the range of 1-100 μg·L-1 with limits of detection（LODs,S/N=3） and limits of quantitation（LOQs,S/N=10） of 015-027 μg·kg-1 and 050-089 μg·kg-1,respectively.The recoveries for three FWAs in flour at three spiked levels ranged from 812% to 102% with relative standard deviations（RSDs） of 43%-127%.The developed method was simple,accurate and sensitive,and could be applied in the determination of FWAs in flour samples.关键词：flour;fluorescent whitening agents;covalent organic polymers;solid phase extraction（SPE）;high performance liquid chromatography（HPLC）
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发布时间： - 摘要：A novel benzenesulfonate silica based mixed mode stationary phase with double ligand was prepared by thiol ene click chemistry method.Both 13C NMR and elemental analysis data showed that the phenyl and benzenesulfonate were successfully bonded to the surface of stationary phase.Depending on solute structure and composition of mobile phase,the mixed mode stationary phase provided different separation modes,including reversed phase（RP）,hydrophilic（HILIC） and strong cation exchange（SCX） interactions.The RP capability achieved the separation of alkylbenzenes with good methylene selectivity.The HILIC behavior was evaluated by employing several nucleosides and bases.Moreover,retention factors of solutes versus volume percentage of aqua in mobile phase exhibited a typical U shaped curve,which indicated that Ph/BS phase has RP and HILIC dual retention mechanism.The retention behavior of amine compounds on the stationary phase reflected RP and SCX mixed mode retention characteristic.In addition,the effective separation of melamine and related purities was obtained in SCX mode.Acidic,neutral and basic drugs were also well separated under the RP and SCX mixed mode conditions.This mixed mode stationary phase has the potential advantages in the separation analysis of complex samples.关键词：mixed mode stationary phase;thiol ene click chemistry;reversed phase;cation exchange;hydrophilic interaction;drug separation
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发布时间： - 摘要：A method of gas chromatography-tandem mass spectrometry（GC-MS/MS） was developed for the determination of 8 polyaromatic hydrocarbons（PAHs）,18 polychlorinated biphenyls（PCBs） and 16 organochlorine pesticides（OCPs） in geographical original soil of bamboo shoot.The samples were extracted with acetone-hexane（1∶1,by volume） in an superpower ultrasonic bath,then purified with a Florisil composite column.The eluant was concentrated by N2 blowing,finally detemined by GC-MS/MS.42 persistent organic pollutants（POPs） were efficiently separated within 35 min,and there were good linearities for the analytes in the concentration range of 2.0-2 000.0 μg/L with their correlation coefficients（r2） of 0.995 2-0.999 8.The spiked recoveries ranged from 62.3% to 128% with relative standard deviations of 0.5%-15.8%,and the limits of detection（S/N=3） were 0.070-6.902 μg/kg.With the characteristics of easy operation,high sensitivity and accuracy,the method could be applied in the simultaneous detection of 42 POPs in original soil of bamboo shoot.关键词：polyaromatic hydrocarbons（PAHs）;polychlorinated biphenyls（PCBs）;organochlorine pesticides（OCPs）;original soil of bamboo shoot;solid phase extraction;gas chromatography-tandem mass spectrometry（GC-MS/MS）
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发布时间： - 摘要：A gas chromatography-mass spectrometry(GC-MS) with silanized derivatization was developed for the determination of major tobacco constituents in 21 cigarette samples of three brands.The obtained GC-MS fingerprint data were processed by cluster analysis and principal component analysis,respectively.Results showed that the method could be used in the comparison and discrimination on cigarettes of different brands,and the proportion distribution of various silanized components reflected fairly well the characteristics of different brands of cigarettes.The developed method could provide a reference for cigarette style characterization,quality maintenance and authenticity discrimination.关键词：silanization;gas chromatography-mass spectrometry(GC-MS);fingerprint;cluster analysis;principal component analysis
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发布时间： - 摘要：A method of ultrahigh performance liquid chromatography(UPLC) with DOLPA/AOT-isooctane reverse micelles was developed for the determination of heliosupine,heliotrine,lasiocarpine and heliotridine in Cynoglossum amabile Stapf et Drumm.Experimental conditions affecting the reverse micelles such as types and concentration of surface active agent,pH value,salt species and concentration,ratio of sample and reverse micelles,extraction time and back extraction time were optimized.The optimal conditions were as follows:DOLPA /AOT concentration:06 mol/L,pH value:40,KCl concentration:02 mol/L,ratio of sample and reverse micelles:4∶1,extraction time:10 min,back extraction time:30 min.Under the optimal conditions,heliosupine，heliotrine，lasiocarpine and heliotridine were separated,and determined by UPLC with acetonitrile-02% triethylamine as mobile phase by gradient elution.Four ingredients were separated in 16 min.There existed good linear relationships for the analytes between peak areas and concentrations,with detection limits of 0030,0050，0040 and 0020 mg/L,respectively.The recoveries were in the ranges of 982%-103%,979%-102%,981%-101% and 978%-104%,respectively.The RSDs for recovery,precision and reproducibility were not more than 23%.The method is convenient，sensitive and accurate,and is suitable for the determination and confirmation of 4 alkaloid in Cynoglossum amabile Stapf et Drumm.关键词：Cynoglossum amabile Stapf et Drumm;alkaloids;reverse micelles;ultrahigh performance liquid chromatography(UPLC)
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发布时间： - 摘要：A novel method of high performance liquid chromatography coupled with oxidized sepiolite（O-Sep） based solid phase extraction（SPE） was developed for the analysis of sulfonamides in environmental water samples.The O-Sep was successfully synthesized by acid treatment,then packed into a homemade PEEK micro column,which had a high adsorption capacity towards sulfameter（SMD）,sufladoxine（SDX） and sulfaphenazole（SPP）,and the corresponding saturated extraction amounts of 10 mg O-Sep were 203.2,150.3 and 102.1 ng,respectively.The calibration curves of SMD,SDX and SPP showed good linear relationships in the range of 1.0-50.0 μg/L,with their detection limits of 0.3-0.5 μg/L and relative standard deviations（RSDs） not more than 5.0%.The method was applied in the simultaneous analysis of three analytes with satisfactory recoveries,which were 79.5%-98.3% for tap water,74.3%-98.6% for river water and 70.2%-98.7% for rain water with RSD of 1.4%-7.6%.This method was simple,sensitive and accurate,and showed a great potential in the determination of trace sulfonamides in environmental samples.关键词：sulfonamides;oxidized sepiolite;online μ-SPE;high performance liquid chromatography（HPLC）
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发布时间： - 摘要：Based on replicate results of liquid chromatography-mass spectrometry(LC-MS),a statistical learning model,which combined time difference and peak shape similarity,was proposed in this paper to solve the problems of low matching accuracy and low coverage of peptide chain alignment.A time difference statistical model was built,which focused on the statistical characteristics of time shift.However,only based on the time feature,the error of alignment could not be eliminated completely.Besides the time,peak shape feature was also introduced in this paper under the hypothesis that the same peptide chain would produce similar LC peaks in repeated experiments.This model was also tested by testing peptide sequences signal.Results showed that the accuracy of the proposed method could reach 98.3%.The coverage for the union of the two datasets could achieve 91.0%.The peak shape similarity model could improve the final result of the time model,helping to confirm the corresponding peak pair in LC-MS replicates data.关键词：liquid chromatography-mass spectrometry(LC-MS);alignment;similarity of peak shape;statistical learning model
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发布时间： - 摘要：A method was developed for the detection of protein concentration with a smart phone confirming the parameter for image colorimetry,which was used to determine the concentration of reactants in different colors.The linear correlation coefficient of the proposed method was higher than 0.99,and the limit of detection(LOD) was 0.21 g/L.The detection performances of different brands of smart phones were investigated.Results demonstrated that the detection performances were basically independent from hardware configuration of smart phones.The repeatability of this method was also investigated.On detection of a single sample,the relative standard deviations (RSDs) for three concentrations of the sample were 2.0%,4.6% and 11.9%,respectively.Four samples were determined simultaneously,and the RSDs were 2.2%,3.8%,3.5% and 11.5%,respectively.The influences of brightness,color temperature and shooting distance were discussed.Results showed that brightness and color temperature were insignificant to detection,while the shooting distance could influence the detection results.The APP of smart phone was applied in the sample detection.The correlation coefficient(r2) between detection results of smart phones and spectrophotometer was 0.969.With the characteristics of high accuracy,high repeatability,portability and easy operation,the method could realize the fast detection on various products.关键词：image colorimetry;smart phone;quantitative detection;protein
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发布时间： - 摘要：A cobaltion-5-（5-iodide-2-pyridylazo）-2,4-diamino toluene（5-I-PADAT）（Co2+-5-I-PADAT） modified electrode was prepared via cyclic voltammetric electrodeposition with Co2+-5-I-PADAT,a coordination compound as supporting electrolyte in the scanning potential range of-1.5-0.5 V by 50 deposition circles.The morphology and composition of the modified electrode were characterized by scanning electron microscopy and X ray crystalline diffraction.The electrocatalytic oxidation behavior of hydrazine on the modified electrode was also investigated.Results indicated that a significant hydrazine oxidation peak appeared at a potential of 0.55 V in a pH 7.0 phosphate buffer solution.Based on that,a novel method for the quantitative analysis of hydrazine was established.There was linear relationship for the oxidation peak current with hydrazine in the concentration range of 0.64-2 150 μmol/L with a correlation coefficient of 0.998 0.The detection limit（S/N=3） was 0.28 μmol/L,and the recoveries were in the range of 95.3%-102%.With the advantages of good reproducibility and selectivity,the sensor could satisfy the requirements for detection of hydrazine in environmental samples.关键词：electrochemistry;modified electrode;5 （5 iodide 2 pyridylazo） 2,4 diamino toluene(5 I PADAT);hydrazine;nano cobalt
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发布时间： - 摘要：Fluorescent carbon dots(PM-CDs) were synthesized by a simple one step hydrothermal carbonization method with the extract of unripe persimmon(Diospyros Kaki L.f).TEM image showed that the PM-CDs were homogeneous spheres with a average particle diameter about 15.39 nm.XRD revealed that the PM-CDs were a kind of amorphous carbon material like graphene.The elements of PM-CDs were determined by XPS,which contained complicated elements,and the principal elements presented in PM-CDs were in accordance with those in the general CDs.The PM-CDs contained some active groups,such as hydroxyl,carboxyl and amino.There existed an absorbance for PM-CDs at 350 nm,which emitted an excitation dependent fluorescence at a maximum excitation wavelength of 355 nm and a maximum emission wavelength of 445 nm.Meanwhile,the PM-CDs had a pH independent fluorescence,and showed a stable emission peak in a pH range of 5.0-11.0.The PM-CDs had a strong blue fluorescence under UV irradiation at 365 nm.The PM-CDs had higher selectivity toward Fe3+ compared to other co existed metal ions.The fluorescence intensity of PM-CDs had a linear response to Fe3+ in the concentration range of 0.45-50 μmol/L with correlation coefficients(r2) of 0.923 4,which demonstrated that they were available in the detection of Fe3+.It is necessary to further explore the purification technology for CDs from biomaterials,improving the recognition sites for target analytes and obtaining the higher efficiency for detection.关键词：carbon dots(CDs);hydrothermal synthesis;persimmon;Fe3+;fluorescent probe
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发布时间： - 摘要：A continuous flow analytical method with rapid solid phase extraction was developed for the determination of hexavalent chromium in colorful cigarette paper and tipping paper.The pigments in colorful cigarette paper and tipping paper were removed by a rapid solid phase extraction,which improved the sample cups for continuous flow analytical system.The developed method greatly simplified the sample pretreatment process with no need of sample transferation,effectively overcoming the shortcomings of traditional methods,such as more pretreatment steps,cumbersome operation and low detection efficiency,etc.Furthermore,the method has the advantages of simple operation,high sensitivity,rapid detection,automation of detection,etc.The detection limit and the quantitation limit of the method was 0.85 μg/L and 2.5 μg/L,respectively.The recoveries for hexavalent chromium at three spiked levels were in the range of 88.5%-97.3%.The intra day and inter day relative standard deviations were below 4.0%.The results of this method were agreed with those of the Chinese tobacco standard method.The presented method could be successfully used in the rapid determination of hexavalent chromium in colorful cigarette paper and tipping paper.关键词：continuous flow analytical system;sample cups;improvement;rapid solid phase extraction;hexavalent chromium;colorful cigarette paper and tipping paper
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发布时间： - 摘要：A high performance liquid chromatographic(HPLC) method was developed for the direct and simultaneous determination of cystine,tyrosine and histidine in hair of rat.The chromatographic separation and detection conditions were optimized,and the samples were analyzed after acid hydrolysis.The determination was performed on a Titank C18 column(4.6 mm×250 mm,5 μm) with acetonitrile-10 mmol/L diammonium hydrogen phosphate buffer(containing 10 mmol/L sodium 1-octanesulfonate and obtaining pH 2.0 by phosphoric acid) as mobile phases by gradient elution at a flow rate of 1.0 mL/min.The detection wavelength was set at 205 nm,and the injection volume was 100 μL.The column temperature was set at 8 ℃.Under the optimal conditions,cystine,tyrosine and histidine in hair of rat were effectively separated．Good linearities for the analytes were obtained in their respective ranges,with correlation coefficients(r) larger than 0.999.The limits of detection(S/N=3) were in the range of 49- 442 μg/L and the limits of quantitation(S/N=10) were 148-884 μg/L.The spiked recoveries were in the range of 97.8%-102% with relative standard deviations of 0.1%-1.6%.This method is simple,accurate,reliable and reproducible,and could be applied in the determination of cystine,tyrosine and histidine in hair of rat.关键词：hair of rat;cystine;tyrosine;histidine;high performance liquid chromatography(HPLC)
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发布时间： - 摘要：A method of gas chromatography-mass spectrometry（GC-MS） with solid phase extraction was developed for the determination of nitrogen compounds in fluid catalytic cracking（FCC） diesel fraction.The neutral and alkaline nitrogen compounds in FCC diesel fraction were separated and concentrated by solid phase extraction（SPE） technique.The type and dosage of different elution solvents were optimized.It was found that dichloromethane and acetone-dichloromethane could effectively separate the neutral and alkaline nitrogen compounds in FCC diesel.The recovery and repeatability of the SPE method were investigated.Results showed that the recovery of the separation method was as high as 99.5%，and the relative standard deviations for the repeatability results of three separation experiments were less than 4%.The separated components were confirmed by gas chromatography-mass spectrometry（GC-MS）.It was revealed that neutral nitrogen compounds generally consisted of C0-C3 indoles and C0-C5 carbazoles，while alkaline nitrogen compouns were made up of C1-C4 anilines and C0-C2 quinolines.The quantitation on nitrogen compounds was carried out by gas chromatography with nitrogen chemiluminescence detector（GC-NCD）.Results showed that 96.6% of the identified compounds in FCC diesel attributed to the neutral compounds，in which the content of carbazoles was the highest，accounting for 64.3% of the total of the qualified nitrogen compounds.From the aspect of compound structure，the content of nitrogen compounds increased first and then decreases with the increase of the number of methyl substituents.In general，this method could be used in the analysis on the type distribution of nitrogen compounds in FCC diesel fraction.关键词：nitrogen compounds;gas chromatography;solid phase extraction;diesel;gas chromatography-mass spectrometry
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发布时间： - 摘要：A method of proton nuclear magnetic resonance was developed for the determination of hydrochloride palmatinein in tablets.CD3OD was employed as solvent and maleic acid as an internal standard,the 1H NMR spectra were obtained with a Bruker AVANCE Ⅲ 400 spectrometer.The content of hydrochloride palmatinein in tablets was determined by comparing the response signal areas of the internal standard（maleic acid,Ar） and hydrochloride palmatine（As）.Results showed that there was a linear relationship for hydrochloride palmatine in the range of 1.00-10.00 g/L with its correlation coefficient of 0.999 3.The limit of quantitation（LOQ） was 25.0 mg/L and the limit of detection（LOD） was 8.5 mg/L.The recoveries were in the range of 98.5%-104%.The content of hydrochloride bamatine in tablets was determined by high performance liquid chromatography （HPLC） and proton nuclear magnetic resonance（qNMR）,respectively.Results indicated that the two methods had no difference.The qNMR method was easy and simple to handle,and the analysis results was accurate.Furthermore,the structure of the analyte could be identified at the same time.Therefore,qNMR could be used for the quality control of Huangtengsu tablet.关键词：Huangtengsu tablet;hydrochloride palmatine;NMR;quantitative analysis;identify
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发布时间： - 摘要：A reversed phase high performance liquid chromatographic(RP／HPLC) method was established for the determination of imidacloprid in rat plasma,which was used to investigate the imidacloprids pharmacokinetics in rats by intragastric administration.The plasma sample was extracted with methanol,then determined by RP／HPLC.The sample was separated on a C18 column(4.6 mm×250 mm,5 μm ) with a mobile phase of methanol-water(30∶70) at a flow rate of 1.0 mL·min-1,and detected at a wavelength of 245 nm.The imidacloprid concentration in plasma was detected at predetermined time intervals after SD rats were intragastrically given a single dose of lutein suspension at 68.1 mg·kg-1,then the concentration time curve was plotted and the pharmacokinetic parameters were calculated.The main parameters for intragastric administration were follows:Cmax=23.557 mg/L,tmax=7.333 h,t1/2α=4.472 h,AUC(0-t)=276.727 mg·h/L.There was a linear relationship for imidacloprid (r2=0.999 8) in the concentration range of 0.5-100 mg·L-1 with a detection limit of 10 μg·L-1.The average recovery for the analyte was 74.7%.The pharmacokinetic results in rats showed that imidacloprid was distributed in two compartment models in rats,and eliminated by the first order pharmacokinetics.The method was simple and reliable,and could satisfy the requirements for the detection of imidacloprid and its pharmacokinetic study in rat plasma.关键词：imidacloprid;pharmacokinetics;reversed phase high performance liquid chromatography(RP／HPLC)
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发布时间： - 摘要：A 4-aminobiphenyl molecularly imprinted polymer modified pencil graphite electrode（4-ABP-MIP／PGE） was fabricated with a pencil graphite electrode（PGE） as working electrode,a platinum electrode as counter electrode and a saturated calomel electrode as reference electrode.The PGE was put into a pH 7.17 PBS containing 4.0×10-3 mol/L acrylic acid and 1.0×10-3 mol/L 4-aminobiphenyl（4-ABP）,scanned via cyclic voltammetry by 16 cycles in range of-1.6-1.6 V at a scan rate of 0.1 V·s-1,followed by ultrasonic elution for 6 min.By means of the interfacial potentiometry with double poles,the zero current potential EZCP of 4-ABP-MIP／PGE was linear with logarithm of 4-ABP concentration in the range of 0.005-50 μmol/L,with a detection limit of 1.07 nmol/L.The sensor was used in the determination of 4-ABP in real samples with recoveries of 96.0%-102%.关键词：4-aminobiphenyl;molecularly imprinted polymer;interfacial potential;zero current potential
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发布时间： - 摘要：There are two kinds of redox reactions occurring in electrospray ionization mass spectrometry,ie.electrochemistry and corona discharge induced redox reactions.On one hand,the two kinds of redox reactions will complicate the mass spectra,and decrease the sensitivity for analyte detection.On the other hand,the reactions could be used to develop new ionization sources,improve the ionization efficiency for hardly ionized species and study the protein interaction.The research progress of electrochemistry and corona discharge induced redox reactions at home and abroad was introduced in this review,including their advantages and disadvantages,as well as the methods used to control the two redox reactions.Finally,the methods used to distinguish the two kinds of oxidation reaction were summarized.关键词：electrospray;mass spectrometry;electrochemistry;corona discharge;redox reaction
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发布时间： - 摘要：Hairpin structured DNA self assembly is widely used in the detection on biomolecules as it possesses the advantages of enzyme free,isothermal and high recognition rate,etc.In this paper,the types of DNA self assembly and its application in the detection of foodborne pathogens,tumor marker,protein,inorganic metal and small biomolecules are briefly summarized,and its future developments are also discussed so as to provide a reference for the study of biomolecules based on hairpin structured DNA self assembly.关键词：DNA self assembly;determination;research progress
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