最新刊期
卷 36 ， 期 5 ， 2017
- 摘要：Traditional Chinese medicine(TCM) is a treasure of Chinese medical science, and it has been widely applied in the prevention and treatment of disease at home for century.Owing to the reasons that the gradient of TCM is complex and the mechanism of drug efficiency is not clear,the process of modernization and internationalization for TCM has been restricted seriously.With the advantages of high sensitivity,high selectivity,high stability and high-throughput,mass spectrometric(MS) technology is especially suitable for the qualification and quantitation of complex components and their metabolites in TCM.In this paper,the typical application research of MS technology in composition identification and quality control,metabolomics and pharmacokinetics of TCM study in recent years are reviewed,and the problems existed and the improvements are discussed.关键词：mass-spectrometry(MS);traditional Chinese medicine(TCM);quality control;metabolomics;pharmacokinetics
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发布时间： - 摘要：A rapid and accurate method was developed for the determination of 7 mycotoxins (PAT,OTA,AOH,AME,ALT,TEN and TeA) in apple, apple juice, apple wine, apple acid, apple jam and canned apples by UPLC-MS/MS.10 g of the sample(10 mL of liquid sample) was precisely weighed, and extracted with acetonitrile containing 10 mmol/L citric acid solution, then 4 g of 4A molecular sieve and 1 g of NaCl were added. After oscillation and centrifugation, the liquid supernatant was purged with C18 decontaminant. Finally, it was filtered through a 0.22μm PTFE membrane and analyzed by UPLC-MS/MS. The method showed good linear relationships for 7 mycotoxins in the concentration range of 2-150μg/L with correlation coefficients above 0.99.The detection limits were in the range of 0.02-1.8 μg/L, and the limits of quantitation were 1-5μg/L. The recoveries of 7 mycotoxins were between 71.8% and 112.4% at three spiked concentrations levels of 10,50,100μg/L. This method is rapid and efficient in the simultaneous detection of 7 mycotoxins in apple and its products. This will lay a foundation for the risk monitoring of mycotoxin contamination in apple and its products.关键词：mycotoxin;UPLC-MS/MS;4A molecular sieve;apple;apple product
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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 7 pyrethroid pesticide residues in tea was developed using dispersive solid phase extraction and dispersive liquid-liquid microextraction(d-SPE-DLLME) as sample preparation methods. The samples were extracted with acetonitrile，purified with primary secondary amine(PSA) and multi-walled carbon nanotubes(MWCNTs) as sorbents，concentrated into carbon tetrachloride(CCl4)，and analyzed by GC-MS/MS. The effects of different kinds of extractants, volume and types of extractants, volume of dispersants and extraction time on extraction efficiency were investigated by using full fermented black tea as the matrix. In the experiment, acetonitrile was used as extractant in d-SPE，200μL of CCl4 was used as extractant, 1 mL of acetonitrile was used as dispersant，and extraction time was 1 min in DLLME. The results showed that the calibration curves of 7 pesticides were linear in the range of 10-500μg/kg，and the limits of quantitation were 1.0-10.0μg/kg. The average recoveries of 7 pesticides in four kinds of tea(black tea，green tea，oolong tea and dark tea) at four spiked levels were in the range of 75.4%-113.6%.The relative standard deviations(RSD,n=5) were not more than 8.8%.The proposed method showed the advantages of simplicity, rapidness, low cost and low detection limit, and was successfully applied in the detection of twelve commercially available tea samples.关键词：dispersive solid-phase extraction(d-SPE);dispersive liquid-liquid microextraction(DLLME);gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS);pesticide residue;tea
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发布时间： - 摘要：A method for the determination of ten plant growth regulator residues in fruit and bean sprout by ultra performance liquid chromatography-electrospray tandem mass spectrometry(UPLC-MS/MS) was established. The samples were extracted by the stirring and ultrasound using formic acid-acetonitrile(1∶1000), and purified with the solid phase extraction column. The analytes were separated by using methanol-5mmol/L ammonium acetate as mobile phase. The identifications were achieved by the electrospray ionization in positive and negative mode(ESI+/ESI-) using the multiple reaction monitoring(MRM).The quantifications were performed by the matrix matched isotope-labelled internal standards. Under the optimal experimental conditions, the calibration curves of ten analytes showed good linearities in the concentration range of 0.1-50.0μg/L with correlation coefficients(r2) above 0.995. Recoveries were between 52.4% and 119.6% with RSDs less than 13.0%.The limits of detection were 0.2μg/kg. The method had the advantages of simple pretreatment, good purification and low matrix effects, and was suitable for the rapid, high-throughput quantitative analysis of plant growth regulator residues in fruit and bean sprout.关键词：ultra performance liquid chromatography-tandem mass spectrometry;plant growth regulator;isotope-labelled internal standards;fruit;bean sprout
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发布时间： - 摘要：In order to study the adaptability of using different kinds of spectral information for quick analysis of the quality of radix scutellariaes(RS)，the contents of baicalin in 73 batches of RS determined by high performance liquid chromatography(HPLC) were used as dependent variables(y)，the near infrared spectra(NIRs)，ultraviolet-visible spectra(UV-Vis) and multi-source complex spectral(MSCs) information including UV-visible and near infrared spectra were used as independent variables(x).The partial least square regression(PLSR) and a novel method called as keeping same relationship between X and Y space on K nearest neighbors(KNN-KSR for short) were applied to predict the contents of baicalin in the RS samples based on above three kinds of spectral information.By comparing the root mean square error of prediction(RMSEP)，the average relative error(MRE) and correlation coefficient(R) between the measured and predicted values in validation set were applied to evaluate prediction precision. Regardless of the types of spectral information，the prediction precision of KNN-KSR method was always better than the PLSR method. The analysis results of baicalin based on NIRs were the best，and those based on the UV-visible spectra were the second. Although the prediction error of baicalin contents was the biggest based on the multi-source complex spectral information，it was still lower than 6%.The error satisfied the requirement of industrial analysis. The multi-source complex spectrometer has the advantages of small volume，light weight，low cost and portability. It is expected to improve the analytical precision of the instrument by optimizing its wavelengths and modeling method，so that it could be adapt to rapid spot acquisition of more herbs，and to analyze and monitor the quality of follow-up products.关键词：Multi-source complex spectrometer;near infrared spectroscopy;ultraviolet-visible spectra;baicalin
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发布时间： - 摘要：The mechanisms underlying the interaction of miRNAs with their mRNA targets are quite complex,which makes miRNA target prediction be a hot issue in the field of miRNA research.The features of miRNA-target sites pairing sequences were proposed based on the CLASH dataset,and the random forest models were applied for modeling.The average values of Acc,Sen,Spe,Pre and Mcc are 90.05%，89.47%，90.56%，90.43% and 0.799 8,respectively,and the AUC of ROC and PRC are 0.954 and 0.958,respectively.The results indicated that the current method shows a better performance compared with the existed methods, and the features newly constructed have a very significant impact on the identification of miRNA target genes.关键词：miRNA;target prediction;CLASH;sequence analysis
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发布时间： - 摘要：Metabonomics technology was used to investigate the mechanism of Liuwei Dihuang Pill treating acute kidney injury induced by gentamicin.The ultra performance liquid chromatography-mass spectrometry(UPLC-MS) coupled with principle component analysis(PCA) and orthogonal partial least squares discriminant analysis(OPLS-DA) were used to evaluate the changes of biomarkers of control group,model group and treatment group.Significant differences between the control group,model group and treatment group were observed in clustering analysis,PCA and OPLS-DA model.Seventeen potential biomarkers between control group and model group were identified as multiple phosphatidycholines,sphinganine,phytosphingosine,SM(d18∶0/16∶1(9z)),arachidonic acid.The relative contents of sphinganine,phytosphingosine,SM(d18∶0/16∶1(9z)) and arachidonic acid increased in model group compared with control group,while decreased in treatment group.Therefore,Liuwei Dihuang Pill may achieve the aim to treat acute kidney injury induced by gentamicin through adjusting the content of these biomarkers.This study provides a theoretical basis for Liuwei Dihuang Pill treating kidney injury in clinical practice.关键词：Liuwei Dihuang Pill;acute kidney injury;gentamicin;UPLC-MS;biomarker
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发布时间： - 摘要：In this study，a gold nanocrystal colloid was used as the enhancement factor for surface-enhanced Raman scattering(SERS).Raman spectra were transformed by continuous wavelet transform(CWT)，and Mexican hat wavelet were chosen as the wavelet basis.This procedure could be used to alleviate the influence of baseline variations and random noise，and find peak positions and the best scale wavelet coefficients of signal-Reverse search method was proposed to compare the spectrum of an unknown sample with a spectrum of standard using the information in wavelet space.Reverse match quality(RMQ)could be obtained automatically to determine whether a substance is present.It was used to identify colorants in a variety of food successfully.The colorants could be identified with 99 percent accuracy.It shows a better performance compared with traditional hit quality index(HQI).The study confirmed that the wavelet-based reverse search is feasible and accurate in qualitative analysis.关键词：continuous wavelet transform;reverse search;surface-enhanced Raman spectroscopy(SERS);rapid qualitative identification
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发布时间： - 摘要：The pretreatment conditions，including extraction solvent，derivatization time and temperature，as well as internal standard were optimized for metabolome analysis of Botrytis cinerea(B-cinerea)，an important pathogenic fungus that could induce a severe grey mold on plants.The results showed that，using salicin as the internal standard，a mixture of methanol and water(80∶20) with a dosage of 4.0 mL for 0.1 g of mycelium as extraction reagent，a silylation of N，O-bis(trimethylsilyl)trifluoroacetamide with methoxylamine for 6 h of derivation at 37 ℃ was the optimal for most kinds of metabolites in derivatives yield and stability.In B-cinerea hypha metabolome，210 peaks were detected by GC-MS， and the metabolome was identified as a group of metabolites including mainly amino acids，alcohols，organic acids，sugars and others.Among the metabolites，50 of them were identified by NIST 2008 with a match quality of 80% or more, and part of them by standards.As a result，typical 17 metabolites obtained good linearities in the range of 1.0-100 μg/mL with correlation coefficients more than 0.98.The limits of detection and limits of quantitation were in the range of 0.02-10.0 ng/mL and 0.1-34.0 ng/mL，respectively.Investigation on the reproducibility of the optimal method suggested that the RSD for 89.05% metabolites detected were in the range of 0.01%-16.8%.The good reproducibility implied that the method established was suitable for the metabolome detection of mycelial fungi,and could provide a good reference for microorganism metabolomics research in the field of agricultural and medical science.关键词：Botrytis cinerea;metabolomics;sample pretreatment;silylation
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发布时间： - 摘要：A method for the analysis of polybrominated diphenyl ethers(PBDEs) in urine of occupational worker was developed using QuEChERS(quick，easy，cheap，effective，rugged，safe) pretreatment coupled to gas chromatography-mass spectrometry(GC-MS).Urine sample was extracted with an acetone-hexane mixture by dehydration and salting-out using NaCl and anhydrous MgSO4.The purification was performed with C18 particlet,and GC-MS determination was perfomed under negative chemical ionization(NCI) mode.The calibration curves were linear in the ranges of 10-1 000 pg/μL for BDE-209，and 1-100 pg/μL for the rest of analytes，with correlation coefficients higher than 0.999 .The average recoveries were in the range of 91.7%-110.2% at three spiked levels，with relative standard deviations lower than 10%.The limits of detection(LOD) of PBDEs ranged from 0.3 pg/mL to 36 pg/mL.This method was validated to be simple，sensitive and selective，and was suitable for the exposure accessment of pollutant in occupational workers.关键词：polybrominated diphenyl ethers(PBDEs);urine;gas chromatography-mass spectrometry(GC-MS);occupational worker
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发布时间： - 摘要：A microRNA(miR，miRNA) electrochemical biosensor was proposed in the present research.Firstly，graphene(GN) was dispersed in the chitosan(Chi) solution to promote the conductivity of chitosan film.Then，prussian blue(PB) was in situ deposited on GN to obtain the PB@GN-Chi nanocomposite.The obtained nanocomposites were modified on the surface of electrode.Compared with the PB@GN-Chi prepared by ultrasonic method，the prepared composite could effectively prevent PB leaking into detection solution and display a prominent stability when modified on the electrode.The capture probe was subsequently modified by amino group and covalently linked to the modified electrode via glutaraldehyde.After blocked by hexanethiol，the miRNA biosensor was successfully prepared.The prepared PB@GN-Chi nanocomposite was observed with transmission electron microscope，and the electrochemical characteristics of the miRNA biosensor were investigated by cyclic voltammetry and differential pulse voltammetry.Under the optimal conditions，the biosensor displayed a linear relationship between current response and the logarithm of concentration of miR-21 in the range of 2.8-2.8×104 pmol/L.The detection limit was calculated to be 0.87 pmol/L.The prepared biosensor owns good stability and repeatability，and could be employed to detect miR-21 in human serum sample.关键词：electrochemical biosensor;prussian blue;graphene;nanocomposite;microRNA
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发布时间： - 摘要：A rapid analytical method was developed for the determination of saccharin sodium salt in dry fruits by surface-enhanced Raman spectroscopy(SERS).The saccharin in real samples was extracted with water, followed being separated and cleaned up on the activated C18 solid phase extraction column before surface-enhanced Raman scattering measurement.The linear range of this method was from 50.0 mg/L to 250 mg/L,and the detection limit was 0.6 g/kg.The good recoveries were in range of 80.0%-125% with relative standard deviations(RSD,n=5) no more than 8.4%.The results suggested that this method, with good anti-interference capability, was sensitive and reliable in the rapid determinattion of saccharin sodium salt in dry fruits.It is expected that this SERS based rapid analytical method possesses a great potential in monitoring the quality of dry fruits.关键词：SERS;rapid analysis;saccharin sodium salt;dry fruits
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发布时间： - 摘要：A study was conducted to assess the application of differential scanning calorimetry(DSC) in identification of the proportion of sunflower oil as an adulterant in extra virgin olive oils.A method of cooling program was proposed based on the repeatability and reliability of the oils tests which were started with the up-down temperature recycling in the olive oils.The cooling program method was used to measure the crystallization peak temperatures of eight extra virgin olive oils and other six edible oils together with five proportions of simulated adulterated oils.The regression equations were established according to the crystallization peak temperatures in the system.The results showed that the extra virgin olive oils had sharp crystallization peaks between-60 ℃ and-46 ℃compared with other six edible oils.The crystallization temperatures of the simulative adulterate extra virgin olive oils became lower,and the crystallization peaks became wider and shorter with the increase of mixing ratio of sunflower oil.The adulterated extra virgin olive oils could be identified rapidly and accurately with the regression equations.关键词：differential scanning calorimetry(DSC);extra virgin olive oils;identifications of the adulterate oils;regression equations
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发布时间： - 摘要：Combined with molecular docking model,quenching fluorescence,synchronous fluorescence,tridimensional fluorescence and UV-Vis absorption spectroscopy were applied to investigate the interactions of 4-methoxy-N-［4-(3-morpholin-4-yl-propoxy)-phenyl］-3-(4-pyridin-3-yl-pyrimidin-2-ylamino)-benzamide(1z) and human serum albumin(HSA) under simulative physiological conditions(pH 7.4) at the temperature of 298 K and 310 K,and the interaction mechanism was studied.The results showed that the quenching of 1z to HSA is probably a static process,and the conformation of HSA altered with the addition of 1z.The combination of theoretical research and experimental result provides a basis for studying the action mechanism of protein with drug,which further provides a certain experimental basis for study of small molecules of drugs in treatment of chronic myeloid leukemia.关键词：1z;HSA;interaction;fluorescence spectrum;molecular docking;UV-Vis absorption spectroscopy
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发布时间： - 摘要：A high performance liquid chromatographic(HPLC) method was developed for the determination of tranexamic acid(TA) in toothpaste.Sample was extracted with methanol, and the extract was evaporated to dryness under nitrogen before it was derived with dansyl chloride.Chromatographic separation was performed on an X-Bridge C18(250 mm×4.6 mm×5 μm) column using 0.1% formic acid-acetonitrile mixture aqueous solution as mobile phase.The ultraviolet detection wavelength was set at 250 nm.Effects of pH value of buffer solution，reaction temperature and time were investigated.Under the optimized experimental conditions，the TA derivative was successfully separated from the other impurities, and showed a good linearity in the range of 1-425 mg/L with a correlation coefficient(r) of 0.999 5.At three spiked concentrations of 20，200，1 600 mg/kg，the recoveries ranged from 98.7% to 102% with relative standard deviations(RSDs) of 0.85%-2.5%.The limit of detection for this method was 2.0 mg/kg.With the advantages of accuracy，reliability and high sensitivity，this method was suitable for the determination of tranexamic acid in different kinds of toothpaste.关键词：tranexamic acid(TA);dansyl chloride;toothpaste;high performance liquid chromatography(HPLC)
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发布时间： - 摘要：An analytical method was developed for the determination of 8 pyrethroid pesticide residues in nuts(hawaii nuts，pigeon nuts，almonds imported from ASEAN).The samples were extracted with acetonitrile by ultrasonic technique，purified with Alumina-N SPE and Florisil SPE.The components were separated with two different polarity capillary columns，and 8 kinds of pyrethroid pesticide residues were detected by GC with ECD detector.The linear range of the method was in the range of 0.01-1.0 μg/mL(r=0.999 2-0.999 9).The recoveries at three spiked concentrations of 10，20，50 μg/kg were in the range of 71%-115%，with relative standard deviations(RSD) of 4.5%-9.8%.The limits of detection(LOD，S/N=3) were in the range of 0.014-0.28 μg/kg.The limits of quantitation(LOQ，S/N=10) were in the range of 0.047-0.94 μg/kg.The established method has the advantages of good separation，high accurancy，high recovery， convenience and rapidness，and could be used for the routine analysis of pesticide residues in nuts.关键词：gas chromatography(GC);pyrethroid pesticide;Hawaii nuts;pigeon nuts;almonds
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发布时间： - 摘要：A high performance liquid chromatographic(HPLC) method was developed for the rapid determination of five synthetic sweeteners，including acesulfame K(AK)，saccharin sodium(SA)，aspartame(ASP)，alitame(ALT) and neotame(NTM) in white spirit，mixed liquor and wine.The HPLC separation was carried out on a C18 column.Several parameters，including the composition and gradient elution program of the mobile phase，column temperature and optimum detection wavelength of diode array detector(DAD) were optimized for improving the chromatographic performance and the sensitivity of determination.The results demonstrated that the separation could be completed within 15 min by gradient elution with acetonitrile and 0.02 mol/L ammonium sulfate solution(pH 4.4) as mobile phase.The column temperature was set at 40 ℃.The calibration curves of five synthetic sweeteners were linear in the range of 4-200 mg/L with correlation coefficients more than 0.999.The recoveries were in the range of 95.2%-103.2%，with relative standard deviations(n=5) not more than 3.4%.The experimental results indicated that the established method was simple，efficient and sensitive，and was suitable for the determination of five synthetic sweeteners in white spirit，mixed liquor and wine.关键词：HPLC/DAD;artificial sweeteners;white spirit;mixed liquor;wine
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发布时间： - 摘要：A Fourier transform ion cyclotron resonance mass spectrometry combined with electrospray ionization source(ESI FT-ICR MS) method was applied to detect the groundwater.Benefitted from the high precision molecular weight，three categories of Oxand N1Ox and N2Ox were identified，which are composed of a total of 27 heteroatomic compounds classes.Ox are dominant in these classes that nitrogen compounds combining with several O atoms are widely existed.Depending on the distribution pattern of equivalent double bond(DBE) and carbon number of heteroatomic compounds，large amounts of carboxyl were found to be present in Ox and nitrogen compounds were speculated to be derived from Ox.This work has broadened the understanding of soluble organic matter in groundwater and laid a foundation for the further research on its molecular structure.关键词：ground water;ESI FT-ICR MS;dissolved organic matter;molecular composition
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发布时间： - 摘要：A molecularly imprinted photocurrent chemical sensor was fabricated by using TiO2 film for the detection of carbofuran.Effect of doping modification on photocatalytic efficiency of TiO2 was studied.The results showed that the molecularly imprinted membrane of Au doped TiO2 had a good detection effect on the template molecule carbofuran.The experimental conditions such as film thickness and adsorption time were optimized.The experimental results showed that the concentrations of carbofuran had a good liner relationship with photocurrent in the range of 1.00×10-9-2.20×10-7 mol/L under the optimal experimental conditions，and the detection limit(S/N=3) was 1.10×10-10 mol/L.The sensor has demonstrated outstanding features such as excellent sensitivity，selectivity and stability.The determination of carbofuran in water was carried out by using the sensor，and the recoveries were in the range of 98.7%-104.0%.关键词：molecularly imprinted;carbofuran;titanium dioxide;photocurrent;sensor
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发布时间： - 摘要：A rapid method was established for the determination of clopidol in chicken by gas chromatography-tandem mass spectrometry(GC-MS/MS).Samples were extracted with acetonitrile-water.The extract was frozen to remove the lipid within,and derivated with propionic anhydride.Then,it was analyzed by GC-MS/MS under MRM mode.The calibration curve for clopidol was linear in the concentration range of 0.5-40 ng/mL with a correlation coefficient of 0.999 4.The limit of quantitation for this method was 5.0 μg/kg.The average recoveries at spiked concentrations of 5.0,10,20 μg/kg ranged from 101.5% to 111.8%,with relative standard deviations less than 7.7%.The method is simple,quick and high sensitive,and could be applied to detect clopidol residues in real samples.关键词：clopidol;gas chromatography-tandem mass spectrometry(GC-MS/MS);chicken
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发布时间： - 摘要：A proton-nuclear magnetic resonance(1H-NMR) method was established for the determination of polysaccharide content in mannatide using potassium acid phthalate as the internal standard.Effects of some experiment parameters were investigated.The optimal conditions were selected as follows:relaxation delay time(d1):1 s；transient number(ns):16.The results indicated that,under the optimal conditions,the good precision and repeatability for the method were obtained.The polysaccharide content in mannatide, determined by the 1H-NMR method with inner standard model,was similar to that of the ultraviolet spectrophotometry method.The established method was simple,specific and repeatable.Therefore,it could be used not only for the determination of polysaccharide content in mannatide,but also for detection of other kinds of polysaccharide with definite structures.关键词：1H nuclear magnetic resonance;polysaccharide content;mannatide
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发布时间： - 摘要：Based on the Safety and Technical Standards for Cosmetics(2015),a staticheadspace/gas chromatography-mass spectrometric(SHS/GC-MS) method was established to analyze 22 volatile organic compounds(VOCs) residues,including dichloromethane,cis-1，2-dichloroethene,trans-1，2-dichloroethylene,2-chloro-1，3-butadiene,trichloromethane,1，2-dichloroethane,benzene,carbon tetrachloride,trichloroethylene,methylbenzene,tetrachloroethylene,chlorobenzene,ethylbenzene,tribromomethane,m-xylene,p-xylene,phenylethylene,o-xylene,isopropylbenzene,1，4-dichlorobenzene,1，2-dichlorobenzene and hexachlorobutadiene in cosmetics.The experimental conditions for SHS/GC-MS,such as headspace conditions,analytical conditions of GC,quantitative ion’s selection and concentration of the samples were optimizedThe cosmetic samples were extracted and cleaned up by headspace at 80 ℃ for 30 min,determined and quantified by MS.22 kinds of VOCs had good linear relations in the range of 0.5-50 ng/mL with correlation coefficients higher than 0.99.The spiked recoveries ranged from 80.3% to 102.7%,with relative standard deviations(RSD) of 6.4%-9.9%.The limits of detection were in the range of 0.2-5.0 ng/g.This method had the advantages of simplicity,sensitivvity,accurancy, good reproducibility and stability,and was suitable for the screening and analysis of VOCs residues in cosmetics.关键词：static headspace;gas chromatography-mass spectrometry(GC-MS);cosmetics;volatile organic compounds(VOCs);determination
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发布时间： - 摘要：A rapid detection method of surface enhanced Raman spectroscopy(SERS) was established for the detection of ciprofloxacin (CIP) residues in duck meat.UV-visible absorption spectrum of SERS enhanced substrate and the feasibility of SERS detection of CIP residues in duck meat were analyzed.The addition amount of gold colloid， addition amount of duck meat extract containing CIP，addition amount of sodium chloride solution and the adsorption time were optimized by the single factor analysis.The calibration curve for the method was obtained in the optimum experiment condition.The determination coefficient was 0.987 9.The average recoveries of CIP in the prediction samples were between 97.0% and 111.7%.The experiment results indicated that the SERS method was feasible for the detection of CIP residues in duck meat.关键词：ciprofloxacin(CIP);surface enhanced Raman spectroscopy(SERS);duck meat;detection
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