最新刊期
卷 39 ， 期 9 ， 2020
- 摘要：A kind of nitrogen doped carbon quantum dots(N-CQDs),with economy,low toxicity and even strong fluorescence performance,were successfully synthesized by hydrothermal method using L citrulline and urea as precursors.The performance of N-CQDs was characterized by transmission electron microscopy(TEM),Fourier transform infrared spectroscopy(FT-IR) and X-ray photoelectron spectroscopy(XPS),etc.Results showed that the quantum yield of the N-CQDs reached up to 39.2% with an average particle size of 2.8 nm,which could be used for HepG2 cell imaging in view of their good water solubility,stability and biocompatibility.In addition,a fluorescence probe with high selectivity and sensitivity was proposed for the detection of o-nitrophenol(o-NP) based on an experimental phenomenon that the fluorescence of the CQDs could be specifically quenched by o-NP.Results showed that there was a good linear relationship for o-NP in the range of 0.083 3-12.0 μmol/L with a correlation coefficient(r2) of 0.998 and a detection limit(LOD) of 25.2 nmol/L(S/N=3).The proposed method was successfully applied in the detection of o-NP in real water samples from Wanfeng Lake and Dingxiao River in Guizhou province.关键词：nitrogen doped carbon quantum dots;cellular imaging;hydrothermal method;o-nitrophenol(o-NP);water;fluorescence quenching
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发布时间：2023-04-18 - 摘要：A method based on surface enhanced Raman spectroscopy(SERS) was established for the detection of sufentanil in water and urine in this paper.Meanwhile,a silver colloid substrate for SERS was prepared and characterized,and the Raman characteristic peaks of sufentanil were assigned by theoretical calculation and experimental comparison.The optimum experimental conditions were investigated,and the coagulant and its concentration were determined.SERS detection on sufentanil in water and artificial urine was performed,with the detection limits of 0.09 μg/mL and 1.55 μg/mL,respectively.There existed good linear relationships for the characteristic peak(1 004 cm-1) intensities of sufentanil in water and urine in a certain mass concentration range,with their correlation coefficient(r2) of 0.979 and 0.968,respectively.The recoveries for the analytes were in the ranges of 96.3%-107% and 95.8%-106%,with their relative standard deviations of 4.2%-4.7% and 3.3%-5.2%,respectively.The developed method is rapid,accurate,non-destructive and user friendly,and it lays a good foundation for the rapid detection of sufentanil in water and urine.关键词：surface enhanced Raman spectroscopy(SERS);sufentanil;silver colloid;rapid detection;water;urine
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发布时间：2023-04-18 - 摘要：An ultra high performance liquid chromatography-orbitrap high resolution mass spectrometry(UHPLC-Orbitrap HRMS) was used for the determination of N-nitrosodimethylamine(NDMA) in famotidine and its preparations.The samples were extracted with methanol,followed by vortex mixing,constant temperature shaking,high speed centrifugation and microfiltration,and finally analyzed by liquid chromatography-mass spectrometry(LC-MS).The chromatographic separation was performed on an ACE EXCEL 3 C18-AR(150 mm×4.6 mm,3 μm) column at 30 ℃ by gradient elution,with water and acetonitrile both contained 0.1% formic acid as mobile phases at a flow rate of 0.50 mL/min.The temperature of the autosampler was set at 4 ℃,and the mass spectrometer was protected with a valve switching apparatus.The MS analysis was performed with ESI ion source in positive ion parallel reaction monitoring(PRM) scanning mode,and the quantitation was achieved by the external standard method.Results showed that there was a good linear relationships for NDMA in the concentration range of 1.00-100.00 ng/mL with correlation coefficient(r) of 0.999 7.The limit of detection and limit of quantitation were 0.20 ng/mL and 1.00 ng/mL,respectively.The mean recoveries of NDMA from spiked famotidine and its preparations ranged from 98.5% to 108% with relative standard deviations(RSD) of 2.3%-6.7%.The method was then applied to the determination of NDMA in famotidine and its preparations.Among 47 batches of samples,NDMA was detected in 1 batch of famotidine and 2 batches of famotidine preparations,which contents exceeded the limit requirement.This method is sensitive,accurate and easy to operate,and could be used for the determination of NDMA in famotidine and its preparations.关键词：N-nitrosodimethylamine;famotidine;ultra-high performance liquid chromatography;orbitrap;high resolution mass spectrometry;genotoxicity
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发布时间：2023-04-18 - 摘要：An analytical method was established for the determination of 10 illegally adulterated androgen drugs in health foods by high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry(HPLC-Q-TOF MS).The samples were extracted by ultrasonic cleaning or liquid-liquid extraction.10 androgen drugs were separated on a C18 column(3.0 mm×150 mm,1.8 μm) by gradient elution with 0.1%(by volume) formic acid containing 10 mmol/L ammonium acetate and 0.1% formic acid acetonitrile,and determined by HPLC-Q-TOF MS.A data base of the accurate molecular mass and a library containing the 10 androgen drugs were established.An automatic retrieval towards the detected results was carried on according to the characteristics of the compound,such as accurate mass,retention time,isotopic ratio and MS/MS spectrum in order to carry out a rapid qualitative analysis.Results showed that 10 androgen drugs had good linear relationships in the concentration range of 2-500 ng/mL with correlation coefficients(r2) greater than 0.999.The limits of detection(LOD) for 10 androgen drugs in three kinds of matrixes were in the range of 0.01-0.06 mg/kg,while the limits of quantitation(LOQ) were 0.03-0.2 mg/kg.The average recoveries for 10 androgen drugs ranged from 74.3% to 113% with relative standard deviations(RSD) of 1.2%-7.7%.Using library search function to rapid screen, which is efficient,sensitive and accurate，the method is suitable for rapid screening of 10 illegally adulterated androgen drugs in health foods.关键词：high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry;androgen drugs;rapid screening;health food
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发布时间：2023-04-18 - 摘要：he composition of coal pitch is extremely complex,which contains polycyclic aromatic hydrocarbons with large molecular weight and their oxidation products.The coal pitch obtained from different coal raw material sources and production processes vary greatly in terms of aromatization degree,composition,property,molecular structure,etc.In this paper,gas chromatography mass spectrometry(GC-MS),pyrolysis/gas chromatography mass spectrometry(Py/GC-MS) and high performance liquid chromatography(HPLC) were used to develop a universal,stable and simple analytical method for the construction of coal asphalt fingerprint library.In the development of GC-MS method,the HP-5MS column was used,and the method was established under a linear temperature gradient.A chromatogram for 33 components was obtain by this method,which had good stability for different samples.The Py/GC-MS method was used to investigate the changes in component structure and composition at higher temperatures,which may be used for a reference for the processing and aging research of asphalt products.In the development of the HPLC method,the most commonly used C18 column reversed phase chromatographic separation mode was adopted,which was established with methanol and water as mobile phases under linear gradient conditions.The developed method could be used to obtain stable chromatographic peaks for 41 components in different samples.Based on the methods above,a fingerprint spectrum library for coal pitch could be established,which provides theoretical basis data for further improving the evaluation on coal pitch and developing new uses of coal pitch.关键词：coal tar pitch;fingerprint;gas chromatography-mass spectrometry(GC-MS);pyrolysis;high-performance liquid chromatography(HPLC)
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发布时间：2023-04-18 - 摘要：An ultra high performance liquid chromatographic(UPLC) method was developed for the simultaneous determination of seven water soluble fluorescent whitening agents in medicinal composite films.The sample was extracted with 40% acetonitrile aqueous solution adjusted to pH 11.0 with triethylamine,and separated on a Waters ACQUITY UPLC BEH C18(100 mm×2.1 mm,1.7 μm) at 40 ℃ by gradient elution with acetonitrile-methanol solution(2∶3) and 10 mmol/L tetrabutylammonium bromide-methanol solution(5∶95,pH 8.0) as mobile phases at a flow rate of 0.2 mL/min.The detection wavelength was set at 350 nm.Results showed that there were good linear relationships for the analytes in corresponding concentration ranges with their correlation coefficients(r) of 0.998 6-0.999 7.The limits of detection(LOD) and limits of quantitation(LOQ) of the method were in the ranges of 0.17-1.29 μg/mL and 0.55-3.85 μg/mL,respectively.The average recoveries at three spiked levels ranged from 83.2% to 110%,with relative standard deviations(RSD) of 4.0%-9.7%.The detection results showed that two kinds of fluorescent whitening agents were detected in the polyester/aluminum/polyethylene medicinal composite film and paper/aluminum/polyethylene medicinal composite films at most,no fluorescent whitening agent was detected in other varieties.The method is simple,reliable and repeatable,and could be used for the determination of fluorescent whitening agents in medicinal composite films.关键词：ultra high performance liquid chromatography(UPLC);medicinal composite films;water soluble;fluorescent whitening agents
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发布时间：2023-04-18 - 摘要：An ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) with dispersed solid phase extraction was established for the determination of 19 insecticides,fungicides and their metabolites in edible fungi,including mushrooms,black fungus and tremella,etc.The samples were firstly extracted with acetonitrile by homogeneous oscillation,then purified with PSA and C18,and finally separated on an XR-ODS column(2.0 mm×100 mm×2.2 μm) with acetonitrile and water as mobile phases.The analytes were detected under multi-reaction monitoring(MRM) mode,determined by retention time and ion abundance ratio of the fragments and quantified by the external standard method with matrix-matched standard curves.Under the optimized conditions,19 analytes showed good linearities(r2>0.998 0) in their respective concentration ranges.The limits of detection and limits of quantitation were in the ranges of 0.2-0.6 μg/kg and 0.5-2.0 μg/kg,respectively.Average recoveries for the analytes at three spiked levels ranged from 83.1% to 106% with relative standard deviations(RSD，n=6) of 5.0%-12%.The method was rapid,accurate and sensitive,and was suitable for the determination of insecticides,fungicides and their metabolites in edible fungi.关键词：ultra performance liquid chromatography-tandem mass spectrometry;edible fungi;pesticides;metabolites;dispersed solid phase extraction
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发布时间：2023-04-18 - 摘要：An ultra performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was established for the determination of 73 glucocorticoids in cosmetics．Samples were dispersed with saturated sodium chloride and ultrasonically extracted with acetonitrile,then purified with a PRiME HLB SPE column(60 mg/3 mL) and separated on a Waters Cortecs C18 column(150 mm×2.1 mm，2.7 μm) by gradient elution using 0.1% acetic acid solution and acetonitrile as mobile phases.The analysis was performed with electrospray ion source in positive ion mode under multi-reaction monitoring(MRM) mode,and the results were quantified by external standard method.Results showed that there were good linear relationships for 73 glucocorticoids in cosmetics in their respective concentration ranges with correlation coefficients(r) higher than 0.99.The limits of quantitation(LOQ) were in the range of 0.1-0.3 μg/g．The average recoveries for 73 glucocorticoids at three spiked levels of 1LOQ,2LOQ and 5LOQ ranged from 73.3% to 119%,with relative standard deviations(RSD) of 0.40%-18%.The method was rapid and accurate,and could be used as a screening approach for 73 glucocorticoids in cosmetics.关键词：cosmetics;glucocorticoids;ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)
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发布时间：2023-04-18 - 摘要：A high-performance liquid chromatography-tandem mass spectrometric(HPLC-MS/MS) method was developed for the rapid determination of five quaternary ammonium salts,e.g.benzyldimethyldodecyl ammonium chloride，benzyldimethyltetradecyl ammonium chloride,benzyldimethylhexadecyl ammonium chloride,dodecyltrimethyl ammonium chloride,and didecyldimethyl ammonium chloride,in frozen drinks.The samples were extracted twice with acetonitrile-ethyl acetate(1∶1，by volume),then frozen to degrease at-20 ℃.The extract was separated on a CAPCELL PAK CR(1∶20) column using acetonitrile-5 mmoL ammonium acetate containing 0.1% formic acid as mobile phase by gradient elution.The target analytes were detected in multiple-reaction monitoring(MRM) mode,and quantified by the matrix matched external standard method.Results showed that good linearities for the five quaternary ammonium salts existed in the mass concentration range of 0.5-50.0 μg/L,with their correlation coefficients(r) larger than 0.995.The limits of detection(LOD) and limits of quantitation(LOQ) were in the ranges of 0.3-1.5 μg/kg and 1.0-5.0 μg/kg,respectively.The average recoveries for the five analytes at three spiked levels of 5.0,10.0 and 50.0 μg/kg ranged from 80.3% to 114% with relative standard deviations(RSD) of 2.5%-83%.With the advantages of convenient operation,high sensitivity and good precision,this method is suitable for the determination of five quaternary ammonium salts in frozen drinks.关键词：quaternary ammonium;frozen drinks;high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)
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发布时间：2023-04-18 - 摘要：A matrix assisted laser desorption ionization-Fourier transform ion cyclotron resonance mass spectrometric(MALDI-FTICR-MS) method was developed for rapid determination of paraquat in whole blood and urine.The sample was extracted by liquid-liquid extraction method,with acetonitrile solution containing 1% formic acid as extraction solvent.Prior to analysis,the extracted solution was mixed with 2,5-dihydroxybenzoic acid.Results showed that there were good linear relationships for paraquat in whole blood and urine samples in the mass concentration range of 10-5 000 μg/L,with correlation coefficients(r) of 0.995 5-0.999 2.The limits of detections(LODs) and limits of quantitations(LOQs) of the method were in the ranges of 0.6-3.0 μg/L and 2.0-10 μg/L,respectively.The average recoveries at spiked levels ranged from 85.2% to 110%,with relative standard deviations(RSDs) of 0.40%-7.3%.The method showed the advantages of low sample and solvent consumption,simple operation,rapid analysis and high sensitivity,and could meet the requirements for rapid detection of clinical poisoning and forensic.关键词：paraquat;matrix assisted laser desorption ionization-Fourier transform ion cyclotron resonance mass spectrometry;whole blood;urine
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发布时间：2023-04-18 - 摘要：A proton nuclear magnetic resonance(1H NMR) combined with 1D total correlation spectroscopy(1D TOCSY) and quantitative nuclear magnetic resonance spectroscopy(qNMR) was developed for detection and quantitation of 1,2-propanediol in liquid milk.The proton signals of methyl of 1,2-propanediol(1H NMR) and the methylene and methyne of this molecule(1D-TOCSY) were used for rapid screening and precise detection of 1,2-propanediol in liquid milk,respectively.Meanwhile,the content of 1,2-propanediol in liquid milk was detected by the qNMR method,with the signal of 1,2-propanediol at δ 1.15 as quantitative peak and 2,2,3,3-D4-3-(trimethylsilyl) propionic acid sodium salt(TMSP) at δ 0.00 as internal standard peak.The detection limit and quantitation limit of the method were 0.002 mg/mL and 0.006 mg/mL,respectively.Comparison of this NMR and gas chromatography method revealed that they were equal within experimental error.Furthermore,the NMR method was simple in operation and had the high specificity,which not only improved the detection efficiency,but also avoided false positive results.It was suitable for batch and rapid detection of 1,2-propanediol in liquid milk.关键词：proton nuclear magnetic resonance(1H NMR);1D total correlation spectroscopy(1D TOCSY);quantitative nuclear magnetic resonance spectroscopy(qNMR);liquid milk;1,2-propanediol
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发布时间：2023-04-18 - 摘要：A high performance liquid chromatography with fluorescence detector was developed for the simultaneous determination of four benzoxazole fluorescent whitening agents,i.e.FWA 135,FWA 367,FWA 368 and FWA 184 in plastic children's toys.The sample was crushed and pretreated with 20 mL acetonitrile-chloroform(6∶4,by volume) mixed solution by one step solvent extraction,then ultrasonically extracted at 40 ℃ for 30 min,and finally analyzed by HPLC with fluorescence detection.The extract was separated on a Waters SunFire C18 column by gradient elution with acetonitrile and water as mobile phases.The fluorescence excitation wavelength(Ex) was set at 360 nm,and the emission wavelength(Em) was 430 nm.Results showed that the calibration curves were linear(r2≥0.999 3) in the range of 1-100 μg/L for FWA 135,and 2-200 μg/L for the other three fluorescent whitening agents.The detection limits for FWA 135,FWA 367,FWA 368 and FWA 184 were 0.5,1,1 and 1 μg/L,respectively.The recoveries for four fluorescent whitening agents at three spiked levels of 0.1,0.4 and 2.0 mg/kg ranged from 84.2% to 106%,with relative standard deviations less than 10%.Ten kinds of childrens toys were tested,and four kinds of benzoxazole fluorescent whitening agents were detected.With the advantages of simple operation,good recovery and high precision,the method is applicable for the determination of the fluorescent whitening agents in various types of children's toys.关键词：high performance liquid chromatography(HPLC);fluorescence detection;benzoxazoles;fluorescent whitening agents;children's toys
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发布时间：2023-04-18 - 摘要：The high accuracy mass number of fragmentation fragments(resolution>70 000,m/z 200) was obtained by quadrupole/electrostatic field orbitrap high resolution mass spectrometry(Q-Orbitrap-HRMS),and the element composition was obtained by element simulation,and then the fragmentation law for Sudan red Ⅰ,Ⅱ,Ⅲ and Ⅳ was investigated.Results showed that the existence of hydroxyl groups in molecular structure could easily be protonated to form ［M+H］+,and the cracking process occurs in the vicinity of azo groups:First,the presence of azo-conjugated o-phenol hydroxyl group(H group) leads to rearrangement of compound structure from enol to hydrazone,where H is transferred to N atom,and the high bond azo bond(—N‖N—) is rearranged to nitrogen single bond(—NH—N‖).Second,no migration occurs as the azo bond is ortho free for H,while the azo bond(—N‖N—) with high bond energy remains unchanged,and the fragment ions are formed by breaking the C—N bonds on both sides.Third,in high impact energy,there exist simultaneous cleavage of the chemical bond and open-loop cleavage of the ring-ring,and the fragment ions containing a plurality of azo groups are also richer.The best ionization mode and mass spectrum fragmentation law for the four Sudan Red dyes were determined by direct injection,which provided a basis for the rapid identification of such compounds.关键词：Sudan Red dyes;mass spectrum fragmentation law;quadrupole/electrostatic field orbitrap high resolution mass spectrometry(Q-Orbitrap-HRMS)
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发布时间：2023-04-18 - 摘要：A nano platinum/reduced graphene oxide modified glassy carbon electrode(Pt/E-rGO/GCE) was prepared by one step electrodeposition using a mixture of graphene oxide and chloroplatinic acid as the precursor.The electrochemical behavior of 1 hydroxypyrene on the modified electrode was studied,and a sensitive accumulation and detection of 1-hydroxypyrene was performed by differential pulse voltammetry.Results showed that the response current for 1-hydroxypyrene reached the maximum when the solution was set at pH 2.0 and the number of electrodeposition cycles was 5.The concentration of 1 hydroxypyrene showed a good relationship with the reduction peak current in the range of 50-700 nmol/L with a correlation coefficient(r) of 0.976 and a limit of detection(S/N=3) of 12.1 nmol/L.The Pt/E-rGO/GCE exhibited good stability,reproducibility and anti-interference ability,and was applied in the determination of 1-hydroxypyrene in human urine with recoveries of 99.7%-108%and relative standard deviations of 3.2%~4.2%.The good performance of the Pt/E-rGO/GCE provides a certain practical value for the construction of an electrochemical sensor.关键词：1-hydroxypyrene;nano platinum;reduction of graphene oxide;modified electrode;electrochemical sensor
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发布时间：2023-04-18 - 摘要：A micellar electrokinetic chromatography(MEKC) with multiwavelength switching was established for the simultaneous determination of vitamin B1,B2,B6,nicotinamide,calcium pantothenate and sodium benzoate in Five Vitamins Oral Solution.Factors affecting separation efficiency such as detection wavelength,concentration of sodium dodecyl sulfate(SDS),separation voltage of sample,pH value and concentration of background buffer were optimized．An optimal separation of six compounds was obtained on an uncoated fused silica capillary column(75 μm×50 cm,effective length 42 cm),with a background buffer composed of 40 mmol/L borax+40 mmol/L boric acid+20 mmol/L SDS(pH 9.0),at a separation voltage of 20 kV and a column temperature of 25 ℃.The detection wavelength was set at 270 nm for vitamin B1,B2,B6,nicotinamide and sodium benzoate,and 200 nm for calcium pantothenate.The sample was electrokinetically injected at 10 kV for 10 s.Results indicated that the six analytes could be separated within 13 min,while their calibration curves showed good linear relationships in the respective concentration ranges,with correlation coefficients(r) not less than 0.998 9.The average recoveries at three spiked levels ranged from 97.0% to 103%,with relative standard deviations(RSD) of 0.60%-1.8%.The method is rapid,accurate and reliable,and could be used for the determination of vitamin B1,B2,B6,nicotinamide,calcium pantothenate and sodium benzoate in Five Vitamins Oral Solution.关键词：micellar electrokinetic chromatography(MEKC);Five Vitamins Oral Solution;vitamin B1;vitamin B2;vitamin B6;nicotinamide;calcium pantothenate;sodium benzoate
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发布时间：2023-04-18 - 摘要：Food safety is closely related to people's health and life safety,and foodborne pathogenic bacteria is the main factor affecting food safety.Diseases and deaths caused by foodborne pathogenic bacteria continue to threaten global public health.Therefore,development of rapid,accurate and sensitive detection methods for foodborne pathogenic bacteria is the key to prevent foodborne disease outbreaks and ensure food safety.Current conventional detection methods are time consuming and labor intensive,which require expensive equipment and professional personnel,and limit their own applications.In recent years,with the rapid development of nanotechnology,nanoparticles have become a research hotspot in the field of foodborne pathogenic bacteria due to their unique physical and chemical properties such as small size,high specific surface area,high reactivity,etc.In addition,the specificity and sensitivity of detection could be improved by modifying the recognition element on the surface of nanoparticles and combining with novel analytical techniques.In this review,the applications of magnetic nanoparticles,noble metal nanoparticles,fluorescent nanoparticles and silica nanoparticles in the detection of foodborne pathogenic bacteria are mainly summarized and compared,aiming at providing a new idea for rapid detection of foodborne pathogenic bacteria.关键词：magnetic nanoparticles;noble metal nanoparticles;fluorescent nanoparticles;silica nanoparticles;foodborne pathogenic bacteria;detection
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发布时间：2023-04-18 - 摘要：Polysaccharides are one of the important active ingredients in traditional Chinese medicine,which have hypolipidemic,hypoglycemic,immune enhancing,anti tumor,antioxidant,anticoagulant,anti inflammatory,anti aging activities,etc.It has become a bottleneck for development of new polysaccharide medicines in traditional Chinese medicine as they contain the characteristics of strong polarity,large molecular weight and difficult to confirm for structure.The pretreatment and analysis methods for polysaccharides in traditional Chinese medicine are reviewed in this article,aiming to provide references for qualitative and quantitative analysis of polysaccharide components in traditional Chinese medicine,improvement of quality control,in depth development of polysaccharide medicines and comprehensive research on the substance basis of traditional Chinese medicine.关键词：traditional Chinese medicine;polysaccharide;pretreatment;analysis methods
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发布时间：2023-04-18 - 摘要：Thermoanalytical coupling technique is a kind of method which combines thermoanalytical technique with different detection means,in order to research exactly the characteristics of structure,composition,thermal reaction,etc.of materials and reveal the nature of materials thermodecomposition,especially in the process of the variation of mass and heat and the ingredient of thermodecomposition of metallic materials.In this paper,thermoanalytical technique coupled with several kinds of analytical methods such as differential thermal analysis,differential scanning calorimetry,Fourier infrared spectroscopy and mass spectrometry were emphatically introduced.Taking the research of metallic materials for example,the applications of thermoanalytical coupling technique in the structure and properties of metal materials were described in detail,and the application prospect of thermoanalytical coupling technique was outlooked.关键词：thermogravimetric analysis;coupling technique;metal materials;characterization of properties
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发布时间：2023-04-18
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