摘要:In order to enable food production enterprises to conduct more efficient and convenient daily monitoring of foodborne pathogens in the production environment,this study developed a rapid detection technology for Listeria monocytogenes based on recombinase polymerase amplification(RPA)-lateral flow strip technology,and analyzed the specificity,sensitivity,and detection limit of the method. The sensitivity of the lateral flow strip detection was 6.5×102 CFU/mL after 15 min of RPA amplification. The detection limit was 1 CFU/mL after 8 hours of enrichment of artificially contaminated samples. The rapid detection method for Listeria monocytogenes established in this study does not require the assistance of large experimental equipment,and can be completed within 20 minutes after simple training for testing personnel,providing good technical support for enterprises to monitor Listeria monocytogenes in the production environment from the source,and also promoting the improvement of food safety quality control levels in the entire industry.
摘要:In this study,the conductive metal-organic framework(Cu3(HITP)2) nanosheet structures were successfully growth on titanium carbide(MXene) via wet etching and in situ growth methods. Au nanoparticles(Au NPs) were modified on the surface of Cu3(HITP)2-MXene nanocomposites using a chemical reduction technique. The morphology and elemental composition of the synthesized samples were systematically characterized through scanning electron microscopy(SEM) and X-ray photoelectron spectroscopy(XPS). The electrochemical performances of the as-developed Au NPs@Cu3(HITP)2-MXene immunosensor were investigated by cyclic voltammetry(CV),electrochemical impedance spectroscopy(EIS) and differential pulse voltammetry(DPV). The obtained results demonstrated that the electrochemical immunosensor displays a linear range from 100 fg/mL to 10 μg/mL with a low detection limit of 35 fg/mL,as well as excellent selectivity and stability toward alpha-fetoprotein(AFP). As results,the as-proposed electrochemical immunosensor based on Au NPs@Cu3(HITP)2-MXene nanocomposites exhibits highly performances toward AFP detection,which is potential for the application for the analysis of human serum sample.
关键词:electrochemical immunosensor;conductive metal organic framework;titanium carbide;Au nanoparticles;alpha-fetoprotein
摘要:The objective of this study was to develop a rapid and straightforward visual colorimetric detection method for Mn2+. A V4+-incorporated V2O5/NC composite nanozyme(V4+-V2O5/NC,where NC represents nitrogen-doped carbon material) was successfully synthesized via a calcination process. The morphology,composition,and structure of the as-fabricated V4+-V2O5/NC were characterized and analyzed in detail. This nanomaterial exhibited a rich porous structure and remarkable peroxidase-like activity(POD). Notably,the presence of V4+ significantly enhances the catalytic activity of V2O5/NC,promoting the generation of superoxide radicals(·O2-) from H2O2,which subsequently oxidizes the colorless 3,3',5,5'-tetramethylbenzidine(TMB) into blue oxidized TMB(oxTMB). The introduction of Mn2+ into the chromogenic system triggered complexation to convert the solution from blue to colorless. Leveraging this phenomenon,we developed a visual colorimetric detection method for Mn2+ that offered high selectivity and sensitivity. A satisfactory linearity existed between Mn2+ concentration and 652 nm absorbance with a linear range of 0.01-50 µmol/L and a detection limit of 3.3 nmol/L. This colorimetric approach is both simple and cost-effective,thereby providing a viable and reliable solution for rapid Mn2+ detection.
摘要:Oil painting is a key medium in contemporary Chinese art,with complex materials that are prone to aging,and many kinds of diseases. The introduction of modern synthetic materials in the 20th century has significantly impacted these works. This study focuses on Huang Shaojing's representative work of early realism“Grandfather”,which is in the collection of the Anhui Museum,it employs employing a range of scientific analysis methods,including stereomicroscopy,scanning electron microscopy-energy dispersive spectroscopy(SEM-EDS),infrared spectroscopy(FT-IR),X-ray diffraction microanalysis(μ-XRD),micro-Raman spectroscopy(μ-Raman),pyrolysis/gas chromatography-mass spectrometry(Py/GC-MS),and thermally assisted hydrolysis and methylation/gas chromatography-mass spectrometry(THM-Py/GC-MS) to study the structure and material composition of micro-samples from the painting. The results show that the selected micro-sample analysis techniques can effectively and maximally uncover the latent information contained within the samples. The study shows that the oil painting sample consists of four layers:the ground layer uses zinc white as the inorganic filler;the underpainting and pigment layers contain synthetic organic pigments,with the yellow being Monoazo-PY3 and the blue being Phthalocyanine-PB15∶6. The binding agents was polyvinyl acetate and linseed oil,and acrylic monomer and styrene were used as the main modified materials,with dibutyl phthalate and diisobutyl phthalate used as plasticizers,polyvinyl alcohol serves as a protective colloid and thickener,trimethyl phosphate as an antifoaming agent,and zirconium oxychloride or zirconium oxide as a drier to modify and enhance the overall performance of the oil painting materials after film formation. The surface varnish layer consists of a hard resin varnish made from rosin dissolved in linseed oil. This research provides a scientific basis for the identification,restoration,and conservation of components(such as pigments,binders,and additives) in modern and contemporary oil paintings.
关键词:oil painting;Huang Shaojing;micro-area analysis;Py/GC-MS;comprehensive research
摘要:The extraction process of Guizhi prescription was optimized by analytic hierarchy process-criteria importance through intercriteria correlation hybrid weighting method(AHP-CRITIC) and backpropagation artificial neural network(BP-ANN). The weight coefficients determined by the AHP-CRITIC method for ginsenoside Rg1,ginsenoside Re,ginsenoside Rb1,tenuifolin,paeoniflorin,ferulic acid and extract yield were 0.190 7,0.217 5,0.234 1,0.089 4,0.119 5,0.087 5,and 0.061 3,respectively. The optimal extraction process was as follows:10 times the solvent volume,2 hours per extraction,and 3 extraction cycles. The network prediction results of BP-ANN test samples were consistent with the orthogonal test results. In addition,AHP-CRITIC and BP-ANN integrating analysis suggested that the extraction efficacy of another extraction process(10 times the solvent volume,1 hour per extraction,and 2 extraction cycles) showed no statistically significant difference with the optimal extraction process,thus the energy conserved extraction process is more suitable for the large-scale production. This study provides a reference for the further development and large-scale production of Guizhi prescription,moreover,it builds a reliable methodology basis for modernizing extraction process method of traditional Chinese medicines.
摘要:By comprehensively applying modern analytical methods,taking the extract yield,the content of CaCO3,the transfer rate of CaCO3,as well as simultaneous thermal analysis(TG-DSC),Fourier transform infrared spectroscopy(FTIR),and high performance liquid chromatography(HPLC) fingerprints as key quality attributes,this study reveals the“quantity-quality”transfer rules of Ostreae concha,calcined slices of Ostreae concha,and the standard decoction of calcined Ostreae concha,providing a reference for their quality control. Fifteen batches of Ostreae concha medicinal materials were selected as raw materials to prepare the calcined slices of Ostreae concha and the standard decoction of calcined Ostreae concha. The extract yield of the standard decoction of calcined Ostreae concha was calculated. The complexometric titration method was used to determine the CaCO3 content of the three,and the transfer rate of CaCO₃ from the calcined slices of Ostreae concha to the standard decoction was calculated. TG-DSC was used to study the thermal decomposition characteristics and thermal effect characteristics of the three,and TG-DSC fingerprints were constructed. FTIR was used to establish FTIR fingerprints to analyze the dynamic changes of chemical groups in the three. HPLC was used to determine the amino acid components of the three,and HPLC fingerprints were constructed,and similarity evaluation was carried out. At the same time,combined with principal component analysis(PCA) and partial least squares-discriminant analysis(PLS-DA),the similarities and differences among the three in terms of FTIR characteristics and amino acid components were explored. The results showed that the CaCO3 contents of 15 batches of Ostreae concha,calcined slices of Ostreae concha,and the standard decoction of calcined Ostreae concha were 94.68%-97.79%,96.53%-98.41%,and 81.86%-90.21%,respectively. The extract yield of the standard decoction of calcined Ostreae concha was 2.78%-4.94%,and the transfer rate of CaCO3 from the calcined slices of Ostreae concha to the standard decoction was 2.54%-4.42%. The results of TG-DSC showed that the organic components and CaCO3 in Ostreae concha,the calcined slices of Ostreae concha and the standard decoction of calcined Ostreae concha decomposed within the temperature ranges of 30-580 ℃ and 580-800 ℃ respectively. Compared with Ostreae concha and the calcined slices of Ostreae concha,the endothermic peak of CaCO3 in the standard decoction of calcined Ostreae concha appeared earlier,and its thermal stability decreased significantly. The FTIR results showed that the main component of the three was calcite-type CaCO3. The main groups in Ostreae concha were O—H,C=O,and CO32- groups,and the C=O group was not observed after calcination. The HPLC results showed that the average similarity of the established fingerprints was all above 0.9,and 14 amino acid components could be effectively transferred. In addition,the multivariate statistical analysis method could effectively distinguish the three,and 7 FTIR differential bands and 3 amino acid differential components were screened out. The method established in this study can be used for the quality control of the whole process of the standard decoction of calcined Ostreae concha.
摘要:In this paper,using tetraethyl orthosilicate(TEOS) as raw material,hexadecyl trimethyl ammonium chloride(CTAC) as porosity agent,flower-like spherical mesoporous silica nanoparticles was prepared by a soft template method,and using hippuric acid(HA) as a template molecule,3-aminopropyltriethoxysilane(ATPES) as a functional monomer and TEOS as a cross-linking agent,a molecular imprinted polymers(FSMSNs@MIPs) of HA with specific recognition were prepared on the surface of FSMSNs. The FSMSNs@MIPs nanoparticles were characterized using Fourier transform infrared spectroscopy(FT-IR),transmission electron microscopy(TEM),dynamic light scattering(DLS) and X-ray photoelectron spectroscopy(XPS). The adsorption performance of the prepared FSMSNs@MIPs was investigated,and the adsorption mechanism was discussed with the adsorption models such as Langmuir model and quasi-second-order dynamics model. The results showed that FSMSNs@MIPs had high selectivity and good stability for HA,and the maximum adsorption capacity was 85.32 mg/g. The adsorption process belonged to surface single molecular layer chemisorption. FSMSNs@MIPs were used as solid-phase extraction(SPE) packing materials to prepare molecularly imprinted solid-phase extraction packed columns. The solid-phase extraction conditions were optimized for the adsorption separation and determination of HA in fresh milk by combining with high performance liquid chromatography(HPLC) with spiked recoveries ranging from 92.1%-99.3%,and RSD≤3.6%. The imprinted material showed good specific recognition ability to HA.
摘要:This study investigated the in vitro antioxidant activity and analytical methods of thiosulfinate compounds in garlic,elucidating the relationship between antioxidant components and their structural characteristics. The antioxidant capacity of freeze-dried garlic powder and alliin extract was evaluated through 1,1-diphenyl-2-picryl-hydrazyl radical(DPPH) and 2,2'-azinobis(3-ethylbenzothiazoline-6-sulfonic acid) diammonium salt (ABTS) radical scavenging assays. The results demonstrated that thiosulfinates generated via enzymatic reactions exhibited significantly higher scavenging rates against DPPH and ABTS radicals compared to deactivated enzyme and non-enzymatic systems (p<0.01). UPLC-MS/MS and HPLC analysis identified four thiosulfinate products:dimethyl thiosulfinate,allicin,methyl allyl thiosulfinate,and allyl methyl thiosulfinate. Combined with thin-layer chromatography-bioautography,allicin,methyl allyl thiosulfinate,and allyl methyl thiosulfinate were identified as the primary antioxidant components. The 5,5'-dithiobis(2-nitrobenzoic acid) (DTNB) method was employed to determine the potential total thiosulfinate content,which showed a positive correlation with the antioxidant activity of the test samples and was directly related to the content of the precursor alliin. This study established a comprehensive research framework for investigating the “component-activity”relationship of thiosulfinates,providing theoretical foundations and innovative directions for the development of natural antioxidants and strategies for preventing and treating oxidative stress-related diseases.
摘要:The gas chromatography-ion mobility spectrometry(GC-IMS) technology was employed to analyze the differences in volatile components of Dracocephalum heterophyllum Benth. subjected to different drying methods. Based on the compositional characteristics,a method was established for distinguishing samples treated by different drying. The sample was handled by natural shade,hot air drying and vacuum freeze drying. A total of 72 volatile components in the plants were analyzed by GC-IMS. The difference map of volatile components was constructed,and the principal component analysis was conducted. The results showed that compared with fresh plants,the types and contents of volatile substances in Dracocephalum heterophyllum Benth. after being dried were both increased,and there exist significant differences among different drying methods. The types and contents of volatile components in natural dried samples were the most abundant,followed by hot air dried samples,and the types and contents of volatile components in vacuum freeze dried samples were lowest. Among several drying methods,natural shade drying is the most suitable for the drying of fresh samples of Dracocephalum heterophyllum Benth.. The method exhibited the advantages of high efficiency,non-destructiveness and simple sample processing. This research could provide a certain reference for the subsequent quality evaluation and processing of Dracocephalum heterophyllum Benth..
摘要:This study aims to address the growing problem of adulteration in the global fragrant rice market by establishing a non-targeted metabolomic model for distinguishing jasmine rice from non-fragrant rice. Liquid chromatography-high-resolution mass spectrometry was used to analyze the metabolomic profiles of Thai Hom Mali Rice and Chinese non-fragrant indica rice. Key differential metabolites such as 4-hydroxy-3,5-dimethoxy cinnamic acid,caffeic acid,L-tyrosine,indole,and 4-hydroxyquinoline were identified through the Mann-Whitney U test,heat map analysis,and principal component analysis(PCA). A discrimination model based on the random forest algorithm was developed,achieving 100% accuracy in both the modeling and testing groups,and 95% accuracy in real samples. This research offers a valuable technical solution for ensuring fragrant rice quality,regulating the market,and protecting consumer rights.
关键词:Thai Hom Mali Rice;authentication;non-targeted metabolomics;random forest algorith;mass spectrometry
ZHAO Yun-xia, LI Zi-ying, CHEN Xin, ZHANG Yu-xin, XIAO Wei-min, LIU Ai-ping, LI Mei-fang, JIN Yi-bao, DU Qing-ping, WANG Qi, SU Jia-ting, YANG Guo-wu, FANG Wen
摘要:This study developed a method for the determination of 37 amino acids in serum using liquid chromatography-tandem mass spectrometry(LC-MS/MS). Serum sample was treated with 10% sulfosalicylic acid to achieve protein precipitation. The sepernatant was chromatographically separated using a Phenomenex Kinetex F5(250 mm×4.6 mm,5 μm) column with a gradient elution consisting of 0.02% formic acid-acetonitrile,and detected under electrospray ion source positive ion(ESI) and multiple reaction monitoring(MRM) mode. The results showed that the developed method exhibited good sensitivity and linearity for the selected 37 amino acids within the concentration range from the limit of detection to 1 000 ng/mL,with correlation coefficients exceeding 0.999. The retention time for individual amino acid was ranged from 4.60-9.16 min,while the limits of detection and limits of quantification was in the ranges of 0.2-10.0 ng/mL and 0.5-20.0 ng/mL,respectively. The recoveries across different spiked levels were 83.2%-118%,and the relative standard deviations varied between 0.90%-9.4%. The method was applied to quantify 37 amino acids in 49 serum samples. The results indicated that,with the exception of anserine and cystathionine,which were not detected,and homocysteine,which had a detection rate of 10.20%,the detection rates of the other 34 amino acids were greater than 90%. This method demonstrates good detection performance and can be used for the determination of amino acid in serum samples,providing more comprehensive data for diseases related to amino acid metabolism disorders.
关键词:liquid chromatography-tandem mass spectrometry(LC-MS/MS);amino acid;serum;sulfosalicylic acid
摘要:A method for determining the content of polychlorinated terphenyls in heavy oil samples based on distillation cutting separation-solid phase extraction-Ni online catalysis-gas chromatography-tandem mass spectrometry method has been established. Nickel catalyst was used for online catalysis to convert chlorinated triphenyl compounds into dicyclohexylbenzene. Gas chromatography-tandem mass spectrometry in multiple reaction monitoring mode with internal standard method was used for determination. This study conducted optimization analyses on the distillation cut temperature,selection of catalytic carriers,solid phase extraction conditions,and catalytic reaction parameters. The linear ranges of the recovered curve ranged from 1 to 50 μg/mL. The limits of quantification(LOQ) were 0.35-0.60 μg/mL,which was equivalent to having a LOQ at 4.7 μg/kg. The recoveries ranged from 87.3% to 112%,and the relative standard deviations(RSDs) were not more than 6.2%. The results showed that this method was accurate and reliable,and was suitable for the analysis and determination of chlorinated triphenyl compounds in imported diluted asphalt,residual fuel oil,and other heavy oil products.
关键词:gooey oil;cutback asphalt;fuel oil;polychlorinated terphenyl;online catalysis;gas chromatography-tandem mass spectrometry
摘要:The determination of dissolved oxygen is a crucial tool in ecological,environmental science,and hydrological research. By monitoring and regulating dissolved oxygen concentrations in real time,it is possible to effectively maintain aquatic ecological balance and promote sustainable development. Therefore,it is necessary to develop a dissolved oxygen sensitive material with low cost,simple preparation and high stability,and to realize rapid detection of dissolved oxygen in a fluorescence turn-on mode. The paper has described a green carbon nanodots(GCDs) with an excitation wavelength of 563 nm for sensing dissolved oxygen prepared by the precursor of o-phenylenediamine. The GCDs has been found to display a fluorescence-switchable property,the fluorescence of GCDs can be quenched by sodium dithionite and then restored by dissolved oxygen. The conversion between the two states is reversible and can be repeatedly alternated. Moreover,the fluorescence intensity of GCDs remains unaffected by the number of alternations. On this basis,the quenched GCDs can be used as a turn-on fluorescence dissolved oxygen sensor. The sensor shows a linear relationship with the dissolved oxygen content ranging from 0.4 to 0.8 mL and 0.143 mmol/L of the limit of detection. It also demonstrates good precision and good reproducibility for measuring the oxygen in air,as indicated by the recoveries of 92.6%-102% and the relative standard deviation(RSD) of 0.99%-9.5%(n=3). By immobilizing the GCDs onto the test paper,the above method has been extended to make a test paper-based dissolved oxygen sensor. The dissolved oxygen content can be directly sensed by the color change of the test paper,and the prepared test strip can be applied to the constructed dissolved oxygen sensor with a dual-fiber optic probe to enable semi-quantitative detection of the dissolved oxygen concentration in a solution. Compared with commercial sensors,it shows fast response time(~6 min relative to~12 min of the solution manner above) and higher sensitivity(1.17 relative to 1.35 of the solution manners above). This method has been proved to be a feasible method for rapid detection of dissolved oxygen with the advantages of convenience,low cost and rapid response.
摘要:The identification of stamp pad ink types is a critical component in the field of forensic document examination,holding significant practical value for the analysis of seal impressions. In this study,hyperspectral imaging technology was employed to acquire spectral data from multiple brands of stamp pad inks,followed by preprocessing using the Savitzky-Golay(SG) method. Subsequently,a stamp pad ink type identification model was constructed based on the random forest (RF) algorithm. To validate the model's performance,the RF model was systematically compared with traditional methods such as the backpropagation neural network(BP) and the multilayer perceptron (MLP). Additionally,grid search combined with five-fold cross-validation was utilized to optimize model parameters,thereby enhancing the model’s performance and generalization capability. Experimental results demonstrated that the RF classification model(with 20 decision trees and 3 leaf nodes) outperformed the BP and MLP models across evaluation metrics including precision,sensitivity,specificity,and F1-score,achieving classification accuracies of 99.77% and 98.66% on the training and test sets,respectively. The proposed method,integrating hyperspectral imaging technology with the RF algorithm,enables rapid,non-destructive,and accurate identification of stamp pad ink types,offering a novel technical reference for the analysis of atomic seal ink traces.
摘要:A microRNA-31(miRNA-31) amplifying detection signals method based on nucleic acid isothermal strand displacement amplification(ISDA) and CRISPR-Cas12a system were established and achieved visualizing detection by combining with reverse fluorescence enhancement lateral flow strip(rLFTS) platform. Under optimizing the primer toehold design and reaction buffer of ISDA reaction,miRNA-31 signal was efficiently amplified to output copious double stranded DNA,which activated CRISPR-Cas12a trans-cleavage activity to digest single-stranded reporter molecules and led to gold nanoparticles couldn′t be captured on the test lines by sandwich method to quench Cy5 fluorescence,causing corresponding quantitative fluorescence signals for improving miRNA-31 detection sensitivity. The results showed that the detection limit of 57.9 amol/L and recoveries of 91.6%-111% for detection miRNA-31 in saliva samples by the method. Moreover,the quantitative results had good consistency with qRT-PCR method in a much faster detection time(90 min). Given its simplicity,sensitivity and rapid,ISDA-Cas12a-rLFTS could meet the demand for ultra-sensitive detection of miRNA-31 in saliva samples.
摘要:A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) analytical method was developed for the determination of thirteen mycotoxins in grains by using Captiva EMR-Lipid column for purification. After being grinded,samples were extracted with acetonitrile-water-formic acid(84∶15∶1,volume ratio). Extract solution was purified by Captiva EMR-Lipid solid phase extraction column,and then concentrated by nitrogen blowing,diluted to a certain volume and determined. The targets were seperated on a XSelect HSS T3(2.1 mm×100 mm,3.5 μm) column. Acetonitrile and 0.1% formic acid water were selected for the positive ion mode and methanol and 0.1% ammonia water for the negative mode. Gradient elution and mass spectrometry under multiple reaction monitoring(MRM) mode were used for testing and external standard method was used for quantitative analysis. Thirteen mycotoxins exhibited good linear relationships across different mass concentration ranges with their correlation coefficients(r2) greater than 0.99. The limits of detection(LOD)were 0.10-3.12 μg/kg,and limits of quantitation(LOQ)were 0.33-10.4 μg/kg. Corn,wheat,rice,and sorghum were used as the blank matrix,and spiked at three levels of high,medium,and low. The average recoveries were 76.4%-108%,and the relative standard deviations(RSDs) were 3.2%-8.8%(n=6). Imported grain samples were tested by the method. Aflatoxin B1,T-2 and ochratoxin A were detected in a rice sample,and zearalanone was detected in a corn sample. The method is accurate,reliable and reproducible,which can be used for the quantitative analysis of thirteen mycotoxins for imported grains.
关键词:high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS);mycotoxin;grains;simultaneous determination
摘要:This study applied ultra-performance liquid chromatography tandem quadrupole electrostatic field orbitrap high resolution mass spectrometry(UPLC-Q-Orbitrap-HRMS) to analyze the changes of chemical constituents of Sanguisorba officinalis L.before and after carbonized,and to screen the different hemostatic components. Waters BEH C18(100 mm×2.1 mm,1.7 μm) column was used to process with 0.1% formic acid water solution and acetonitrile as the mobile phase for gradient elution. The heated electrospray ion source(HESI) was adopted to collect the data in both positive and negative ionization modes. Based on the accurate mass,fragment ions,literature and network database,a total of 41 chemical components were identified by matching precise molecular ion masses,MS/MS fragmentation patterns,literature data,and database references. These included 17 phenolic acids,12 flavonoids,9 triterpenoids,and 3 other compounds. Principal component analysis(PCA) and orthogonal partial least squares-discriminant analysis(OPLS-DA) were conducted using SIMCA 14.1 software to screen differential components between Sanguisorba officinalis L. before and after carbonization. After carbonization,the contents of hemostasis-enhancing components(gallic acid,ziyuglycoside Ⅱ,tormentic acid and ursolic acid) increased significantly,while glucogallin,catechin,brevifolin carboxylic acid,ellagic acid and pomolic acid decreased. The results showed that triterpenoids and phenolic compounds in Sanguisorba officinalis L. after carbonized may constitute the key material basis for its enhanced astringent hemostatic effect. This investigation provides scientific insights into the intrinsic mechanisms underlying the strengthened hemostatic efficacy of Sanguisorba officinalis L. after carbonization.
关键词:Sanguisorba officinalis L.;UPLC-Q-Orbitrap-HRMS;chemical constituents;Chinese medicine processing;high resolution mass spectrometry;differences analysis
摘要:The rapid detection of urine adenosine is of great significance for the screening of tumors and other diseases,but the existing methods have problems such as complex operation and low sensitivity. In this study,a G quadruple tandem labeled aptamer sensor was proposed for the rapid and sensitive detection of adenosine in urine. Firstly,double-stranded nucleic acids containing an adenosine aptamer(Apt) were covalently modified on the electrode surface. Upon the presence of adenosine,it specifically binds to the aptamer,exposing the primer probe(Primer,P). Subsequently,rolling circle amplification(RCA) is initiated using the exposed primer as a template,which rapidly generates single-stranded nucleic acids rich in G-base repetitive sequences. These sequences self-assemble into G4 structures(G4) in the presence of potassium ions,which could immobilize a large amount of methylene blue(MB),thereby enhancing the response current and elevating the detection sensitivity. Electrophoresis,cyclic voltammetry and AC impedance were used to characterize the sensor construction process,and the adenosine detection conditions were optimized. Under the optimal experimental conditions,the linear detection range of the sensor is 1 fmol/L-1 nmol/L,and the detection limit is 0.68 fmol/L. In addition,the sensor exhibits good stability(RSD=5.4%),reproducibility(RSD=4.1%),and selectivity. The recoveries of adenosine in fresh urine samples were 104%-105%,and the RSDs were 1.5%-5.5%. The aptamer biosensor has the characteristics of easy to operate,high sensitivity,good specificity and low cost,which is anticipated to detect adenosine in urine rapidly and sensitively.
关键词:adenosine;aptamers;rolling circle amplification;G-quadruple;electrochemical sensors
摘要:In this study,a rapid detection method based on portable mass spectrometry technology for the detection of pesticide residues in Chinese medicinal materials(CMM) was established. Notoginseng Radix et Rhizoma,Lonicerae Japonicae Flos and Lycii Fructus were used as detection objects,acetamiprid and carbendazim were used as detection indicators to investigate the sensitivity and accuracy of the established method. The results indicated that by using a direct extraction combined with hydrophilic and lipophilic balance(HLB) solid-phase extraction column clean-up method,acetamiprid and carbendazim showed good linearity(r>0.99) in the ranges of 1.0-40 mg/kg and 0.125-5.0 mg/kg,respectively. The detection limits (LOD) for acetamiprid and carbendazim were 0.30 mg/kg and 0.05 mg/kg,while the quantitation limits (LOQ) for carbendazim and carbendazim were 1.0 mg/kg and 0.125 mg/kg,respectively. The method achieved recoveries ranging from 72.8% to 95.3%,with relative standard deviations(RSDs) between 10% and 34%. The portable mass spectrometry was used to determine acetamiprid and carbendazim in Notoginseng Radix et Rhizoma,Lonicerae Japonicae Flos,Lycii Fructus,validated by liquid chromatography-tandem mass spectrometry(LC-MS/MS). The results were basically consistent,which indicated that portable mass spectrometry can meet the daily detection needs of acetamiprid and carbendazim in CMM.
关键词:portable mass spectrometry;Chinese medicinal materials;pesticide residues;rapid detection
摘要:This study utilized infrared spectroscopy to systematically identify and analyze adulteration in raw lacquer. Authentic lacquer samples were collected from multiple production regions,and simulated adulterated samples were prepared by incorporating six common adulterants:raw tung oil,blended oil,urea,brown sugar,curing agent [isocyanate],and diluent [ethylene glycol dimethyl ether]. A comprehensive spectral database was constructed,comprising a reference infrared spectral library for pure lacquer,a quality control(QC) spectral library,and an adulterated sample retrieval library. By integrating simulated spectral computations with experimental validation of adulterant spectra,we developed a novel dual-parameter discrimination model based on optimal spectral matching degree and characteristic absorption peak analysis. Experimental results demonstrated that this method achieved high detection sensitivity(3%-10%) for five of the tested adulterants(raw tung oil,blended oil,urea,curing agent [isocyanate],and diluent [ethylene glycol dimethyl ether]),with a recognition accuracy of 92% within the corresponding adulteration range. The proposed approach provides a reliable and efficient analytical tool for quality assessment and adulteration screening of raw lacquer products. This study holds significant practical value for regulating the lacquer market and preserving the integrity of traditional lacquerware craftsmanship.
摘要:In traditional isothermal exponential amplification reaction(EXPRA),the target nucleic acid has the same energy at both ends of the symmetrical amplification template. However,when the target nucleic acid hybridizes with the 5' end of the template,amplification becomes difficult to trigger,limiting the method's use in the analysis of trace amounts of target nucleic acids. To address this issue,this study introduces a highly sensitive and rapid analytical method for microRNA detection,employing asymmetric hybridization-induced isothermal exponential amplification reaction(AEXPRA),with miR-196b as the target. An asymmetric linear amplification template was meticulously designed,enabling miR-196b to fully hybridize to the 3' end of the template due to complete complementarity,while only partially complementing the 5' end. This innovative approach boasts high sensitivity,strong specificity,and rapid detection capabilities. The entire reaction time is efficiently contained within 30 minutes,allowing for the detection of as low as 0.42 amol/L of miR-196b. To validate the practical applicability of this method,it was utilized to analyze miR-196b levels in serum extracts. Remarkably,the method effectively distinguished miR-196b expression levels between non-small cell lung cancer patients and healthy controls,with results that were consistent with those obtained through RT-qPCR,thereby demonstrating high accuracy and reliability. Consequently,this AEXPAR method holds substantial promise for advancing clinical diagnosis and pathological research in the realm of miRNAs.
摘要:A rapid analytical method was established for the determination of three organic amine risk substances(DMAPA,LAPDMA,and MYPDMA) in cosmetics using ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). The analytes were ultrasonically extracted with acetonitrile,separated on a BEH Amide chromatographic column(2.1 mm×100 mm,1.7 μm),and detected in multiple reaction monitoring(MRM) mode. The whole analysis was completed within 4 min. The results showed that DMAPA had a good linear relationship within the range of 5-500 µg/L,while LAPDMA and MYPDMA had good linear relationships within the range of 0.5-50 µg/L(correlation coefficient r>0.995). The limits of detection(LOD) were determined as 0.8 μg/g for DMAPA,and 0.08 μg/g for both LAPDMA and MYPDMA. The average recoveries were 80.5%-93.4% with the relative standard deviations(RSDs,n=6) between 2.6%-6.4% for low,medium and high standard QC samples in three cosmetics matrices(water,cream and lotion). The developed method demonstrates simplified sample pretreatment procedures,and effectively fulfills the requirements for rapid screening of three organic amine contaminants associated with cocamidopropyl betaine(CAPB) in diverse cosmetic matrices.
关键词:cosmetics;organic amine;ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS);cocamidopropyl betaine(CAPB)
摘要:The presence of 37Ar,produced via 40Ca(n,α)37Ar during nuclear explosions,is a key Comprehensive Nuclear-Test-Ban Treaty(CTBT) verification indicator. Its activity concentration is measured against collected argon volume; levels above background indicate a nuclear test. However,residual oxygen in samples,which has nearly identical physical properties to argon,is difficult to remove completely,causing errors in argon volume and 37Ar quantification,compromising verification reliability and potentially leading to false compliance conclusions. To address this oxygen-argon separation analytical challenge,this study systematically investigated the separation efficiency of oxygen and argon mixtures using gas chromatography(GC). Key operational parameters including column oven temperature,inlet pressure,and gas concentration were optimized to achieve the baseline separation of oxygen and argon. After an extensive series of experiments and in-depth analysis,the results demonstrated that a column oven temperature of -65 ℃ and an inlet pressure of 35 kPa could effectively separate oxygen and argon across a wide range of concentration ratios. For a 50% O2-50% Ar mixture,a resolution(R) of 1.50 was achieved,indicating a good separation degree. While for a 95% O2-5% Ar mixture,although the separation was more challenging,an R value of 1.14 was still obtained,and in both cases,the total analysis time were within 5 minutes,which demonstrate the high efficiency of this method. Furthermore,a linear external standard calibration curve with a high correlation coefficient(r2>0.999) was established for argon quantification,validated using an oxygen-rgon mixture gas with an argon volume ratio concentration of 3%. Verification tests were conducted,and the results showed that the relative deviation between the experimentally measured argon concentrations and the certified reference values was less than 4%. This low relative deviation not only highlights the high precision of the established method but also provides strong support for its reliability in practical applications,ensuring more accurate and reliable nuclear test verification under the CTBT framework.
摘要:In situ X-ray diffraction(in situ XRD) was used to analyze the effects of different gases on the reducing process of iron-based F-T catalysts and the growth of iron carbide in CO,CO+H2,and H2 followed by CO at 275 ℃. The Fe2O3 precursor mainly transforms into Fe5C2 phase in three gases with grain sizes of 12.1,16.9 and 20.6 nm. The diffraction peaks corresponding to the(021),(510) and(112) crystal surfaces change from complete overlap to separation. And there is always a small amount of residual Fe3O4 phase in the product. Fe2O3 was reduced in H2 for 10 hours. The reduction sample was characterized using in situ X-ray photoelectron spectroscopy(in situ XPS). The results show that the sample is mainly consist of Fe phase and Fe3O4 phase exists on the surface of Fe phase. Based on the analysis results of XRD and XPS,iron carbide grains grow faster in higher H2/CO ratio gas during the Fe2O3 reduction process. There is always a small amount of residual Fe3O4 phase on the surface of the particles,which may be caused by the equilibrium reaction of Fe3O4-Fe(Fe5C2) conversion. These results are of great significance for understanding the effects of different gases on the reduction process of Fe-based catalysts and the crystal phase of active phase iron carbide,and also provide a useful reference for optimizing the preparation conditions of catalysts and improving their catalytic performance.
摘要:To implement the concept of integrating scientific research and education,a comprehensive experiment was designed to improve the performance of immunochromatography for salbutamol in swine urine. Based on the principle of small molecule competitive reaction,different sizes of colloidal gold were prepared. The key factors affecting the method's performance,such as labeling pH,antibody amount,and blocking agent,were designed and optimized. A rapid immunochromatography based on colloidal gold for salbutamol in swine urine was established. The cut-off value of the method was 3 ng/mL,with sensitivity comparable to similar products on the market. Through the entire design and practice of the immunochromatography,the frontiers and practical applicability of teaching contents were enhanced,enabling students to thoroughly understand the principles and development process of this technology,thus cultivating their abilities in scientific research innovation and practical application. Moreover,ideological and political education elements were introduced into experimental teaching to foster students' unwavering commitment,dialectical analysis skills,and teamwork spirit in scientific research.
关键词:immunochromatography;salbutamol;comprehensive experiment;practical teaching;course ideology and politics
摘要:Rapid diagnosis of acute myocardial infarction(AMI),as one of the key triggers of sudden cardiac death,is essential to reduce cardiovascular mortality. Among many AMI biomarkers,cardiac troponin I(cTnI) has become the gold standard for the diagnosis of AMI due to its high specificity and sensitivity. To meet the clinical demand for rapid and accurate detection of cTnI,a variety of biosensor technologies have emerged,among which biosensors based on the principle of magnetic separation are particularly compelling. These sensors utilize the unique properties of magnetic nanomaterials to efficiently separate and enrich cTnI in complex biological samples,such as blood,for highly sensitive detection. By optimizing the magnetic separation process and sensor design,the accuracy and reproducibility of the detection can be further improved,providing strong support for early diagnosis and treatment of AMI. We have outlined the recent advancements in research on electrochemical sensors,optical sensors,and visual sensors based on magnetic separation,as well as their applications in cTnI detection. The existing challenges of cTnI biosensors based on magnetic separation technology are discussed,and we provide an outlook on magnetic separation-based biosensors,offering insights for the further development of portable,miniaturized,and intelligent cTnI detection devices.