摘要:RNA plays a crucial role in biological processes,and its single-nucleotide mutations and modifications are closely associated with various diseases. However,existing RNA detection methods are limited in widespread application due to their operational complexity and analytical challenges. Consequently,the development of analytical techniques capable of precisely identifying RNA single-nucleotide mutations and modifications is essential. Among various approaches,nanopore single-molecule technology demonstrates significant potential. Recently,Nature Nanotechnology reported a novel method utilizing solid-state glass nanopores for detecting single-nucleotide RNA mutations and modifications—RNA single-nucleotide characterization and analysis nanolatch(RNA-SCAN). By integrating RNA/DNA origami nanotechnology with programmable nanolatches,RNA-SCAN achieves precise identification of single-nucleotide variations within complex RNA structures without requiring labeling or amplification steps. This technology presents a novel approach for detecting RNA-related diseases and provides a powerful tool for in-depth research into RNA properties,further expanding the applications of nanopore technology.
关键词:RNA;single-nucleotide mutations and modifications;nanopore;nanolatch
摘要:With the advancement of precision medicine,there is a growing demand for high-throughput platforms capable of detecting multiple biomarkers. Framework nucleic acids(FNAs),owing to their highly programmable structures and functional scalability,have emerged as ideal materials for the construction of next-generation bioanalytical platforms. FNAs enable highly sensitive detection of various biomarkers,including microRNA(miRNAs),proteins,and metabolites,with exceptional specificity and signal amplification capabilities,making them particularly suitable for multiplexed and synergistic target recognition. The integration of FNAs with microfluidic chips and portable detection devices further enhances detection throughput and sensitivity,facilitating their translational applications in clinical scenarios such as early disease screening,personalized intervention,and point-of-care diagnostics. This review systematically summarizes recent progress and representative applications of FNAs in multiplexed bioanalysis,focusing on the design of recognition elements,sensing interfaces,spatial configuration control,signal amplification strategies,hardware integration,and signal acquisition. The aim is to provide theoretical support and practical guidance for the development of robust multi-biomarker detection systems.
摘要:Volatile organic compounds(VOCs) in human exhaled breath serve as end products of diverse metabolic pathways,offering critical insights into the body’s physiological and pathological states. The development of rapid analytical methods for small-molecule VOCs holds significant scientific value and promising potential for noninvasive disease diagnosis. Direct inlet mass spectrometry(DIMS),owing to its high sensitivity,rapid analysis,and exceptional versatility,has emerged as a key technique for high-throughput characterization of complex samples. Vacuum ultraviolet photoionization(VUV-PI),a core ionization technology for DIMS,exhibits distinct advantages,including high molecular ion yield,minimal fragmentation,and broad operational pressure compatibility(from high vacuum to ambient conditions). Its ability to efficiently ionize compounds across a wide polarity range—from nonpolar to strongly polar species—makes it a powerful and versatile tool for mass spectrometric detection. This article systematically reviews advancements in photoionization mass spectrometry(PI-MS),covering critical components such as ionization sources,ion optics,and mass analyzers. Furthermore,it highlights recent progress in PI-MS-based exhaled breath analysis for disease screening and discusses future perspectives in this rapidly evolving field.
关键词:time-of-flight mass spectrometry;ion mobility spectrometry;photoionization;exhaled breath;volatile organic compounds;disease screening
摘要:Mercury(Hg),as a global pollutant,can accumulates in brain tissues and induces irreversible neurodegenerative damage,posing a severe threat to human health. Conventional studies predominantly focus on tissue-level Hg content and distribution,masking its cellular heterogeneity. Single-cell investigations into Hg distribution within brain tissues unveil cell-type-specific accumulation and metabolic variations,resolving heterogeneous cellular responses to Hg exposure. These advances deepen the understanding of Hg's neurotoxic mechanisms and provide scientific foundations for precise assessment of neurotoxic risks and development of targeted intervention strategies. This review summarizes the characteristics of single-cell Hg distribution in brain tissues,and discusses key determinants including Hg speciation,exposure conditions,cellular phenotypes,functional states,and tissue microenvironment. We further summarize advancements in single-cell metal detection technologies for Hg analysis and critically address current challenges and future directions in this emerging field.
关键词:Hg;single-cell;brain tissue;single-cell metal detection technology
摘要:In order to assess the hygiene of retail refrigerated pre-marinated beef steaks rapidly and accurately,this study developed a colony count detection method based on flow cytometry. The T-test results showed no significant difference between the flow cytometry results and the national standard method(p<0.05),and Pearson’s correlation analysis demonstrated a significant relationship between the two methods(p<0.001). This indicates that flow cytometry can be used to replace the GB 4789.2 national standard for analyzing colony counts in refrigerated pre-marinated beef steaks. Further,Chi-square analysis revealed no significant differences in hygiene among beef steaks sold in different supermarkets,suggesting that temperature control at the retail level is not the main factor affecting beef steak hygiene. Further metagenomic tracing confirmed that the hygiene of beef steaks is closely related to the hygiene control of the production environment.
摘要:To meet the demands for rapid on-site detection,high-throughput operations,and intelligent data processing,miniaturization and intelligence have become key development directions for environmental analytical instruments. However,traditional research and development models face challenges such as long developing cycle,high cost,and difficulty in customization. The development and integration of digital technologies,such as 3D printing,computer-aided design,and artificial intelligence,offer new pathways for innovation in environmental analytical instruments. 3D printing can significantly shorten the "design-manufacture-optimize" period,reduce costs,and enable customized designs and precise manufacturing of complex microstructures,thus laying a hardware foundation for the miniaturization and intelligence of environmental analytical instruments. Additionally,the integration of 3D printing with other digital technologies is expected to facilitate the construction of detection networks and cloud-based collaborative analysis. This paper summarizes the research progress of 3D printing in the development of customized environmental analytical instruments,and discusses future trends and challenges,aiming to provide new insights for the development of miniaturized and intelligent environmental analytical instruments in the future.
关键词:development of environmental analytical instruments;3D printing;miniaturization;intelligence;digital technology
摘要:Nanopore sensing technology is a simple and efficient single-molecule electrochemical analytical technique,which is widely used in fields such as DNA sequencing,molecular sensing,disease diagnosis,and environmental monitoring. Compared to traditional analytical techniques,nanopore sensing presents many advantages,including ultrahigh detection sensitivity,rapid detection,portable device,and low cost,making it particularly suitable for on-site and rapid detection applications. In recent years,the application of nanopore sensing technology in rapid detection of food contaminants has been developing rapidly,covering targets such as foodborne pathogens and chemical contaminants including mycotoxins and pesticides. It gradually grows as a new hot topic in the fields of analytical chemistry and food safety. This review mainly focuses on the research progress of biological nanopore-based sensing technology for the rapid detection of food contaminants in the past five years,including the basic principles of nanopore sensing technology,recent key advances in the rapid detection of foodborne pathogens and chemical contaminants in food. It also provides an outlook on future trends on this topic.
关键词:biological nanopore;gene sequencing;rapid detection for food safety;foodborne pathogens;mycotoxins;pesticide residues;α-hemolysin
摘要:Micro/nanoplastics in environment can enter organisms through cross-media processes,posing significant threats to ecological environments and human health. Precise imaging and quantification of micro/nanoplastics within organisms are basis for assessing their ecological risks and health threats. This review summarizes relevant literature on the imaging and quantification of micro/nanoplastics in organism by bibliometric methods,thereby elucidating advances in imaging and analytical methods. Furthermore,we summarize progresses and challenges in imaging and quantification methods of micro/nanoplastics in terms of aquatic organisms,terrestrial organisms,and microbial/cellular. The applicability of current methodologies is summarized,and we propose future trends for the imaging and quantification analysis methods of micro/nanoplastics in biological organisms to promote methodological research and improve environmental health risk assessments.
摘要:Chemiluminescence(CL),with its rapid response,excellent sensitivity,no need for external excitation light source,and suitability for online monitoring,has become a research hotspot in the field of analytical chemistry. This review systematically summarizes recent advancements in nanostructure-enhanced CL sensing strategies,encompassing material functionalization design principles,performance optimization mechanisms,and analytical applications. First,we systematically elucidates the structure-property correlations for enhancing the luminescence efficiency of chemiluminescence in the surface/interface engineering of nanomaterials(including zero-dimensional,one-dimensional,two-dimensional and three-dimensional nanostructures). Next,we systematically classified the function-driven nanomaterial design strategies to develop high-fidelity chemiluminescence sensing systems,particularly focusing on breakthroughs in specific recognition and trace analysis in complex matrices. Additionally,we also systematically discussed the typical application progress of chemiluminescence sensing technology in the continuous monitoring of emerging environmental pollutants,the multiple detection of disease biomarkers in vivo and in vitro,and the screening of food pollutants. This review not only reveals the critical role of nanoengineering in achieving metric-level improvements in selectivity,signal stability,and anti-interference robustness,but also provides a systematic theoretical framework and technical guidance toward next-generation CL sensing platforms
摘要:In vivo acquisition of chemical information from living organisms is crucial for unraveling the underlying molecular mechanisms of physiological and pathological conditions. Over the past two decades,real-time,on-line and non-invasive direct mass spectrometry approaches are of increasing importance in in vivo analysis,owing to their high sensitivity,exceptional accuracy,rapid response capability,as well as the absence of physical damage or physiological stress inflicted upon the organisms. In this paper,the principles and technical characteristics of in-situ,real-time and non-invasive direct mass spectrometry approaches which are applied to the analysis of exhaled breath samples and body surface samples,including extractive electrospray ionization mass spectrometry(EESI-MS),neutral desorption extractive electrospray ionization mass spectrometry(ND-EESI-MS),proton transfer reaction mass spectrometry(PTR-MS),secondary electrospray ionization mass spectrometry(SESI-MS),selected ion flow tube mass spectrometry(SIFT-MS),and low-temperature plasma probe mass spectrometry(LTP-MS),are comprehensively reviewed,based on the types and properties of living samples(human tissues,plant tissues,microorganisms). Finally,we outlook the future directions and prospects of real-time non-invasive in vivo mass spectrometry approaches from the perspectives of sampling approaches,ionization techniques,and application prospects(such as in medical science,environmental science,agricultural and plant sciences,and public safety).
关键词:mass spectrometry;real-time non-invasive;in vivo sampling;exhaled human breath;body surface samples
摘要:Atmospheric pressure matrix-assisted laser desorption ionization mass spectrometry (AP-MALDI-MS) is an analytical technique that performs ionization in an atmospheric pressure environment. It has become a powerful analytical tool for multidisciplinary research in biology,medicine,plant science and food science with high throughput,high sensitivity,low sample consumption and direct real-time analysis. In recent years,the rapid development and widespread application of AP-MALDI-MS technology has made it a focus of attention for researchers. This review provides an overview of the latest research progress on its application in key areas,including the analysis of biological macromolecules,mass spectrometry imaging,small molecule detection and non-targeted screening. It also delves into its potential applications and limitations,with the aim of providing a reference for the further development of AP-MALDI-MS technology.
摘要:With the rapid advancement of biomedicine,biomacromolecular drugs such as monoclonal antibodies,peptide-based targeting agents,oligonucleotides,and vaccines have gradually become fundamental components of modern healthcare,offering new therapeutic options for a variety of human diseases. Unlike traditional small-molecule chemical drugs,biomacromolecules exhibit characteristics such as structural complexity,susceptibility to inactivation,and high immunogenicity,which present significant challenges to their development and application. Additionally,macromolecular drugs often possess complex topological structures,and spatial denaturation can lead to the formation of topological isomers. These isomers,despite sharing highly similar physicochemical properties with the original drugs,may exhibit entirely different physiological activities,potentially impacting drug safety and efficacy. Recent studies have shown that certain human diseases,such as Alzheimer’s disease and Parkinson’s disease,are closely associated with phase transitions or isomerization of proteins within the body. Consequently,the analysis,separation,and structural investigation of topological isomers in biomacromolecules are essential for elucidating the mechanisms of action of biomacromolecular drugs and advancing our understanding of the pathogenesis of complex diseases. These research efforts are currently at the forefront of analytical science and biomedical research. Ion mobility-mass spectrometry(IMS-MS),particularly cyclic ion mobility-mass spectrometry(cIMS-MS),has increasingly become a crucial tool in the analysis of complex macromolecular topological isomers. This paper focuses on the working principles of IMS and highlights recent innovative applications of IMS in the analysis of macromolecular drug isomers and macromolecular isomers associated with complex diseases. Additionally,the future prospects for its applications are discussed.
摘要:With the acceleration of urbanization and industrialization,odor gas pollution has become a significant environmental issue. Its low olfactory threshold and multi-pathway exposure pose threats to the environment and public health. The thermal desorption-gas chromatography-mass spectrometry(TD-GC-MS) technique has emerged as one of the primary methods for odor gas analysis due to its capabilities for accurate identification and sensitive quantification. Based on a bibliometric analysis of literature over the past 15 years,this review summarizes the technical characteristics and development trends of TD-GC-MS. Furthermore,it systematically discusses the application of TD-GC-MS in the analysis of odor gas from different sources,including the identification of odor characteristics and source tracing of multiple sources such as natural sources,industrial sources,domestic sources,agricultural sources,and disinfection sources. Future research can focus on directions such as the construction of artificial intelligence data models,the integration with electronic nose technique,and the development of portable devices,aiming to enhance the automated analysis capabilities of odor gas and on-site monitoring efficiency,thereby providing more comprehensive technical support for environmental pollution prevention and control,as well as public health protection.
摘要:The long production cycle of traditional Chinese medicines from cultivation to market circulation,combined with inadequate control at the source or during processing,makes them highly susceptible to mycotoxin contamination,significantly compromising their quality and safety. Systematic detection and assessment of mycotoxin contamination levels and potential risks in these materials are crucial for refining safety and quality control standards and ensuring the safe medicinal and edible use of traditional Chinese medicines. However,the extensive metabolic components in traditional Chinese medicines pose substantial matrix interference for trace-level mycotoxin detection,while the unpredictability of contamination and the structural diversity of mycotoxins present major challenges in developing broad-spectrum,high-throughput detection methods suitable for complex traditional Chinese medicines matrices. This review summarizes the research progress in high-throughput mycotoxin detection based on liquid chromatography-tandem mass spectrometry(LC-MS/MS),integrating advancements in sample pretreatment,chromatographic separation,and instrumental detection methodologies,thereby providing valuable references for the development of high-throughput mycotoxin detection methods in traditional Chinese medicines.
关键词:traditional Chinese medicines;mycotoxins;LC-MS/MS;sample pretreatment;liquid chromatographic separation;mass spectrometry detection
摘要:Traditional Chinese medicine has the characteristics of multiple components,multiple targets,and multiple pathways. The research on its pharmacological substances and mechanism of action is the core for explaining the overall efficacy and the essence of the action of traditional Chinese medicine. Mitochondria are the main organelles for energy production within cells,participating in the regulation of multiple important physiological and biochemical processes in the body. By exploring the effects of traditional Chinese medicine on mitochondrial structure and function,it is possible to reveal the basis of the pharmacological substances of traditional Chinese medicine and to explore its mechanism of action. This review will summarize the mechanisms and research progress of traditional Chinese medicine and its active components exerting regulatory effects on mitochondria from two directions:the effects of traditional Chinese medicine on mitochondrial structure and function,and the effect targets and active components of traditional Chinese medicine acting on mitochondria. It will provide a reference for further development of targeted research on the functional regulation of mitochondria using traditional Chinese medicine or natural products and for the study of their active mechanisms.
关键词:mitochondrial structure and function;therapeutic targets of traditional Chinese medicine;active substance;mechanism of action
摘要:Adsorption as an effective technique for the remediation of wastewater has been widely used in industrial wastewater treatment due to the advantage of cost-effectiveness,availability of the adsorbent and ease of operation. However,the low adsorption capacity of the reported adsorbents is still a challenge for wastewater treatment with high-efficiency. Here,we developed a super adsorbent(SUA-1),which was a kind of porous carbon nanofibers derived from a composite of PAN-based electrospinning and ZIF-8(PAN/ZIF-8) via simple heat treatment process. The as-prepared SUA showed an ultra-high adsorption capacity for adsorbing methyl blue(MB) at nearly three times its own weight,as high as 2 998.18 mg/g. A series tests demonstrated that the pore-making effect of ZIF-8 during heat treatment process endowed high BET surface area and generated ZnO components as chemical adsorption center. Under the synergistic effect of bonding and non-bonding forces including ionic bond,electrostatic interaction,and π-π interaction,the adsorption capacity has been greatly improved. In view of promising efficiency,this work provides guidance and insights for the preparation of highly efficient adsorbents based on electrospinning derived porous carbon nanofibers.
摘要:Calcium ions(Ca2+) and manganese ions(Mn2+) are essential for sustaining life activities and are key monitoring indicators in drinking water. Developing highly sensitive,selective,and portable detection methods for Ca2+ and Mn2+ is significant for water quality monitoring and human health. In this paper,blue fluorescent Ti3C2 MXene-based quantum dots(MQDs,λem=445 nm) are prepared using Ti3C2 MXene as the precursor. Through the chelation effect of ethylene diamine tetraacetic acid(EDTA),a blue and red dual-emission fluorescent probe,MQDs-EDTA-Eu3+-DPA,was constructed. Herein,dipicolinic acid(DPA) acts as an absorbing ligand and significantly enhances the red fluorescence of europium ions(Eu3+) at 616 nm through the “antenna effect”. The blue fluorescence of MQDs serves as an internal reference signal. High concentrations of Ca2+ can quench the red fluorescence of Eu3+-DPA;Mn2+ can be excited to emit purple fluorescence at 380 nm after coordinating with DPA,red fluorescence of Eu3+-DPA serves as the internal reference signal. Based on the above two fluorescence intensity changes,ratiometric fluorescence detection methods for Ca2+ and Mn2+ are established. The fluorescence intensity ratio(IF616/IF445) exhibits a linear relationship with Ca2+ in the range of 35-120 μmol/L,with a detection limit of 5.98 μmol/L. The fluorescence intensity ratio(IF380/IF616) shows good linearity with Mn2+ in the range of 0-14 μmol/L,with a detection limit of 28.6 nmol/L. This method was successfully applied to the quantitative analysis of Ca2+ and Mn2+ in commercially available mineral water(Nongfu Spring,Ganten,and Evergrande),with recovery rates of 80.6%-117% and relative standard deviations(RSD) of 0.76%-4.6%. Additionally,by preparing MQD-based fluorescent test strips,visual detections of Ca2+ and Mn2+ are achieved. This work demonstrates the application potential of MQDs in the field of visual fluorescence sensing of ions in water quality.
摘要:The chemical differences of alkaloids from Fritillariae Cirrhosae bulbus(Songbei,Qingbei,Lubei) and their common counterfeits(Fritillaria ussuriensis,Fritillaria walujewii,Fritillaria palldiflora) were studied to clarify the quantitative identification index of them. High performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) was used to determine the alkaloids of genuine and common counterfeit products. The differential compounds were analyzed by multivariate statistical methods,and identified by comparison of reference information,matching of mass spectrometry database and literature mass spectrometry information. The quantitative identification compounds were confirmed by combining their distributions in different samples. A HPLC-MS/MS method was established and verified by methodology. Twenty different metabolites in Songbei and Fritillaria ussuriensis,Qingbei and Fritillaria walujewii,Lubei and Fritillaria palldiflora were identified. Peimine and peiminine can be used as quantitative indicators to distinguish Songbei and Fritillaria ussuriensis,and imperialine and edpetiline can be used as quantitative indicators to distinguish Qingbei and Fritillaria walujewii,Lubei and Fritillaria palldiflora. HPLC-MS/MS technology combined with chemometrics can effectively clarify the different chemical components of genuine and common counterfeit Fritillariae Cirrhosae bulbus. The quantitative identification indexes were clearly defined,and it provided reference for the subsequent quantitative identification and quality control of Fritillariae Cirrhosae bulbus.
关键词:Fritillariae Cirrhosae Bulbus;HPLC-MS/MS;alkaloid;differential compounds;quality control
摘要:A novel method was developed for the simultaneous determination of 151 pesticides and 15 mycotoxins in Ziziphi Spinosae Semen(ZSS) using a combination of one-step automated QuEChERS and liquid chromatography-quadrupole-time of flight mass spectrometry(LC-Q-TOF MS). The sample was hydrated with 10 mL of deionized water and left to stand for 10 minutes. Subsequently,extraction was carried out using a 5% formic acid acetonitrile solution,followed by the addition of 4 g of anhydrous magnesium sulfate and 1 g of sodium chloride to induce phase separation. Cleanup was performed using 100 mg of octadecylsilane(C18),100 mg of N-propylethylenediamine(PSA),and 5 mg of multi-walled carbon nanotubes(MWCNTs) as purification materials. Both extraction and cleanup steps were conducted using a one-step automated QuEChERS pretreatment system. Separation was performed using a ZORBAX SB-C18 column(100 mm×2.1 mm,3.5 µm) with gradient elution,utilizing 0.1% formic acid aqueous solution(containing 5 mmol/L ammonium acetate) and 0.1% formic acid methanol as mobile phases. Detection was performed using LC-Q-TOF MS with electrospray ionization(ESI) and All ions MS/MS scanning in both positive and negative modes,and quantification was carried out via the matrix-matching external standard method. The analysis demonstrated that all 166 compounds exhibited good linearity,with correlation coefficients(r² ≥ 0.992 6) across their respective concentration ranges. The screening detection limits(SDLs) and limits of quantification(LOQs) ranged from 0.5 to 20 µg/kg for both raw and fried ZSS samples. Recovery experiments were performed on raw and fried ZSS at three spiked levels of 1-fold,2-fold and 10-fold LOQ(n=6),and the recoveries ranged from 71.2% to 118% with RSDs of 0.80% to 19% for raw ZSS and from 71.1% to 120% with RSDs of 1.0% to 19% for fried ZSS. The established method was applied to detect pesticide and mycotoxin residues in 20 batches of ZSS samples. Two pesticides and three mycotoxins were detected in actual samples. Notably,aflatoxin B1 was detected in both raw and fried ZSS samples,with its content exceeding maximum residue limit(MRL) set by the Chinese Pharmacopoeia(2020). The method developed in this study offers a highly effective and reliable approach for quality control and safety supervision of ZSS,making a significant contribution to the assessment of the safety of ZSS products in the market. The method has great potential for food safety and herbal product safety.
关键词:Ziziphi Spinosae Semen(ZSS);one-step automated QuEChERS;liquid chromatography-quadrupole-time of flight mass spectrometry;pesticides;mycotoxins
摘要:This article systematically analyzed the chromatographic behavior of solutes in mixed mode columns packed with C18 and SCX stationary phases in different proportions,obtaining theoretical expression of relationship between the retention factor of solutes on mixed mode chromatographic columns and packing ratios of the two stationary phases. Six mixed mode chromatography columns were prepared by mixing C18 stationary phase and strong cation exchange stationary phase prepared by the same silicon matrix with exact size and morphology in different packing ratios. The dead time of the mixed bed chromatography columns was measured by sodium nitrate marker method and Peterson-Hirsch method,which were used to predict retention factor trends with benzene derivatives,amino acids,alkaloids as model samples according to the theoretical expression. The predicted results were compared with the experimental data,showing the same trend. Sichuan Fritillaria sample was used as real sample to evaluate the performance of the mixed mode columns. The mixed mode columns packed with two stationary phases in different ratios provide significantly different retention behavior for solutes with different structures,and the variation trends were consistent with theoretical predictions. Obviously,the mixed bed column can fully utilize the characteristics of different separation modes,and the selectivity can be easily controlled by changing the packing ratio. The separation behavior of solute on the mixed bed column can be predicted based on its retention behavior on two original stationary phases,which provides a new idea for the design of chromatographic columns and separation modes,showing broad application prospects.
关键词:mixed mode chromatography;mixed bed stationary phase;dead time;retention factor
摘要:Due to the biosafety and ethical limitations of biomedical samples in the traceability of environmental exposure to organophosphorus nerve agents(OPNAs),the environmental exposure of OPNAs was traced and analyzed by identifying the OPNAs tyrosine adducts(OPNAs-Tyr) of plant abundant ribosyl-1,5-diphosphate carboxylase(RuBisCO) in the manuscript. Arabidopsis thaliana and rice(Oryza sativa L. cv.‘Nipponbare’) were selected as the main research objects and exposed to VX(VX),Tabun(GA) and Soman(GD),and the OPNAs-Tyr adducts were identified by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) analysis. The tyrosine adducts formed by RuBisCO protein with VX,GA and GD were successfully identified. The enzymatic hydrolysis conditions,solid-phase extraction conditions and the purification method of RuBisCO protein(protamine sulfate precipitation method(PSP)) were optimized. In Arabidopsis thaliana,the minimum detectable exposure doses of VX,GA and GD were 7.4 μg per plant,9.3 μg per plant and 91 ng per plant,respectively. In rice,the minimum detectable exposure doses for VX were 74 ng per plant,and the same results for GA and GD were obtained compared with those in Arabidopsis thaliana. The adducts concentration was positively correlated with the exposure dose and could remain stable up to six months in freeze-dried plant. This study demonstrates for the first time that the tyrosine adducts from the RuBisCO protein can be used as a reliable biomarker for the traceability analysis of environmental exposure to OPNAs. Given that RuBisCO protein is the most abundant edible protein in plants,this study also provides new ideas for the analysis of organophosphorus pesticide residue pollution in green food.
摘要:Based on the concept of analytical quality by design(AQbD),a quantitative fingerprint method was established using high performance liquid chromatography(HPLC) for the content determination of three main components—caffeic acid,rosmarinic acid,and salviaflaside — in the aqueous extract of Prunella vulgaris. The critical method parameters(CMPs) were determined using an Ishikawa diagram and single-factor experiments. A Box-Behnken design(BBD) experimental design method was employed to identify critical quality attributes(CQAs) and establishing the quantitative relationship model between CQAs and CMPs,with the P values of all models being less than 0.000 1 and R2 value greater than 0.97. Then a reliable method operable design region(MODR) was constructed. After verification,the method demonstrated good results in linearity,precision,stability,and repeatability tests,with relative standard deviations(RSDs) all less than 5.0%. The recoveries for the three main components and their RSDs complied with the requirements in Chinese Pharmacopoeia 2020 edition. The method is suitable for evaluating the similarity of the fingerprints of the Prunella vulgaris aqueous extracts,and provides a basis for the evaluation of the aqueous extract of Prunella vulgaris.
关键词:analytical quality by design;Prunella vulgaris aqueous extract;caffeic acid;rosmarinic acid;salviaflaside;quantitative fingerprint;HPLC
摘要:This paper has developed a miniature multi-channel portable electrochemical measurement device,which can realize real-time online content detection of multi-component substances in human sweat. This device has the advantages of multi-channel,low cost and portability,and can simultaneously perform two-channel current-time curve and three-channel open-circuit potential-time curve tests. The paper elaborates on the design idea of the device and the issues that need attention in the design of miniaturized electrochemical measurement devices.This device can obtain four different gains by adjusting the Current-to-Voltage Converter(I-V) resistor,with a current measurement range of 10 pA-100 μA,an applied potential range of ±1.25 V,an applied potential accuracy of less than 1 mV,an open-circuit potential measurement range of ±1.25 V,and a potential resolution of up to 0.1 mV,which meets the online detection needs of most screen-printed electrodes. The output accuracy of the excitation signal and the sampling accuracy of the analog signal of the circuit have been tested and verified .Solid-state potassium ion-selective electrodes were prepared using GC/rGO-MoO₃ and rGO synthesized by members of the research group as transduction layers to measure the open-circuit potential function,and glucose and lactic acid sensors were fabricated to verify the current-time curve test effect of the device. At the same time,the device was used to actually verify the changes in the content of sweat components(glucose,lactate,K+,Na+,pH value) during human exercise. The results show that the miniature multi-channel portable electrochemical measurement device not only reaches the practical level in technical parameters,but also its successful application in sensor adaptability and actual detection of human sweat fully proves its great potential in the field of real-time monitoring of physiological indicators,providing a solid technical support for the subsequent development of more advanced wearable health monitoring equipment and the promotion of personalized health management.
摘要:Single-crystal X-ray diffraction(SCXRD) serves as the core technique and gold standard for the structural determination of chiral small-molecule crystals,providing direct,visualizable three-dimensional molecular structures at atomic resolution. Leveraging the anomalous scattering effect of X-rays,SCXRD uniquely and unambiguously determines the absolute configuration of molecules,clearly distinguishing enantiomers(e.g.,R/S configuration). Using the standard crystal C12H13Cl3O as an example,this study optimized its SCXRD testing conditions by varying five key parameters:data collection strategy,crystal-to-detector distance,data collection temperature,exposure time per frame,and crystal size. The aim was to enhance diffraction data quality and determine the optimal main instrument settings for the structural determination of small-molecule chiral single crystals using the Agilent SuperNova diffractometer.
关键词:X-ray single crystal diffraction;chiral small molecules;test conditions;C12H13Cl3O single Crystal
摘要:The inorganic elements in Citrus grandis exocarpium(Huajuhong) from Huazhou(Guangdong),Guangxi,and Hunan provinces were analyzed in this study by using inductively coupled plasma mass spectrometry(ICP-MS). Differences between the origins were investigated through chemical pattern recognition methods to establish an origin discrimination method for Exocarpium Citri Grandis. Following microwave-assisted digestion with nitric acid,the contents of 44 mineral elements in 30 batches of Exocarpium Citri Grandis samples from these three regions were determined by ICP-MS. Compared to Hunan samples,samples from Huazhou(Guangdong) exhibited differences in 37 elements; compared to Guangxi samples,differences were observed in 26 elements. Sample data were subjected to principal component analysis(PCA) and orthogonal partial least squares-discriminant analysis(OPLS-DA) using SIMCA-P 14.1 software. The results revealed distinct clustering of samples from the three producing regions. The models demonstrated good stability,strong predictive ability,and no overfitting. Grouping analysis of calibration set and validation set samples using the predictive function achieved 100% accuracy in both sets. This study establishes a discrimination method for Exocarpium Citri Grandis origins,providing a scientific basis for origin traceability of genuine medicinal materials and market supervision.
关键词:Citrus grandis exocarpium;inductively coupled plasma mass spectrometry(ICP-MS);geographical origins;mineral elements;differences
摘要:A solid-phase extraction(SPE) coupled with gas chromatography-mass spectrometry(GC-MS) method was developed for the determination of migration amounts of seven organic phosphate esters(OPEs). By optimizing parameters including the pH of the migration solution,volume of washing solvent,as well as the type of elution solvent,the results demonstrated that the seven OPEs exhibited good linearity within the range of 0.05-5.0 μg/mL(r²>0.999). Under the optimized conditions for sweat matrix(pH 4.0,10 mL sample loading,5 mL ultrapure water washing,and 5 mL ethyl acetate elution),the recoveries were ranged from 81.6% to 108% with relative standard deviations(RSDs) not more than 15%. For saliva matrix under optimized conditions(pH 4.0,10 mL sample loading,5 mL methanol elution),the recoveries were between 84.1% and 110% with RSDs not more than 14%. Both the method limit of detection of the two matrixes were 0.08 mg/kg for seven OPEs. This method was subsequently applied to commercially available polylactic acid(PLA) products(straws,towels,clothing) and stimulate positive samples. The target analytes were not detected in the actual commercial samples. However,among the stimulate positive samples,migration was only observed for tris(2-chloroethyl) phosphate(TCEP) in the spiked straws,with a migration rate of 3.75%. These findings indicate that the developed method holds significant application potential for analyzing OPE migration amounts in PLA products.
摘要:An ultrasonic assisted extraction method combined with high performance liquid chromatography-evaporative light scattering detector(HPLC-ELSD)was established to analyze and detect seven water-soluble sugars in tobacco flavorings. The extraction effects of water-soluble sugars by ultrasonic-assisted extraction,microwave-assisted extraction,vortex extraction and heating reflux were optimized and compared. The pretreatment conditions were determined as ultrasonic assisted extraction with 40%(volume fraction) acetonitrile-water solution for 15 min. Rhamnose,fructose and sorbitol showed good linearity within the range of 32.0-500.0 mg/L,with relative standard deviations(RSDs) of 3.1%-3.6%. Xylose,glucose and sucrose showed good linearity within the range of 75.0-750.0 mg/L,with the RSDs of 2.8%-3.9%. The linear range of maltose was 75.0 to 1 500.0 mg/L,and the RSD was 8.5%. The detection limit range of seven water-soluble sugars was between 8.0 and 17.0 mg/L. And recoveries of the spiked samples were in the range of 72.1%-128%,with RSDs all not more than 9.7%. This method was applied to the detection of water-soluble sugars in nine tobacco flavorings. The results showed that the concentration of sugar substances in the concrete was higher than that in the tincture,and there were relatively few sugar substances in the essential oil. This method can be used for the analysis and detection of water-soluble sugars in batches of tobacco flavorings due to the advantages of simple operation,short time consuming and good accuracy.
摘要:Due to their extensive use in the prevention and treatment of diseases in crops caused by the genera peronosporales and phytophthora,dimethomorph and fluopicolide have high detection rates in fruits and vegetables,posing potential risks to human health and environmental safety. Therefore,establishing a rapid,accurate,and visualization-compatible on-site detection method is crucial. In this study,we successfully developed a colloidal gold immunochromatographic assay(GICA) by conjugating broad-spectrum monoclonal antibodies with colloidal gold as recognition elements,and utilizing the aggregation of gold nanoparticles in the detection areas as the visual signal readout. The GICA achieved simultaneous qualitative and quantitative detection of dimethomorph and flumorph. The results indicate that under optimal conditions,the quantitative detection limit was 0.50 to 0.59 ng/g for dimethomorph in fruit and vegetable samples,with a detection range was 0.50 to 10 ng/g and a naked-eye cutoff value was 4 ng/g. For flumorph,the quantitative detection limit was 0.63 to 1.06 ng/g,and the detection range was 0.50 to 10 ng/g,and the naked-eye cutoff value was 8 ng/g. Additionally,the average spiked recovery rate for both samples was between 75.0% and 118%,which is consistent with the results obtained by HPLC-MS/MS(r2=0.97). The method exhibits excellent specificity with a cross-reactivity rate of less than 0.1% for other functionally similar substances,and it can accurately complete the qualitative or quantitative detection of the target analytes within 10 minutes,making it suitable for rapid screening of dimethomorph and flumorph in a large number of fruit and vegetable samples.
摘要:Addressing the challenges of the lack of detection methods and severe matrix interference for mineral oil aromatic hydrocarbons with three or more rings(3P-MOAH) in printing inks,this study developed a quantitative analytical method based on multi-stage purification coupled with liquid chromatography-gas chromatography-hydrogen flame ionization detection. Through solvent extraction,silica gel column and amino column purification technology,mineral oil saturated hydrocarbons,1-2 ring mineral oil aromatic hydrocarbons and olefin interfering components in the ink are effectively removed. An optimized gradient elution program(n-hexane/dichloromethane system) on the amino column achieved online separation of three or more rings in mineral oil aromatic hydrocarbons. The methodological investigation results indicated that the quantification limit reached 1.0 mg/kg,and the recoveries ranged from 82.3% to 109% with RSD ranged from 7.6% to 9.7%. This research provides a practical solution for the quantitative detection of three or more rings in mineral oil aromatic hydrocarbons in printing inks. The findings offer a reliable analytical tool for the safety assessment of printing inks and food contact materials.
关键词:printing ink;liquid chromatography-gas chromatography;mineral oil aromatic hydrocarbons with three or more benzene rings;determination