摘要:The continuous innovation in display technology is crucial for the development of the information industry. As an emerging type of monolithic integrated driving and light-emitting device,organic light-emitting transistor(OLET) have attracted considerable attention due to their integration of the switching/amplification functions of organic field-effect transistors and the light-emitting characteristics of organic light-emitting diode within a single device architecture. This article reviews the latest advancements in OLET technology in terms of material innovation and device design. In the field of high mobility emissive organic semiconductors,the bottleneck of balancing high mobility with strong luminescence has been successfully overcome through strategies including molecular structure design and aggregation state optimization. In terms of the device performance,leveraging the unique open-plane light-emitting characteristics and gate-voltage modulation mechanism of OLET,highly polarized emission(with a degree of polarization up to 0.97) and ultranarrow spectral emission(with a full width at half maximum as low as 13 nm) have been achieved. These breakthroughs provide a novel technological pathway for the development of next-generation high-performance,multifunctional integrated display technologies,demonstrating the significant potential of OLET in driving the evolution of display technology.
摘要:The clinical diagnosis of ALS lacks early biomarkers,and the complexity of peripheral blood components makes it difficult to directly reflect pathological changes. Blood exosomes,which stably carry protein information from their source cells,provide a window for non-invasive disease monitoring. SUMOylation is a crucial post-translational modification that plays a key regulatory role in disease. However,the characteristics of SUMO-1 modification in the blood exosomes of ALS patients remain unclear. To address this,this study utilized an affinity ligand(CP-1) screened via phage display technology to synthesize a specific enrichment material(M2). Combined with LC-MS/MS,a proteomic analysis of SUMO-1 modifications was performed on blood exosomes from 4 early-stage and 4 mid-to-late-stage ALS patients. A total of 119 SUMO-1-modified proteins were identified. The overall abundance of these modified proteins was significantly higher in middle-to-late-stage patients compared to early-stage patients,and they were primarily enriched in the chemokine signaling and HIF-1 signaling pathways. These findings suggest that exosomal SUMO-1 modification may be involved in the pathological process of ALS,providing new clues for understanding the disease mechanism.
摘要:This study employed a high-fat diet(HFD)-induced hyperlipidemia mice model to systematically evaluate the lipid-lowering and hepatoprotective effects of Microctis Folium and to elucidate its regulatory mechanism on the arginine-proline-polyamine metabolic axis using integrated untargeted and targeted metabolomics. Serum untargeted metabolomics was performed using UPLC-QTOF-MS/MS to screen for differential metabolites and conduct pathway enrichment analysis. Subsequently,targeted metabolomics based on UPLC-TQ-MS/MS was employed to quantify key metabolites including L-arginine,proline,creatine,and polyamines(spermidine and spermine). Microctis Folium significantly reduced TC,TG,and LDL-C levels and decreased ALT and AST while increasing HDL-C across dose groups. Untargeted metabolomics revealed broad metabolic disturbances induced by HFD,with significant enrichment of arginine and proline metabolism;differential metabolites mainly involved amino acids and derivatives,polyamines,creatine-related metabolites,as well as lipids and organic acids. Microctis Folium treatment globally reversed these metabolic abnormalities. Targeted quantification further confirmed that L-arginine,proline,creatine,and polyamines(spermine/spermidine) were decreased in the model group,and Microctis Folium markedly restored their levels toward those of controls. Collectively,Microctis Folium exhibits pronounced lipid-lowering and hepatoprotective activities,which may be mediated by modulation of the arginine-proline-polyamine metabolic axis and associated metabolic remodeling of nitrogen and energy metabolism,thereby promoting restoration of metabolic homeostasis. These findings provide metabolomics-based evidence for the mechanism of action of Microctis Folium and support future screening of its bioactive constituents and translational development.
摘要:In this study,a tertiary amine silane coupling agent bearing bis[3-(trimethoxysilyl)propyl] groups was first synthesized via the nucleophilic ring-opening reaction of N,N'-dimethyl-1,3-propanediamine with KH560(γ-glycidoxypropyltrimethoxysilane),which was then grafted onto the surface of silica gel. Subsequently,the silane coupling agent-bonded silica microspheres were further reacted with 1,3-propanesultone to afford a bidentate-bonded silica chromatographic stationary phase(denoted as Sil-SAI). Fourier transform infrared spectroscopy(FT-IR) and elemental analysis(EA) confirmed that the Sil-SAI stationary phase was successfully modified with sulfobetaine zwitterionic and tertiary amine bifunctional groups.Furthermore,the separation mechanism of the Sil-SAI column,the effects of buffer salt concentration and pH value of the mobile phase on chromatographic retention behavior,as well as the hydrolytic stability of the stationary phase were systematically investigated. The results indicated that:Sil-SAI exhibits a typical hydrophilic interaction liquid chromatography(HILIC) separation mechanism. Owing to the multiple interactions(including hydrophilic interaction,electrostatic interaction,hydrogen bonding,and dipole-dipole interactions) between probe molecules and the Sil-SAI stationary phase,this stationary phase presents a mixed separation mechanism involving both partition and adsorption processes;With variations in the concentration and pH of the buffer salt in the mobile phase,the neutral,acidic,and basic probe molecules display distinct chromatographic retention behaviors;Benefiting from its bidentate bonding structure,the Sil-SAI stationary phase possesses superior hydrolytic stability.The application of Sil-SAI stationary phase for the separation of six sugars and seven sugar alcohols demonstrated excellent separation efficiency and satisfactory separation reproducibility for all analytes.
摘要:Gas chromatography-ion mobility spectrometry(GC-IMS) was employed to analyze the volatile components of Cyperi Rhizoma from different origins. Partial least squares-discriminant analysis(PLS-DA) was applied to screen differential characteristic components. Based on these characteristic components,9 machine learning algorithms such as SVM-L were constructed to develop rapid discrimination models for Cyperi Rhizoma from different origins. Fifty-nine volatile compounds were identified in Cyperi Rhizoma decoction pieces from five provinces,including alcohols,esters,aldehydes,ketones,and unsaturated hydrocarbons. Ten characteristic components were screened by PLS-DA analysis,such as 1,4-dimethylbenzene,3-methyl-1-pentanol,and ethyl acetoacetate. Furthermore,nine machine learning models all demonstrated excellent predictive performance(Accuracy=1),indicating good potential for practical application. This study provides a simple and rapid method for discrimination and identification of Cyperi Rhizoma from different geographical origins,while also offering a reference for establishing a quality evaluation system for Cyperi Rhizoma.
摘要:The identification of HN-DNA adducts formed in animals after exposure to nitrogen mustards(NMs,codenamed HN) enables the traceability and confirmatory analysis of HN exposure. Six-week-old Sprague-Dawley(SD) rats,with a mean weight of approximately 200 g,were given intraperitoneal injections of HN1,HN2,and HN3,respectively,to establish an exposure animal model. The nitrogen mustard exposure groups(0.3 LD50,0.5 LD50,or LD50 exposure dose) as well as a blank solvent control group were set up. A high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) method employing multiple reaction monitoring(MRM) mode was established to quantitatively analyze the types and concentrations of HN-DNA adducts in rat urine samples. The results demonstrated a good linearity for the 12 HN-DNA adduct standards within the concentration range of 0.02-500 ng/mL,with limits of detection(LODs) of 0.01-0.02 ng/mL and limits of quantification(LOQs) of 0.02-0.05 ng/mL. The relative standard deviations(RSDs) of intra-assay and inter-assay precision were less than 15%. Urine analysis of HN-exposed SD rats at 12 hours post-exposure revealed the presence of HN-AN3,HN-GN7,HN-GO6,and HN-Bis-GN7 adducts,with concentrations decreasing in the order of HN-GN7>HN-Bis-GN7>HN-AN3>HN-GO6. The concentrations of the four DNA adducts demonstrated a dose-dependent positive correlation and a gradual decrease over time. The application of HPLC-MS/MS technique to detect these urinary DNA adducts allows for the non-invasive early detection,accurate traceability,and damage assessment of HN exposure. These findings provide an experimental basis for further study of HN-induced DNA damage repair processes and mechanisms.
关键词:nitrogen mustard;DNA adducts;biomarker;traceability analysis;high-performance liquid chromatography-tandem mass spectrometry
摘要:A detection method based on dispersive solid phase extraction coupled with ultra-performance liquid chromatography-tandem mass spectrometry(d-SPE/UPLC-MS/MS) was established for the simultaneous determination of 19 chemical components in roasted coffee. This method compared the effects of solvent type,feed-to-solvent ratio,solvent pH value,ascorbic acid concentration,ultrasonication time,and the type and amount of adsorbent used as the packing material for sample purification. The optimal experimental conditions selected were a solid-liquid ratio of 1∶10,with 70% ethanol aqueous solution at pH 2 as the extraction solvent,the ascorbic acid concentration was 5 mg/mL,ultrasound time of 60 minutes,and purification packing consisting of 60 mg octadecylsilane(C18),30 mg diatomaceous earth(DE),and 20 mg primary secondary amine(PSA). Using a 0.01% formic acid aqueous solution and a 0.01% formic acid methanol as the mobile phase,separation was achieved within 6 minutes using a Kinetex PFP column(100 mm×3 mm,2.6 μm). The validation results demonstrated an excellent linear relationship for all 19 compounds across the concentration range of 0.2-5 000 μg/L(r²>0.995). The verification results show that,with the exception of malic acid(LOD is 100 μg/L;LOQ is 200 μg/L),the limits of detection(LODs) and limits of quantification(LOQs) for the other 18 compounds range from 0.1 to 20 μg/L and 0.2 to 50 μg/L,respectively. The recoveries for spiked samples at three concentration levels ranged from 73.2% to 111%,with relative standard deviations ranging from 1.4% to 11%. This method was applied to the analysis of 21 batches coffee samples from Yunnan with different processing combinations(variety×processing method×roasting degree),and combined with principal component analysis(PCA) for statistical analysis. The results indicated that among the measured chemical components,Yellow Bourbon has the highest total sum,in addition,the content of the majority of phenolic acids contained in coffee beans tends to decrease gradually as the degree of roasting increases. For the part of flavonoids,which mainly include catechin and epicatechin,tends to increase steadily with the degree of roasting. This research not only provides a specific technical method for detecting chemical components in Yunnan coffee but also offers reliable theoretical support for the processing procedures and production practices of high-quality coffee.
摘要:To address the odor issue in surface water,a method for the simultaneous determination of 64 odor-causing substances in surface water was established based on headspace arrow solid-phase microextraction coupled with gas chromatography-triple quadrupole mass spectrometry(HS-SPME Arrow/GC-MS/MS). The targeted odor-causing substances cover multiple categories,including typical algal-derived and industrial-derived ones such as sulfides/thiols,halohydrocarbons/aromatic hydrocarbons,terpenes,pyrazines,esters,phenols,aldehydes and ketones,ethers,and amines. Single-factor experiments were conducted to investigate the effects of parameters,including SPME fiber type,extraction time,extraction temperature,incubation time,and sodium chloride(NaCl) addition amount,on the extraction efficiency of the 64 odor-causing substances. The results indicated that the optimal conditions were as follows:after introducing 1.80 g NaCl to 5.0 mL solution,the bottle was incubated for 5 min at 60 ℃,then a DVB/CAR/PDMS(divinylbenzene/carboxen/ polydimethylsiloxane) SPME fiber was used for the extraction for 30 min.The limits of detection for the 64 odor-causing substances ranged from 0.92 to 29.06 ng/L,with all linear correlation coefficients(r2) greater than 0.990 in the linear range of 5.0-2 000 ng/L. At three spiked concentration levels,the average spiked recoveries ranged from 60.1% to 134%,and the relative standard deviations(RSDs) varied between 1.8% and 21%. When this method was used to detect 5 surface water samples from Shanghai,methyl sulfide(5.13-18.04 ng/L),methanethiol(6.58-25.12 ng/L),and 2-methylisoborneol(2-MIB,11.13-11.42 ng/L) were detected,respectively.This method is characterized by automated sample pretreatment,and can be applied to the high-throughput rapid screening of odor-causing substances in surface water.
关键词:SPME Arrow;GC-MS/MS;odor-causing substances;surface water
摘要:Carbon quantum dots(CQDs) are a type of nanomaterial with excellent luminescent properties and have promising applications in various fields. Green fluorescent carbon quantum dots(g-CQDs) were synthesized by a solvothermal method using pomegranate juice as the carbon source and absolute ethanol as the solvent. The structure and optical properties of g-CQDs were characterized by UV-Vis absorption,fluorescence spectroscopy,FTIR and TEM. The results showed that g-CQDs had an average particle size of approximately 2.96 nm,with abundant surface functional groups such as hydroxyl and carboxyl groups,exhibiting good water dispersibility and fluorescence stability. Under excitation at 410 nm,g-CQDs emit green fluorescence at 500 nm with a quantum yield of 15.24%. The fluorescence of g-CQDs was quenched by Fe3+ and Fe2+,and the quenching mechanism mainly involves photo-induced electron transfer resulting from surface coordination. The detection limits of Fe2+ are 0.155 µmol/L(linear range 1.25-18 µmol/L) and 0.221 µmol/L(linear range 18-50 µmol/L),respectively. The detection limit of Fe3+ within the linear range of 2.5 to 72.5 µmol/L is 0.211 µmol/L. It can be concluded that g-CQDs has sensitivity for Fe3+ and Fe2+. The antibacterial experiments indicated that g-CQDs exhibited inhibitory effects on mold growth,with the antibacterial activity increasing at higher concentrations . This study provides a reference for the green synthesis of multifunctional CQDs and their applications in ion detection and antibacterial fields.
摘要:The volatile components in different parts(root,fruit,leaflet,old leaf,tender stem and old stem) of Rubus chingii Hu(R.chingii) were determined by headspace gas chromatography ion mobility spectrometry(HS-GC-IMS). By focusing on the differences of volatile components in six different parts of R. chingii,combined with principal component analysis,partial least squares discriminant analysis and cluster heat map,the differences of volatile components in different parts were studied. The results showed that a total of 128 volatile components were obtained from six different parts,92 of which were identified,including 23 alcohols,28 aldehydes,13 ketones,and 8 esters,etc.;GC-IMS fingerprints showed that the volatile components in six different parts were similar,but the content difference was obvious. According to VIP>1.2,17 different components such as(E)-2-hexenal-D,methyl acetate and 3-methylbutanol-D were screened out. The differences of volatile components in different parts of R. chingii were analyzed,which provided a new method for rapid and accurate identification of volatile components in different parts of R. chingii.
摘要:β2-microglobulin is an important biomarker for early renal impairment in diabetic kidney disease,and its rapid and accurate quantification is essential for early diagnosis and disease monitoring. In this study,a latex-enhanced immunoturbidimetric reagent system for the quantitative detection of β2-microglobulin was constructed. Immunolatex was prepared by conjugating β2-microglobulin antibody to the surface of carboxylated polystyrene latex microspheres,and the immune complex was formed in the presence of the antigen,resulting in turbidity changes of the solution,thereby enabling quantitative determination of β2-microglobulin. The reagent system was further integrated with a self-developed smartphone-based immunoturbidimetric detection platform,using the built-in ambient light sensor for portable signal acquisition and analysis. The detection system showed a good linear relationship in the range of 0-60 mg/L,and the limit of detection was 0.85 mg/L. The spike recovery ranged from 93.5% to 106%,and the coefficient of variation between batches was 5.7%-9.9%,demonstrating good accuracy,repeatability and specificity. The test results of self-made reagents were consistent with commercial reagents(r²=0.988 4),and the correlation coefficient between the detection results of the smartphone immunoturbidimetric platform and the microplate reader was 0.993 5. The latex-enhanced immunoturbidimetric reagent combined with the smartphone detection platform has the advantages of easy operation,fast detection,low cost and strong portability,providing a promising point-of-care testing solution for rapid detection of diabetic kidney disease biomarkers.
摘要:To meet the requirement for rapid and highly sensitive detection of fipronil,this study systematically compared four known aptamer sequences and selected the aptamer with the highest affinity for fipronil. Based on this,a sensitive fluorescence detection method for fipronil has been established by utilizing the property of Exonuclease I to specifically hydrolyze single-stranded DNA and the significant fluorescence enhancement of the aggregation-induced emission molecule DSAI upon binding to the aptamer. The linear range of this method for the detection of fipronil was 1.00-12.50 nmol/L and the limit of detection was 2.23 nmol/L. In the detection of practical samples (cabbage,corn,and tap water),the average recoveries ranged from 89.2% to 107%,with relative standard deviations between 0.80% and 4.3%. The experimental findings indicate that the developed sensor exhibits high sensitivity and excellent selectivity,suggesting substantial potential for its application in the rapid screening of pesticide residues.
摘要:Accurate determination of trace gold in geochemical exploration samples is crucial for geological prospecting. Aiming at the problems of low mass transfer efficiency and cumbersome operation of the traditional activated carbon enrichment method,as well as the technical gap in its coupling with flame atomic fluorescence spectrometry(FAFS),this study established a novel detection system integrating tetraacid digestion,activated carbon enrichment and FAFS. An innovative synergistic strategy was adopted,which combined mass transfer enhancement by a vortex mixer with rapid clarification by a high-speed centrifuge. Meanwhile,activated carbon was pretreated with the combined system of ammonium hydrogen fluoride and hydrochloric acid,and the key process parameters were optimized as 30 min for enrichment and 20 min for desorption with thiourea at(50±5) ℃,thus realizing the efficient coupling of activated carbon and FAFS for the first time. The results showed that,the limit of detection(LOD) and limit of quantitation(LOQ) of the method were 0.07 ng/g and 0.14 ng/g,respectively,which were superior to those of the standard method(DZ/T 0279.35-2022). For six national first-class certified reference materials,the relative standard deviations(RSDs) of the determination results were in the range of 4.4% to 11%,and the absolute value of the relative error ranged from 2.7% to 5.1%,showing no significant difference from the standard method. This method has the advantages of controllable cost and high analysis efficiency,which fills the relevant technical gap and provides a reliable new approach for the accurate determination of trace gold in geochemical exploration samples.
摘要:In this study,a hydrophobic paper-based SERS sensor for the detection of miR-943 in the serum of cerebral infarction(CI) patients was constructed based on silver nanocubes(Ag NCs) and CRISPR/Cas13a trans-cutting strategy. Ag NCs were assembled on hydrophobic paper to initially construct the SERS substrate,and single-stranded DNA(ssDNA) modified with Cy5 signaling molecule was immobilized onto the hydrophobic paper SERS substrate through Ag—S bonding to construct the hydrophobic paper SESR sensor. When the target miR-943 was present,specific activation of the trans-cutting ability of CRISPR/Cas13a and nonspecific cleavage of ssDNA kept Cy5 away from the hydrophobic paper SERS substrate indicated that resulted in a decrease in the SERS intensity of the characteristic peak of Cy5 at 1 468 cm-1. The sensor exhibited good linearity in the range of 10 amol/L to 10 pmol/L(r²=0.986),with a low limit of detection(LOD) of 1.55×10-17 mol/L and excellent specificity and reproducibility.The detection results of clinical samples were highly consistent with qRT-PCR. Therefore,this method provides a reliable and highly promising assay for the early,noninvasive diagnosis of cerebral infarction.
摘要:A novel compound was screened out in 3 batches of food products by high resolution mass spectrometry,and the mass spectrometry data of the compound showed that it was a vardenafil derivative. NMR spectroscopic characterization demonstrated the evidence of coexisting cis-trans tautomerism of the compound,which resulted in the molecular structure of the compound difficult to identify. Subsequently,according to combining with molecular formula search of Chemspider database,3 vardenafil analogs were finally locked among 32 isomers. Further compared the data of the suspected compound with commercial standard,it was finally confirmed as vardenafil derivative KD-027. The results of quantitative analysis by ultra-high performance liquid chromatography-tandem mass spectrometry revealed that KD-027 was well regressed with the mass concentration,and correlation coefficient(r2) was 0.999 6 in the range of 1.0-100 ng/mL. The limit of detection and limit of quantitation were 20 μg/kg and 50 μg/kg,respectively. An average recoveries of 86.2%-115% at low,medium and high spiked levels in the matrix of liquor,pressed candy and solid beverage were obtained,with relative standard deviations(RSDs) of 2.7%-7.3%. The method was used to detect actual samples,and KD-027 was detected in two batches of pressed candies and one batch of solid beverage,with content ranged of 482-2 707 mg/kg. This method could provide a technical reference for the efficient detection of exogenous illegal additives in food.
关键词:vardenafil structural derivatives;structure identification;molecular formula search;Chemspider database;quantitative analysis
摘要:Chiral separation plays a pivotal role in pharmaceutical development and food analysis,as the enantiomeric composition of chiral compounds can critically influence their biological activity and safety. However,conventional chiral stationary phases often suffer from limited enantioselectivity and an inherent trade-off between separation resolution and column efficiency,which hampers their performance in high-resolution chromatographic applications. In this work,a stepwise post-synthetic modification strategy was developed to anchor quinine(QN) sequentially and 1,3-propanesultone(PS) within the nanochannels of a covalent organic framework(COF),yielding a chiral COF material with multiple cooperative interaction sites(denoted as QN-PS COF). The modified COF was subsequently immobilized onto porous silica microspheres via an in situ coating approach to fabricate a novel chiral stationary phase(QN-PS COF@SiO2) for high-performance liquid chromatography(HPLC). The resulting column enabled effective resolution of nine chiral compounds with diverse structural features,demonstrating broad applicability. In addition,the QN-PS COF@SiO₂ column exhibited excellent reproducibility and operational stability over repeated injections. Molecular simulation studies revealed that the enhanced chiral recognition arises from the well-defined chiral microenvironment generated by the synergistic integration of quinine and propanesultone moieties within the confined COF nanochannels,which collectively strengthen stereoselective interactions. Overall,this study provides a COF-based strategy for the rational design of high-performance chiral stationary phases and contributes to the development of efficient and versatile enantioseparation materials.
摘要:A color latex microsphere-based immunochromatographic assay was developed for the rapid detection of chromium using a monoclonal antibody. Firstly,chromium haptens were synthesized by coupling them with carrier proteins via the isothiocyanate method to prepare complete antigens(immunogen and coating antigen). The complete antigens were used to immunize mice,and spleen cells were fused with myeloma cells to obtain a monoclonal antibody(4G9) specifically recognizing chromium. The results showed that the IC50 value of monoclonal antibody 4G9 was 21.9 ng/mL,and its cross-reaction rates with other heavy metals,including Cd,Pb,Hg,As,Cu,Fe and Ni,were all below 0.3%. Based on this antibody,the conditions of the color latex microsphere immunochromatographic assay including antibody dosage,T-line coating concentration,probe loading,and pH of the detection system were optimized. Under the optimum conditions,the limit of detection(LOD) of the test strip for chromium was 0.95 ng/mL,and the linear detection range was 0.78-25 ng/mL. For real asparagus samples,the LOD was 5.15 ng/mL,with spiked recoveries ranging from 75.3% to 119% and relative standard deviations below 10%. These results indicate that the established immunochromatographic assay possesses high specificity and sensitivity and can be applied to the rapid detection of chromium residues in actual samples.
关键词:heavy metal chromium;monoclonal antibody;immunochromatography;test strip
摘要:As light crude oil resources become increasingly scarce,residue cracking processes have emerged as a vital means of securing light oil supplies. However,the presence of silicon in residue oil poisons catalysts,leading to a decline in light oil yield. Consequently,developing a rapid method for detecting silicon in residue oil is of great significance for improving residue conversion efficiency. To address the challenge of quantifying trace amounts of the non‑metallic element silicon in residue oil,this study proposes a quantitative analytical approach combining laser‑induced breakdown spectroscopy(LIBS) with chemometric algorithms. LIBS spectral data were first acquired from residue oil samples. The influence of five pre‑processing methods and their various combinations on the predictive performance of partial least squares regression(PLSR) models was then systematically evaluated,with leave‑one‑out cross‑validation employed to identify the optimal spectral pre‑processing strategy. On this basis,three interval variable selection methods were applied to further refine the spectral feature variables,leading to the development of a quantitative model tailored for predicting silicon content in residue oil. The results demonstrate that the residue oil samples analysed with the WT‑D1st‑biPLS model achieve the best predictive performance,with an optimal root mean square error of prediction(RMSEP) of 0.078 9 mg/kg,an R‑squared for prediction(R2P) of 0.989 2,and a mean relative error of prediction(MREP) of 4.7%. In summary,the proposed method offers a theoretical foundation for the rapid on‑site quantitative analysis of non‑metallic elements in residue oil.
关键词:laser-induced breakdown spectroscopy;chemometrics;residual oil;trace elements;non-metallic elements
摘要:For toner,lotion,cream,and oil-based cosmetic matrices,the sample preparation was performed using acetonitrile containing 1% formic acid extraction combined with EMR-Lipid solid phase extraction column purification. Ultra-high performance liquid chromatography-tandem mass spectrometry detection was performed through dynamic multiple reaction monitoring mode,achieving trace determination of 86 doping substances in cosmetics. In this method,norfenefrine and octopamine showed a linear relationship within the range of 2 to 150 μg/L(r2>0.990),while heptaminol,hydromorphone,methcathinone,oxilofrine and solriamfetol were linear within the range of 2 to 200 μg/L(r2>0.990). The remaining 79 target substances had a good linear relationship within the range of 2 to 400 μg/L(r2>0.990). The detection limit of this method was 0.012 5 to 125 μg/kg,with recoveries ranging from 80.0% to 120% and relative standard deviations not more than 20%,meeting the methodological requirements.In addition,this method has detected high contents of caffeine(112.01,500.90,242.95,168.12,416.77 μg/kg) and ephedrine(531.75,33.22 μg/kg) in actual sample tests. Ephedrine was found in all the cream products containing a large amount of plant extracts. This method is simple to operate,highly sensitive and accurate,and is suitable for the rapid screening and quantitative analysis of multiple stimulants and anesthetics in cosmetics. It provides strong technical support for preventing athletes from being exposed to products contaminated with stimulants and anesthetics,ensuring the safety of athletes from doping in competitions.
关键词:ultra-high performance liquid chromatography-tandem mass spectrometry;dynamic multiple reaction monitoring;doping substances;cosmetics
摘要:A method for rapid determination of 16 polycyclic aromatic hydrocarbons in lubricating oil was established based on gas purge microsyringe extraction(GP-MSE) device. The sample was fully evaporated at a constant temperature of 280 ℃,and then transferred to -10 ℃ dichloromethane using N2 as a carrier gas for low-temperature capture. After the extraction solution was made to volume,gas chromatography-mass spectrometry analysis was performed,and an external standard method was adopted for quantitative analysis. The results indicated that 16 PAHs had a good linear relationship within the mass concentration range of 0.1 mg/L to 50.0 mg/L,with the correlation coefficients(r2) exceeding 0.999. The detection limits and quantitation limits of 16 PAHs were 0.014-0.035 mg/kg and 0.046-0.116 mg/kg,respectively. The average recoveries of 16 PAHs at three spiked levels in different sample matrices ranged from 81.2% to 98.6%,with relative standard deviations(RSDs,n=6) of 1.6% to 7.9%. The method is quick,easy,accurate and sensitive,which is suitable for determination of PAHs in lubricating oil.
摘要:A detection method for 5 endogenous metabolites in serum from cyclophosphamide-induced immunosuppressed rats was established using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). After protein precipitation,the samples of serum were separated on an ACQUITY Poroshell 120 SB-C18(2.1 mm×100 mm,2.7 μm) column with methanol-5 mmol·L-1 ammonium acetate aqueous solution as the mobile phase by gradient elution for the detection of glutathione,DL-glutamine,glutamic acid,and arachidonic acid;then an ACQUITY UPLC BEH Amide(2.1 mm×150 mm,1.7 µm) column with acetonitrile-5 mmol·L-1 ammonium formate aqueous solution as the mobile phase by gradient elution for the detection of LPC(0-16∶0). The electrospray ionization(ESI) mass spectrometer was operated in positive and negative ion mode and an internal standard method was used for quantification. The 5 metabolites had a good linear relationship within the corresponding mass concentration range(r>0.995),with detection limits of 0.043-0.178 ng·mL-1 and quantification limits of 0.145-0.592 ng·mL-1. The method is simple,fast and sensitive,and it is suitable for the detection of endogenous metabolites in rats'serum samples,and to provide experimental basis for the mechanism research of immunosuppressive drugs.
关键词:ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS);serum;endogenous metabolites;immunosuppression
摘要:An analytical method combining modified QuEChERS with UPLC-MS/MS was established for the determination of 14 organic dyes. The samples were extracted with acetonitrile,and purification was completed simultaneously using neutral aluminum oxide. Chromatographic separation was performed on an BEH C18 column with a gradient elution of 10 mmol/L ammonium acetate(pH adjusted to 4.5±0.1 with formic acid) and 0.1% formic acid in acetonitrile. All compounds were detected in positive electrospray ionization mode using multiple reaction monitoring. Except for malachite green and leucomalachite green,which were quantified using the internal standard method,the remaining compounds were quantified by matrix-matched external standard method. The results showed that the 14 dyes exhibited good linear relationships in the range of 0.2-10 μg/L(r²>0.995). The detection limits(LODs) and quantification limits(LOQs) for malachite green,leucomalachite green,crystal violet,and leucocrystal violet were 0.2 μg/kg and 0.5 μg/kg,respectively,while those for the other 10 dyes were 0.5 μg/kg and 1.0 μg/kg,respectively. At three spiked levels(1,5,and 10 μg/kg),the average recoveries of the 14 dyes ranged from 72.6% to 118%,with relative standard deviations(RSDs) not more than 8.8%.By using this method,30 batches of aquatic products were detected. Except for one batch detecting methylene blue(detected content:1.10 μg/kg),none of the other samples detected the 14 dyes.
摘要:Liquid chromatography-mass spectrometry(LC-MS) combines high separation ability with high sensitivity. It has become a core analysis tool. It is widely used in life science. It is also essential in clinical medicine and environmental science. However,LC-MS produces high-dimensional data. The raw data is complex and contains significant noise. Therefore,efficient data processing algorithms are necessary. These algorithms must be robust. The goal is to convert raw signals into effective scientific information. This paper focuses on the data processing workflow. It highlights three key tasks. The first task is signal extraction. The second task is spatiotemporal alignment. The third task is substance identification. This review analyzes the methodological evolution of these tasks. It also explores their internal logic deeply. Furthermore,the study reveals common challenges in current research. One major problem is the lack of algorithm generalization. Another issue is the absence of standardized benchmark datasets. The fragmentation of the software ecosystem is also a critical bottleneck. To address these pain points,specific directions are proposed. One direction is physics-guided artificial intelligence(AI) modeling. Another is the construction of standardized benchmark systems. Algorithm development must integrate instrument mechanisms with data science. This integration is crucial. It aims to build next-generation LC-MS technologies. These technologies should be high-robustness and interpretable. Cloud collaboration is also a key feature for the future.
关键词:liquid chromatography-mass spectrometry;data processing;deep learning;feature extraction;retention time alignment;substance identification
摘要:Trade friction-induced tariff differentials have significantly altered the cost structure of soybean imports,driving fraudulent practices such as origin mislabeling and variety adulteration. These violations pose dual threats to customs supervision and consumer health. Establishing an accurate and efficient technical system for soybean origin traceability has thus become an urgent necessity to safeguard the quality and safety of imported soybeans and to support the sustainable development of the industry. In recent years,chromatographic techniques,mass spectrometry,chromatography-mass spectrometry hyphenated techniques,nuclear magnetic resonance,and spectroscopic methods have demonstrated promising application potential in enhancing the selectivity and sensitivity of soybean origin traceability. This paper systematically reviews the research progress of the aforementioned four categories of techniques,offering a comprehensive overview from the perspectives of technical principles,application cases,advantages,and limitations. The aim is to provide a theoretical reference for the development of a robust soybean origin traceability system.
关键词:soybean;geographical origin traceability;chromatography;mass spectrometry;chromatography-mass spectrometry;nuclear magnetic resonance;spectroscopy
摘要:The explosive growth of the global electric vehicle market has made the recycling and reuse of retired batteries a core link to ensure industrial chain security and achieve the“dual carbon”goals. The hierarchical principle of“prioritizing echelon utilization,with dismantling and recycling as the bottom line”has become the mainstream path for retired battery treatment,as it maximizes the full life cycle value of batteries,and battery State of Health(SOH)assessment is the core prerequisite for the precise implementation of this path. As a key indicator reflecting battery capacity retention, internal resistance and cycle stability,SOH directly determines the residual value of retired batteries and the selection of recycling paths.This paper systematically reviews the five mainstream battery State of Health assessment technologies supporting echelon utilization:state of charge(SOC) enables quantitative real-time assessment of the internal state of batteries,serving as a critical prerequisite for accurate performance estimation. The internal resistance measurement method,with its advantages of online non-destructive testing,is suitable for the initial screening of echelon sorting, and algorithms such as adaptive Kalman filtering can effectively improve its anti-interference ability;the capacity attenuation method,as the“golden standard”,provides an accurate basis for echelon qualification determination,and the incremental capacity curve can assist in identifying aging modes;the model-driven method realizes indirect inference of SOH through mathematical modeling;the data-driven method mines data correlations relying on machine learning;non-destructive testing technologies(especially ultrasonic testing) compensate for the mechanism cognition shortcomings of electrical methods by capturing internal structural changes. Research shows that the above five types of technologies have complementary advantages,jointly constructing a technical system for refined sorting of retired batteries,providing core support for the high efficiency and low carbonization of echelon utilization,and is of great significance for promoting resource recycling in the new energy industry.
摘要:The combination of surface-enhanced Raman spectroscopy(SERS) and mass spectrometry(MS) enables multidimensional analytical strategies for precise identification and confirmation of target compounds,by integrating molecular vibrational fingerprints with ion mass-to-charge ratios and characteristic fragment information. This article systematically reviews the fundamental principles of this hyphenated technique,its online and offline coupling modes,and their complementary mechanisms,highlighting recent research advances in fields such as chemical analysis,reaction monitoring,public safety and health,and pharmaceutical and metabolite analysis. Furthermore,the article examines the current challenges facing this hyphenated approach,including signal reproducibility,quantitative correlation,and methodological compatibility. The advancement of highly stable substrates,the convergence of multimodal imaging,and the implementation of standardized automated workflows are anticipated to drive significant breakthroughs for this technique in spatial omics and complex sample analysis,thereby facilitating its extensive application in diverse real-world scenarios.