摘要:In this study,a new affinity detection and evaluation method is constructed based on the metasurface plasmon resonance(MetaSPR) biosensor,which utilizes a highly sensitive MetaSPR chip and simultaneously constructs a high-precision microfluidic flow-through and high-throughput microtiter plate pipeless affinity detection platform,which makes up for the shortcomings of the existing affinity detection methods.In the study,MetaSPR chips with nanopore array structure were prepared and characterized by scanning electron microscope and enzyme marker for their physical structure and optical properties.The SPR chip was tested by using glycerol solutions with different refractive indexes,and the results showed that the chip was extremely sensitive to changes in refractive index,and a good correlation was presented between the response signal and the change in refractive index(r2=0.995).The kinetic parameters such as binding rate constant(Ka),dissociation rate constant(Kd) and dissociation equilibrium constant(KD) were successfully obtained using the WeSPR series of detector for affinity detection of a variety of molecular pairs without the need for complex optical components and were in agreement with the previously reported data.The results show that both assay platforms constructed in this study are capable of monitoring the intermolecular binding and dissociation processes in a highly sensitive,real-time and label-free manner,with excellent accuracy,stability and universality,providing an efficient,sensitive,portable and low-cost technological means for the study of biomolecular interactions,which is of broad application prospects in the fields of life sciences,drug discovery and screening.
摘要:Oxygen,as an indispensable element in biological activities,exhibits concentration variations that are closely linked to the functionality of organisms,underscoring the critical need for developing highly sensitive real-time oxygen monitoring technologies. To address the prevalent limitations of insufficient sensitivity and delayed response in existing oxygen detection methods,this study synthesized Ru(dpp)₃Cl₂(tris(4,7-diphenyl-1,10-phenanthroline)ruthenium(Ⅱ) chloride)@ZIF-8(zeolitic imidazolate framework-8) composite nanoparticles via a solvothermal method. These nanoparticles were uniformly dispersed within a polydimethylsiloxane(PDMS) matrix to construct a novel Ru(dpp)₃Cl₂@ZIF-8-PDMS composite optical oxygen sensing membrane. Leveraging the confinement effect and porous architecture of ZIF-8,the developed membrane demonstrated a 42% reduction in probe photobleaching rate and achieved a 2.3-fold enhancement in oxygen response sensitivity compared to pristine PDMS membranes. After systematic optimization,the sensing system enabled dynamic real-time monitoring of dissolved oxygen gradients in HeLa cell cultures,offering a robust analytical tool for investigating oxygen microenvironments in life sciences research.
摘要:The polarity and water resistance of conventional stationary phases for reversed-phase chromatography can be improved by C18 stationary phases prepared by embedding an amide polar group in an octadecyl(C18) group. Single bonded polar groups embedded in C18 stationary phases are susceptible to hydrolysis of the silica-oxygen bond,which shortens the service life. In this paper,bis[3-(trimethoxymethylsilyl)]propylamine was prepared by nucleophilic substitution reaction of bis[3-(trimethoxymethylsilyl)]propylamine with stearoyl chloride to produce bis[3-(trimethoxymethylsilyl)]octadecylamido silylating reagent,which was then modified to the surface of silica gel by double-denticle bonding to obtain the amide polar group embedded C18 double-denticle bonded silica gel chromatographic stationary phase(Sil-AM-C18). Characterization by infrared spectroscopy and nuclear magnetic spectroscopy,combined with elemental analysis data,demonstrated that the bidentate amide-modified C18 silane intermediate(AM-C18) had been successfully synthesized and bonded to bare silica gel. The performance of the Sil-AM-C18 column was systematically evaluated,and the results showed that:compared with the traditional C18 stationary phase,the Sil-AM-C18 stationary phase exhibited higher column efficiency;due to the embedding of polar amide groups,the Sil-AM-C18 stationary phase had better aqueous phase tolerance,and still possessed a stable retention and symmetric peak shapes under the conditions of pure aqueous mobile phase. The double-tooth bonding of Sil-AM-C18 stationary phase has higher hydrolytic stability. The Sil-AM-C18 stationary phase was used for the separation of three types of hydrophilic substances,namely,catechin compounds,anti-tuberculosis drugs,and vitamin C and its derivatives,and showed superior separation ability compared with the traditional C18 stationary phase.
关键词:bidentate bonding;polar group embedded C18 packing;catechin analogs;anti-tuberculosisdrugs;vitamin C and its derivatives
摘要:A method was established for the determination of 54 pharmaceuticals and personal care products(PPCPs) in sediments by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) coupled with ultrasonic extraction and QuEChERS purification. Samples were treated with Na2EDTA-McIlvaine buffer and acetonitrile containing 0.5% formic acid. Followed by vortex mixing,ultrasonic extraction and centrifugation,the supernatant was purified by a sorbent mixture of anhydrous magnesium sulfate,N-propylethylenediamine(PSA),octadecyl bonded silica gel(C18) and graphitized carbon black(GCB). Chromatographic separation was achieved on an ACQUITY UPLC BEH C18 column(100 mm×2.1 mm,1.7 μm) with a mobile phase consisting of methanol and 5 mmol/L ammonium formate containing 0.1% formic acid. Mass spectrometric detection was performed in multiple reaction monitoring(MRM) mode,with quantification using the internal standard method. The results showed that 54 PPCPs had good linear relationships within their respective mass concentration ranges,with correlation coefficients(r) ranging from 0.997 9 to 0.999 9. The limits of detection(LODs) and limits of quantification(LOQs) ranged from 0.024 to 0.787 μg/kg and 0.094 to 3.145 μg/kg,respectively. Recoveries of the 54 PPCPs at 2.0,5.0,and 10 μg/kg spiked levels were in the range of 74.5%-114%,and the relative standard deviations(RSDs) for parallel groups were in the range of 2.7%-12%. 11 samples of riverine and coastal sediments were analyzed using the established method and 4 PPCPs were detected with the contents ranged from 0.058 to 0.127 μg/kg. The method is simple,solvent-saving,sensitive,accurate and stable. It is suitable for the simultaneous determination of PPCPs in sediment.
关键词:pharmaceuticals and personal care products(PPCPs);ultrasonic extraction;QuEChERS;UPLC-MS/MS;sediment
摘要:This paper conducts a study on the identification of animal-derived feed materials based on microarray isoelectric focusing(mIEF). At first,a series of optimizations were carried out on the whole process of mIEF for screening of feed materials,which included sample pretreatment,rehydration loading,mIEF separation,and online imaging successfully solving the problems caused by the complex composition and high-salt content of feed materials. Secondly,through repeated experiments,375 mIEF patterns of 15 kinds of animal-derived feeds were obtained,and a feed pattern database based on mIEF data was constructed for further similarity analysis. Finally,the similarity algorithm of Manhattan distance was selected for the comparison and analysis of unknown feed samples,the screening accuracy of actual samples was up to 84.3%,further verifying the technical feasibility of this method. Compared to conventional methods for feed screening,the mIEF technology integrated with the Manhattan algorithm offers advantages of high-throughput,high-resolution,simplified operation,and lower costs,providing a novel approach for feed traceability and quality and safety control.
摘要:In this study,headspace gas chromatography-ion mobility spectrometry(HS-GC-IMS) was employed to qualitatively and quantitatively analyze 75 volatile compounds in fresh saffron samples and those subjected to various drying methods(shade-drying,hot plate-drying,oven-drying,vacuum-drying,and freeze-drying),and a fingerprint profile of volatile components in saffron was established. By focusing on the dynamic changes of volatile components during different drying processes,principal component analysis(PCA),partial least squares-discriminant analysis(PLS-DA),and clustered heatmap analysis were applied to discriminate and analyze differences among samples. Twenty-seven key differential compounds were screened to elucidate the effects of different drying techniques on the volatile components of saffron. The results revealed that different drying methods affect the volatile components through varying degrees of physical(high-temperature volatilization),chemical(photothermal decomposition),and biochemical reactions,thereby influencing the diversity in the quality of saffron:shade-dried samples contained the richest variety of volatile components;hot plate-dried samples had the highest content of safranal(2.91 mg/g);oven-dried and vacuum-dried samples showed the highest abundance of esters and ketones;freeze-dried samples exhibited the highest compositional stability. This study provides theoretical guidance for selecting appropriate drying methods based on practical application scenarios.
摘要:The rapid and highly sensitive detection of foodborne pathogenic bacteria is crucial for food safety. In this study,by optimizing the modification conditions of silane reagent N,N-dimethyl-N-octadecyl-3-aminopropyltrimethoxysilyl chloride(DMOAP),cationic surfactant cetyltrimethylammonium bromide(CTAB) and aptamers,a highly sensitive and visualizable liquid crystal-water interface sensor was successfully constructed. In this biosensor,CTAB was used to regulate the alignment of liquid crystal molecules,and aptamers were combined for the specific recognition of target pathogenic bacteria. The transformation of the ordered and disordered states of liquid crystal molecules was observed by polarizing microscopy,enabling the rapid detection of foodborne pathogenic bacteria (Salmonella typhimurium,Staphylococcus aureus and Escherichia coli). The detection limits reached 13,22 and 28 CFU/mL respectively,and the response time was shortened to 5 minutes. Specificity experiments could distinguish non-target bacteria without complex labeling or amplification steps. This technology provides a label-free and highly sensitive new solution for on-site screening of foodborne pathogenic bacteria,and has the potential to replace traditional time-consuming detection methods.
摘要:To overcome the limitations of commercial solid phase microextraction(SPME) fiber coatings,including mechanical fragility,inadequate thermal stability,and restricted selectivity,this study proposes a titanium(Ti)-based manganese dioxide/polypyrrole(MnO2/PPy) nanocomposite coating with enhanced performance. A hierarchical composite architecture(denoted as Ti@TiO2@SiO2NPs@MnO2/PPyNPs) was engineered by sequentially fabricating nano-pyramidal TiO2 structures on Ti wire via anodic oxidation,electrophoretic deposition of silica nanoparticles(SiO2NPs),and cyclic voltammetry(CV)-assisted co-deposition of MnO2 and PPy nanoparticles.The morphology,chemical composition,and structure of the coating were systematically characterized using scanning electron microscopy(SEM),energy-dispersive spectroscopy(EDS),X-ray photoelectron spectroscopy(XPS),and X-ray diffraction(XRD). Under optimized conditions,the coating exhibited exceptional extraction selectivity for polycyclic aromatic hydrocarbons(PAHs),achieving a wide linear range(0.01-500 μg·L⁻¹),low detection limits(LOD,0.002-0.033 μg·L⁻¹),high precision(relative standard deviation,RSD≤6.9%),and satisfactory spiked recoveries(93.0%-107%). Practical application to real water samples demonstrated its high sensitivity,robust stability,and environmental compatibility,providing a promising technical solution for efficient monitoring of trace PAHs.
摘要:Rapid identification of liquor origins and qualities is one of the key points and difficulties in liquor quality analysis. In order to find a scientific and efficient method to identify and analyze different origins and qualities of sauce-flavor baijiu,this study used surface-enhanced Raman scattering(SERS) technology combined with sensory evaluation methods to systematically analyze 61 sauce-flavor baijiu. Through principal component analysis(PCA) and orthogonal partial least square discriminant analysis(OPLS-DA),the identification model of origins and qualities of sauce-flavor baijiu based on SERS was established. The results showed that the SERS spectra of 61 sauce-flavor baijiu showed high consistency in the main characteristic peaks,including the ethanol characteristic peaks of 880,1 050,1 100,1 270 and 1 450 cm-1. SERS spectra combined with PCA and OPLS-DA model could effectively distinguish different origins and qualities of sauce-flavor baijiu. And the main raman characteristic peaks for distinguishing different origins and qualities of sauce-flavor baijiu are around 2 100,1 750 and 1 100 cm-1.The results of sensory evaluation further revealed that bitterness,astringency,numbness and spiciness are the key taste properties to distinguish sauce-flavor baijiu from different regions. Comparative analysis showed that SERS technology combined with OPLS-DA model was superior to traditional sensory evaluation in distinguishing different origins and qualities of sauce-flavor baijiu. This method provides a new technical path for the origin tracing and quality identification of sauce-flavor baijiu,and has important potential application value.
摘要:A method was developed for simultaneous determination of 30 endocrine disrupting chemicals(EDCs) in urine. The target compounds detected included 9 parabens,9 bisphenols,10 benzophenones,and 2 antimicrobials. The method was based on solid supported liquid-liquid extraction (SLE) and ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Urine sample was first treated with enzyme,then purified on a SLE column. The chromatographic separation was performed on an Acquity UPLC BEH C18(2.1 mm×100 mm,1.7 μm) column with 0.05% acetic acid aqueous solution and methanol as the mobile phase. The electrospray ion source(ESI) was operated in positive and negative ion switching scan. The detection was performed in multiple reaction monitoring(MRM) mode. Internal standard method was applied for quantitative analysis. The method yielded good linearity in the range level of 0.10-80 µg/L. The spiked recoveries of target compounds ranged from 86.9% to 127%. The relative standard deviations(RSDs) of intra-day and inter-day were 1.0%-8.7% and 1.1%-8.2%,respectively. The detection limits(LOD) and quantification limits(LOQ) of the method were 0.003-0.094 µg/L and 0.009-0.313 µg/L,respectively. The proposed method was applied to detect the target EDCs in 150 urine samples,and a total of 23 EDCs were detected,with a detection rate ranging from 0.7% to 100%. Among them,the detection rate of methylparaben(MeP) was the highest(100%),followed by 4-hydroxybenzophenone(4-OHBP,96.7%) and bisphenol A(BPA,94.7%). The developed method is easy to operate,sensitive,and accurate,and is suitable for high-throughput screening and quantitative analysis of EDCs in human urine.
摘要:To support the effective implementation of environmental odor monitoring method standards,the 1-butanol certified reference material with a concentration of 60 μmol/mol in nitrogen was prepared using the weighing method. The purity analysis of high-purity raw materials was conducted. An analytical method based on gas chromatography was developed for sample analysis,and its precision,detection limit,and linearity were systematically evaluated. Furthermore,the preparation technology for the 1-butanol certified reference material was established,the preparation repeatability and coated cylinder suitability were also investigated. The minimum operating pressure and validity period of the sample were determined through pressure release experiments and stability studies. Afterwards,the uncertainty of the 1-butanol certified reference material was evaluated. Results showed that the analytical method exhibited excellent precision and linearity. The 1-butanol certified reference material in nitrogen displayed high preparation repeatability. The coated cylinders were confirmed to be suitable for preparing 1-butanol certified reference material in nitrogen. Pressure variations within the range of 10 MPa to 2 MPa had no statistically significant effect on the characteristic values of 1-butanol. The characteristic values can remain stable throughout the 16-month validation period,confirming long-term stability. Overall,the relative expanded uncertainty(k=2) of 1-butanol certified reference material in nitrogen developed by weighing method was 2%. The certified values are fully traceable to SI units through rigorous calibration protocols. The 1-butanol certified reference material provides a reliable reference for enhancing the accuracy and comparability of odour monitoring and quality management in China’s ambient air and industrial exhaust systems.
摘要:Based on centrifugation-assisted cold induced phase separation(CIPS) and dispersive solid-phase extraction(DSPE) techniques,a detection method for analysis of 11 polyhalogenated carbazoles(PHCs) in seafood was established using liquid chromatography-high resolution mass spectrometry. After ultrasonic extraction using acetonitrile,the samples were subjected to CIPS and DSPE enrichment and purification for 11 PHCs with a 40% acetonitrile/aqueous solution. For instrumental analysis,gradient elution was performed using an acetonitrile-water mobile phase. Separation was achieved on a C8 column(2.1 mm×100 mm,1.7 μm). High resolution mass spectrometry data were acquired in the targeted single-ion monitoring mode,and quantification was carried out using the internal standard method. The results demonstrated that within the given concentration range,all 11 PHCs exhibited good linear relationships(r²>0.996). The limits of detection of the method ranged from 0.04 to 0.1 μg/kg,and the limits of quantification were between 0.1 and 0.3 μg/kg. For blank seafood spiked at three different levels,the recoveries ranged from 71.6% to 112%,and the relative standard deviations(RSDs) were between 1.1% and 13%. This method is simple to operate and highly sensitive. It can effectively mitigate the matrix effects on the detection of PHCs,showing good accuracy and precision. Meeting the requirements of analytical detection,it is applicable for the targeted detection and analysis of PHCs in real samples.
关键词:polyhalogenated carbazoles;cold induced phase separation;high resolution mass spectrometry;seafood;liquid chromatography
摘要:Gasoline is often used in arson crimes because of its easy accessibility and low flashpoint. Therefore,determining the source of gasoline has become a key research element in the investigation of fire-related cases. In this study,hydrogen isotope ratios of 14 characteristic components in 14 gasoline samples from 11 oil companies in Beijing were determined by gas chromatography-stable isotope ratio mass spectrometry(GC-IRMS). The results showed that the hydrogen isotope ratios of all the characteristic components were distributed in a wide range(-220.53‰-13.61‰). One-way ANOVA revealed that about 84% of the samples had at least 10 characteristic components with significant differences. Orthogonal partial least squares discriminant analysis(OPLS-DA) showed that the gasoline from different sources could be effectively distinguished based on the hydrogen stable isotope signature. In this study,GC-IRMS was used to screen out the characteristic components of gasoline and construct a source discrimination model,which provides a scientific basis for the identification of the source of gasoline in fire-related cases.
摘要:An inductively coupled plasma mass spectrometry(ICP-MS) method was established to detect the content of Class 1 elemental impurities(arsenic(As),cadmium(Cd),mercury(Hg),and lead(Pb)),and Class 2A elemental impurities(cobalt(Co),nickel(Ni),and vanadium(V)) in synthetic colorants(Tartrazine,Brilliant Bule,Erythrosine) according to ICH Q3D. The sample was digested by microwave digestion. The results showed that the linear correlation coefficients(r2) of all elemental impurities were greater than 0.999 in the range of 0-100 µg/L,with the exception of Hg, whose linear range was 0-5 µg/L. The detection limits(LODs) ranged from 0.002 to 0.015 mg/kg. The recoveries were within the range of 90.0%-110%,with relative standard deviations(RSDs) less than 5.0%. The method is highly sensitive and accurate,and is suitable for the control of Class 1 and Class 2A elemental impurities in synthetic colorants,with the low residual risk of Class 1 and Class 2A elemental impurities in commercially available synthetic colorants.
关键词:synthetic colorants;inductively coupled plasma mass spectrometry(ICP-MS);elemental impurities;ICH Q3D
摘要:Salmonella is a highly pathogenic foodborne pathogen. As the invA gene is a highly conserved virulence gene in Salmonella,its detection is crucial for rapid and accurate identification of Salmonella. This study constructed a cathodic electrochemiluminescence(ECL) sensing substrate based on a PANI-g-C₃N₄-CeⅣ nanocomposites. By utilizing rolling circle amplification(RCA) for the complementary sequence of invA gene,followed by matching the gold nanoparticle-labeled response probes to enhance the cathodic ECL signal,we developed a targeted detection method of the Salmonella invA virulence gene. The sensor assembly process and experimental conditions were systematically optimized,followed by comprehensive evaluation of its analytical performance. The results demonstrated that the sensor exhibited a linear detection range from 10 amol/L to 1 μmol/L(I=2 131 + 840lgc,r²=0.994 3),with a detection limit of 3.3 amol/L. The spiked recoveries ranged from 96.6% to 111%. The sensor's detection results for actual Salmonella-contaminated meat samples showed complete consistency with those obtained by the gene sequencing,demonstrating its promising prospects for application in public health on-site food safety testing.
关键词:salmonella;invA gene;electrochemiluminescence;PANI-g-C3N4-CeⅣ;rolling circle amplification(RCA)
摘要:Phototherapy sterilization offers advantages such as minimal side effects and broad-spectrum antibacterial efficacy,holding enormous potential for wide-ranging applications. Covalent organic frameworks(COFs) can effectively circumvent the issue of the reduced activity caused by disordered aggregation of traditional photosensitizers,showing promising application prospects in phototherapy sterilization. However,the interlayer π-π stacking inherent in COFs still leads to the aggregation of photosensitizer monomers,which compromises photodynamic activity. To address this,this study presents the synthesis of a porphyrin-based COF(TB) using photosensitizers and vinyl monomers as functional units,then loaded it with the natural antibacterial substance solanesol(Sol) to develop a novel composite material(TB-Sol) integrating photodynamic/photothermal/chemical sterilization. The adsorption capacity of TB porous structure for sol is 207.8 mg·g-1. The highly ordered structure of TB ensures that the TAPP units exhibit excellent singlet oxygen generation and photothermal heating capabilities(the photodynamic performance of TB is 191.51% of that of free TAPP). The incorporation of Sol further improved the antibacterial activity of TB-Sol. Under 100 mW·cm-2 white LED irradiation for 30 minutes,the bactericidal rates of TB-Sol(233 µg·mL-1) against Escherichia coli(E.coli) and Staphylococcus aureus(S.aureus) achieved 99.46% and 97.34%,respectively,significantly higher than those of TB at the same concentration(82.62% and 66.14%,respectively).
关键词:porphyrin based covalent organic framework;solanesol;phototherapy;bacterial infection;synergetic sterilization
摘要:A rapid analytical method for the screening of 11 penicillins in children urine samples was established based on ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high-resolution mass spectrometry(UPLC-Q-Orbitrap HRMS). A certain amount of phosphate buffer solution is added to the urine sample,followed by purification and concentration through HLB solid-phase extraction columns. The samples were separated on the Hypersil GOLD C18 column(100 mm×2.1 mm,1.9 μm) with a gradient elution system consisting of 0.1% formic acid in water and 2 mmol/L ammonium acetate-acetonitrile. Quantification was performed using matrix-matched standard curves and external calibration. Good linear relationships(r²>0.994) were observed for azlocillin,methicillin at 0.5-200 μg/L,and ampicillin,cloxacillin,penicillin V at 1-200 μg/L,and nafcillin,piperacillin,dichloropenicillin at 2-200 μg/L,and amoxicillin,oxacillin,penicillin G at 5-200 μg/L. The detection limits and quantification limits ranged of 0.5-5 μg/L and 1-10 μg/L,respectively. The recoveries at three different levels were between 60.0% to 112%,and the relative standard deviations(RSDs) ranged from 3.6% to 15%. Application of the method to 50 child urine samples revealed penicillin concentrations between 2.5 and 88.6 μg/L,indicating potential exposure risk for children. This method demonstrates simplicity in sample preparation,high sensitivity,reproducibility and precision,making it suitable for rapid determination of 11 penicillins in children urine.
关键词:children urine;penicillin;solid-phase extraction;ultra performance liquid chromatography quadrupole/electrostatic field orbitrap high-resolution mass spectrometry
摘要:A liquid chromatography-tandem mass spectrometry(LC-MS/MS) method was established for the rapid detection of racanisodamine,atropine and scopolamine in gastric contents,plasma and urine of patients with Datura stramonium poisoning. The gastric contents,plasma and urine were extracted with methanol. An C18 column was used for the qualitative and quantitative analysis of scopolamine,racanisodamine and atropine by matrix-matched curve external standard method in multiple reaction monitoring(MRM) mode,with 0.1% formic acid aqueous solution-methanol as the mobile phase in a gradient elution and electrospray ionization(ESI) with a positive ion source. The results showed that scopolamine,racanisodamine and atropine exhibited a good linear relationship(r>0.999) in the range of mass concentrations from 0.1 to 10 ng/mL. The limits of detection(LODs) in gastric contents,plasma and urine were 0.02-0.05 μg/kg,0.01-0.03 ng/mL and 0.04-0.05 ng/mL,and the limits of quantification(LOQs) were 0.07-0.09 μg/kg,0.03-0.10 ng/mL and 0.08-0.10 ng/mL,respectively. Average recoveries of the three alkaloids at the low,medium and high spiked concentration levels were 82.6%-115%,and the relative standard deviations(RSDs) were 0.70%-8.5%,with intra-batch RSDs were 2.2%-8.5% and inter-batch RSDs were 0.70%-7.9% (n=6). The method is qualitatively accurate,with the detection limit meeting the patient's poisoning dose,and it is suitable for the etiological traceability analysis of poisoning events.
摘要:The direct peptide reactivity assay(DPRA) was used to determine the skin sensitization potential of six fragrance ingredients of unknown sensitizing activity,including farnesol,which may be added to cosmetics. The test and control fragrance ingredients were incubated with reaction systems containing cysteine and lysine heptapeptides,respectively. High performance liquid chromatography(HPLC) was used to detect and calculate the peptide depletion rate for sensitization evaluation. The reliability of the assay was validated by testing seven known fragrance ingredients(including positive and negative controls) with established sensitization results from the murine local lymph node assay(LLNA),yielding a 100% consistency rate. Among the test compounds,two ingredients(including cinnamic acid) showed peptide depletion rates less than 6.38% and were classified as non-sensitizers,while the remaining four ingredients(including farnesol) were determined as positive sensitizers. The DPRA is a simple and accurate alternative method for evaluating skin sensitization potential.
摘要:According to ICH M7,Nexu2.7.0 was used to predict the potential mutagenicity of four impurities in apremilast,and the results were all positive and were classified into Class 3. An ultra high performance liquid chromatography-triple quadrupole mass spectrometric(UPLC-MS/MS) method was developed for determination of four potential genotoxic impurities,including APST-ZZ1,APST-ZZ4,APST-ZZ6 and APST-ZZ7,in apremilast. The apremilast was dissolved with 0.1% formic aqueous-acetonitrile(90∶10),and then separated on an ACQUITY UPLC HSS T3(100 mm×2.1 mm,1.8 μm) column by gradient elution using 0.1% formic aqueous-acetonitrile as mobile phases at a flow rate of 0.3 mL/min,a column temperature of 40 ℃,and an injection volume of 10 μL. The detection of analytes was performed in the negative electrospray ionization mode(ESI-) under multiple reaction mode. As a result,the calibration curves of the four impurities all showed good linearity,with their correlation coefficients(r) not less than 0.999 5. The limits of detection(S/N=3) of the method were 0.001 0-0.002 5 mg/kg,and the limits of quantitation(S/N=10) of the method were 0.004 8-0.005 0 mg/kg,respectively. The average recoveries of the four impurities were 90.7%-109% and the relative standard deviations(RSDs) were 0.50%-5.8%,respectively. This method has the advantages of simple operation,short detection time,accurate,reliable,high sensitivity,and could be used for the simultaneous detection of four potential genotoxic impurities in apremilast.
关键词:apremilast;ultra high performance liquid chromatography-triple quadrupole mass spectrometry;potential genotoxic impurity;ICH M7
摘要:A method was proposed for determination of 3 novel herbicides(pethoxamid,pyrimisulfan,ipfencarbazone) residues in grains by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) in combination with QuEChERS pretreatment technology. Samples were extracted with 1% acetic acid in acetonitrile,cleaned up by developed QuEChERS method. The extracts were chromatographically separated using a Waters ACQUITY UPLC® HSS T3 chromatographic column(2.1 mm×100 mm,1.8 μm) and a gradient elution was carried out using acetonitrile-0.1% formic acid in water. Confirmation was achieved using electrospray ionization(ESI) in positive mode with multiple reaction monitoring(MRM) and quantification by matrix-matched external standard method. The results showed that 3 analytes had good linearity in the concentration ranges of 0.5-100 ng/mL,with correlation coefficient more than 0.996. The limits of detection(LODs) of 3 herbicides were 0.005 mg/kg. The limits of quantitation(LOQs) for pethoxamid and pyrimisulfan were 0.01 mg/kg,and the LOQ of ipfencarbazone was 0.02 mg/kg. The recoveries ranged from 81.3%-107%,with relative standard deviations(RSDs) between 0.64%-6.0%. The method successfully identified pethoxamid residues at contents of 0.057 mg/kg and 0.15 mg/kg in two distinct grain sample batches,further validating its efficacy for detecting pethoxamid,pyrimisulfan,and ipfencarbazone in grain samples.
摘要:Based on membrane separation technology,combined with flow analysis and bromothymol blue spectrophotometry,a simple and efficient method for the automatic analysis of ammonia nitrogen in complex industrial wastewater was developed. The impact of substrate pH,salinity and organic nitrogen on the determination of ammonia nitrogen were examined in the experiments. The findings illustrated that the above factors would not interfere with the analysis of ammonia nitrogen by this method. Under optimized conditions,the method achieved a detection limit of 0.16 mg/L and a linear range of 0.57-30 mg/L,with good precision(RSD≤3.0%) and fast analysis speed(sample throughput of 15 h-¹). When applied to ammonia nitrogen detection in industrial wastewater,the results were comparable to those obtained by the distillation-neutralization titration method(HJ 537-2009). The recoveries using industrial wastewater as a spiked matrix significantly(94.1%-99.0%) higher than those from the standard method(47.7%-68.5%). This method provides a reliable,low-cost,highly automated,and interference-resistant solution for ammonia nitrogen detection in complex-matrix wastewater,and shows a good application prospect in the field of water quality detection.
摘要:Compared with polymerase chain reaction(PCR) and loop-mediated isothermal amplification(LAMP),recombinase polymerase amplification(RPA) has a shorter reaction time(5-20 min) and requires less temperature and equipment,and can be carried out at 37-42 ℃. However,the current organic dyes used for real-time fluorescent RPA are dependent on imports and have small Stoke shifts,which are not conducive to visualization and observation. In this study,we applied the nucleic acid molecule “light switch”[Ru(bpy)2(dppz)]2+ as a fluorescent dye for real-time fluorescent RPA amplification,and realized single and multiple real-time fluorescent RPA amplification detection of food-borne pathogens(e.g.,Staphylococcus aureus(S.aur),and Salmonella(S.spp)). In addition,a rapid and visualized RPA detection method was established based on[Ru(bpy)2(dppz)]2+,which determines the amplification results by directly observing the strong red fluorescence signal generated under visible light after the binding of amplification product DNA to[Ru(bpy)2(dppz)]2+,avoiding the obvious inhibition of the amplification reaction caused by high concentration of[Ru(bpy)2(dppz)]2+,and has good visualization effect. It avoids the obvious inhibition of the amplification reaction caused by high concentration of [Ru(bpy)2(dppz)]2+,and has good visualization detection effect,high specificity and high sensitivity,and is expected to be widely used in the field of rapid nucleic acid detection for environmental monitoring,food safety and clinical diagnosis.
摘要:A method for the rapid,real-time,and direct characterization of the distribution of components in sunscreen cosmetics has been established based on micro-Raman spectroscopy. Using the DXR3xi micro-Raman spectrometer,the microscopic morphology of the samples is directly observed to evaluate their uniformity. For larger aggregates or obvious crystalline structures present in the samples,Raman spectral spot scanning is performed. The components are then analyzed by matching the spectra with the instrument's built-in Raman spectral library and a self-built standard spectral library of 16 common sunscreen agents. Additionally,regional Raman scanning of the samples can be conducted,and the distribution of specific components(such as sunscreen agents and surfactants) can be accurately characterized by analyzing the regional correlation of their characteristic spectra. This allows for a comprehensive evaluation of the stability of the sample's microstructure. This method has been successfully applied to the stability assessment of several sunscreen cosmetics,revealing the crystallization of components such as phenylbenzimidazole sulfonic acid and potassium cetyl phosphate. It can serve as a methodological reference for the stability research of sunscreen cosmetics.
摘要:Perfluorinated and polyfluoroalkyl substances(PFAS) are emerging contaminants. Their environmental and health risks cause global concern. Accurate detection methods for PFAS in environmental samples are critical for risk assessment and regulatory control. Therefore,this paper systematically reviews the research progress of PFAS detection methods. This paper covers sampling,pretreatment,and detection techniques. At present,liquid chromatography-tandem mass spectrometry(LC-MS/MS) is the gold standard. It provides high accuracy and sensitivity. It is widely standardized for diverse environmental samples. However,it requires expensive equipment and complex operations. Thus,it is unsuitable for field deployment. To address this gap,researchers developed rapid detection techniques. These techniques primarily use optical and electrochemical methods. Optical/electrochemical rapid detection methods show key advantages:They achieve pg/L level sensitivity; exhibit exceptional selectivity; and feature field portability. These techniques are engineered through sensing architecture optimization and data analytics integration. These advancements establish a breakthrough approach for rapid in-situ detection. But challenges remain in multi-analyte reliability and industrial scalability. Further efforts are essential to overcome these limitations.In the future,PFAS rapid screening technology and laboratory confirmatory method(LC-MS/MS) will co-evolve. This synergy promotes the construction of intelligent monitoring network with automation,intelligence and data interconnection. They provide robust technical support for PFAS control.
关键词:perfluorinated and polyfluoroalkyl substances;optical sensing;electrochemical sensing;rapid detection;in situ detection
摘要:Over the past decade,the global prevalence of severe haze pollution has prompted the academic community to engage in systematic investigations into the toxicity of atmospheric fine particulate matter(PM2.5) and its underlying toxicological mechanisms. In this context,cellular experiments have emerged as a predominant methodology for assessing PM2.5 toxicity,owing to their operational simplicity,efficiency,and high reproducibility. Notably,human lung epithelial A549 cells are frequently employed in toxicity testing due to their relatively stable biological properties and capacity for continuous proliferation. This article reviews the comprehensive toxicity of PM2.5 on A549 cell and the cytotoxicity of its different components,summarizes the methods for isolating PM2.5 and extracting its various components before exposure,and organizes and compares existing cytotoxicity measurement methods. The aim is to provide a reference for the study of the cytotoxicity of atmospheric particles and other particulate matter,which will help to further explore the toxicological mechanisms of particulate matter and optimize detection technologies in related fields.
关键词:PM2.5;components;cytotoxicity;isolating and extracting;cytotoxicity test