This study investigated the physicochemical properties,enzyme activities,volatile flavor components,microbial communities,and sensory evaluation of high-temperature Daqu(HTD)during the maturation process,and a standar...This study investigated the physicochemical properties,enzyme activities,volatile flavor components,microbial communities,and sensory evaluation of high-temperature Daqu(HTD)during the maturation process,and a standard system was established for comprehensive quality evaluation of HTD.There were obvious changes in the physicochemical properties,enzyme activities,and volatile flavor components at different storage periods,which affected the sensory evaluation of HTD to a certain extent.The results of high-throughput sequencing revealed significant microbial diversity,and showed that the bacterial community changed significantly more than did the fungal community.During the storage process,the dominant bacterial genera were Kroppenstedtia and Thermoascus.The correlation between dominant microorganisms and quality indicators highlighted their role in HTD quality.Lactococcus,Candida,Pichia,Paecilomyces,and protease activity played a crucial role in the formation of isovaleraldehyde.Acidic protease activity had the greatest impact on the microbial community.Moisture promoted isobutyric acid generation.Furthermore,the comprehensive quality evaluation standard system was established by the entropy weight method combined with multi-factor fuzzy mathematics.Consequently,this study provides innovative insights for comprehensive quality evaluation of HTD during storage and establishes a groundwork for scientific and rational storage of HTD and quality control of sauce-flavor Baijiu.展开更多
This study explores the controllable synthesis of CuAlO_(2) using copper hydroxide and pseudo-boehmite powders as raw materials via a simple solid-phase ball milling method,along with its catalytic performance investi...This study explores the controllable synthesis of CuAlO_(2) using copper hydroxide and pseudo-boehmite powders as raw materials via a simple solid-phase ball milling method,along with its catalytic performance investigation in methanol steam reforming(MSR).Various catalysts were prepared under different conditions,such as calcination temperature,calcination atmosphere,and heating rate.Characterization techniques including BET,XRD,XPS,SEM and H2-TPR were employed to analyze the samples.The results revealed significant effects of calcination temperature on the phase compositions,specific surface area,reduction performance,and surface properties of the CA-T catalysts.Based on the findings,a synthesis route of CuAlO_(2) via the solid-phase method was proposed,highlighting the importance of high calcination temperature,nitrogen atmosphere,and low heating rate for CuAlO_(2) formation.Catalytic evaluation data demonstrated that CuAlO_(2) could catalyze MSR without pre-reduction,with the catalytic performance of CA-T catalysts being notably influenced by calcination temperature.Among the prepared catalysts,the CA-1100 catalyst exhibited the highest catalytic activity and stability.The findings of this study might be useful for the further study of the catalytic material for sustained release catalysis,including the synthesis of catalytic materials and the regulation of sustained release catalytic performance.展开更多
To investigate the thermal stability of ceramic-matrix composites,three kinds of C/C−ZrC−SiC composites with different Zr/Si molar ratios were synthesized by reactive melt infiltration.Employing region labeling method...To investigate the thermal stability of ceramic-matrix composites,three kinds of C/C−ZrC−SiC composites with different Zr/Si molar ratios were synthesized by reactive melt infiltration.Employing region labeling method,the high-temperature thermal stability of the composites was systematically studied by changing the temperature and holding time of thermal treatment.Results show that the mass loss rate of low Si composites has a growth trend with increasing temperature,and a crystal transformation from β-SiC toα-SiC occurs in the composites.In the calibrated area,SiC phase experiences Ostwald ripening and volume change with location migration,while ZrC phase experiences a re-sintering process with diffusion.Moreover,it is found that increasing temperature has a more obvious effect on the thermal stability than extending holding time,which is mainly attributed to the faster diffusion rate of atoms.展开更多
The new catalytic kinetic spectrophotometric method for Au（III） determination was developed and validated. It was based on the catalytic effect of gold on the oxidation of sudan red III by ammonium peroxodisulfate ...The new catalytic kinetic spectrophotometric method for Au（III） determination was developed and validated. It was based on the catalytic effect of gold on the oxidation of sudan red III by ammonium peroxodisulfate （（NH4）2S2O8） with nitrilo triacetic acid as an activator in microemulsion and H2SO4 medium. Under optimum conditions, there was the linearity of the calibration curve in the concentration range from 0 to 20 μg/L Au（Ⅲ） at 520 nm. The relative standard deviation was 3.0% with a correlation coefficient of 0.9986. The detection limit achieved was 9.75 × 10^-5 μg/mL. A new method using a column packed with sulfhydryl dextrose gel （SDG） as a solid-phase extractant has been developed for the preconcentration and separation of Au（Ⅲ） ions. The method has been applied to the determination of trace gold with satisfactory results.展开更多
High-temperature oxidation is an important property to evaluate thermal protection materials. However, since oxidation is a complex process involving microstructure evolution, its quantitative analysis has always been...High-temperature oxidation is an important property to evaluate thermal protection materials. However, since oxidation is a complex process involving microstructure evolution, its quantitative analysis has always been a challenge. In this work, a phase field method （PFM） based on the thermodynamics theory is developed to simulate the oxidation behavior and oxidation induced growth stress. It involves microstructure evolution and solves the problem of quantitatively computational analysis for the oxidation behavior and growth stress. Employing this method, the diffusion process, oxidation performance, and stress evolution axe predicted for Fe-Cr-A1-Y alloys. The numerical results agree well with the experimental data. The linear relationship between the maximum growth stress and the environment oxygen concentration is found. PFM provides a powerful tool to investigate high-temperature oxidation in complex environments.展开更多
The mechanism of self-propagating high-temperature synthesis （SHS） of TiC-Cu cermets was studied using a combustion front quenching method. Microstructural evolution in the quenched sample was observed using scannin...The mechanism of self-propagating high-temperature synthesis （SHS） of TiC-Cu cermets was studied using a combustion front quenching method. Microstructural evolution in the quenched sample was observed using scanning electron microscope （SEM） with energy dispersive X-ray （EDX） spectrometry, and the combustion temperature was measured. The results showed that the combustion reaction started with local formation of Ti-Cu melt and could be described with the dissolution-precipitation mechanism, namely, Ti, Cu, and C particles dissolved into the Ti-Cu solution and TiC particles precipitated in the saturated Ti-Cu-C liquid solution. The local formation of Ti-Cu melt resulted from the solid diffusion between Ti and Cu particles.展开更多
Valve-regulated-lead-acid (VRLA) battery charging performed in high-temperature environments is extremely risky under overcharge conditions, and may lead to a subsequent thermal runaway. A new pressure-controlled char...Valve-regulated-lead-acid (VRLA) battery charging performed in high-temperature environments is extremely risky under overcharge conditions, and may lead to a subsequent thermal runaway. A new pressure-controlled charging method was adopted and the charging characteristics of the pressure-controlled VRLA battery in high-temperature environments were ex-perimentally studied. The concept was tested in a large temperature gradient to obtain more details about the effects of users' accustomed charging and discharging modes on battery capacity. The premature capacity loss (PCL) phenomenon under high temperature exposure was analyzed. The results showed that the capacity loss could be recovered by charging using a large current.展开更多
Second-generation high-temperature superconducting(HTS)conductors,specifically rare earth-barium-copper-oxide(REBCO)coated conductor(CC)tapes,are promising candidates for high-energy and high-field superconducting app...Second-generation high-temperature superconducting(HTS)conductors,specifically rare earth-barium-copper-oxide(REBCO)coated conductor(CC)tapes,are promising candidates for high-energy and high-field superconducting applications.With respect to epoxy-impregnated REBCO composite magnets that comprise multilayer components,the thermomechanical characteristics of each component differ considerably under extremely low temperatures and strong electromagnetic fields.Traditional numerical models include homogenized orthotropic models,which simplify overall field calculation but miss detailed multi-physics aspects,and full refinement(FR)ones that are thorough but computationally demanding.Herein,we propose an extended multi-scale approach for analyzing the multi-field characteristics of an epoxy-impregnated composite magnet assembled by HTS pancake coils.This approach combines a global homogenization(GH)scheme based on the homogenized electromagnetic T-A model,a method for solving Maxwell's equations for superconducting materials based on the current vector potential T and the magnetic field vector potential A,and a homogenized orthotropic thermoelastic model to assess the electromagnetic and thermoelastic properties at the macroscopic scale.We then identify“dangerous regions”at the macroscopic scale and obtain finer details using a local refinement(LR)scheme to capture the responses of each component material in the HTS composite tapes at the mesoscopic scale.The results of the present GH-LR multi-scale approach agree well with those of the FR scheme and the experimental data in the literature,indicating that the present approach is accurate and efficient.The proposed GH-LR multi-scale approach can serve as a valuable tool for evaluating the risk of failure in large-scale HTS composite magnets.展开更多
Chitosan was prepared with stressing method by blending chitin and solid alkali in a single-screw extruder at given temperature and characterized by potentiometric titration,gel permeation chromatography(GPC),infrared...Chitosan was prepared with stressing method by blending chitin and solid alkali in a single-screw extruder at given temperature and characterized by potentiometric titration,gel permeation chromatography(GPC),infrared spectrum(IR)and carbon-13 magnetic resonance sperctroscopy(^(13)C NMR).Chitosan with a deacetylation degree(DD)of 76.1%was obtained at a mass ratio 0.2∶1∶1 for H_2 O/chitin/NaOH at 160℃for 12 min.Compared to conventional solution method(usually 1∶10 for chitin/NaOH),the alkali assumption greatly decreased.Molecular weight of chitosan obtained by solid-phase method(S3,M_w1.54×10^(5))was lower than that obtained by suspension method(Y2,M_w3.34×10^(5)).During deacetylation,molecular weight decreased with high reaction temperature and long reaction time but remained same at different initial ratios of NaOH/chitin.It might be concluded that degradation of chitosan was caused by breakout of the main chain of the oxidized chitosan catalyzed by alkali during the deactylation.IR and^(13)C NMR showed that structures of chitosans prepared by solid-phase method were not changed.展开更多
For the rational manipulation of the production quality of high-temperature metallurgical engineering,there are many challenges in understanding the processes involved because of the black box chemical/electrochemical...For the rational manipulation of the production quality of high-temperature metallurgical engineering,there are many challenges in understanding the processes involved because of the black box chemical/electrochemical reactors.To overcome this issue,various in-situ characterization methods have been recently developed to analyze the interactions between the composition,microstructure,and solid-liquid interface of high-temperature electrochemical electrodes and molten salts.In this review,recent progress of in-situ hightemperature characterization techniques is discussed to summarize the advances in understanding the processes in metallurgical engineering.In-situ high-temperature technologies and analytical methods mainly include synchrotron X-ray diffraction(s-XRD),laser scanning confocal microscopy,and X-ray computed microtomography(X-rayμ-CT),which are important platforms for analyzing the structure and morphology of the electrodes to reveal the complexity and variability of their interfaces.In addition,laser-induced breakdown spectroscopy,high-temperature Raman spectroscopy,and ultraviolet-visible absorption spectroscopy provide microscale characterizations of the composition and structure of molten salts.More importantly,the combination of X-rayμ-CT and s-XRD techniques enables the investigation of the chemical reaction mechanisms at the two-phase interface.Therefore,these in-situ methods are essential for analyzing the chemical/electrochemical kinetics of high-temperature reaction processes and establishing the theoretical principles for the efficient and stable operation of chemical/electrochemical metallurgical processes.展开更多
Against the background of global warming,research on the spatial distribution of high-temperature risk is of great significance to effectively prevent the adverse effects of high temperatures.By using air temperature ...Against the background of global warming,research on the spatial distribution of high-temperature risk is of great significance to effectively prevent the adverse effects of high temperatures.By using air temperature data from 1951 to 2018 measured by meteorological stations located in the Yangtze River Delta urban agglomeration,the daily maximum air temperature distribution is interpolated at a resolution of 1 km based on the local thin disk smooth spline function;the high-temperature threshold for return periods of 5,10,20 and 30 yr are then calculated by using the generalized extreme value method.The yearly average high-temperature intensity and high-temperature days are finally calculated as high-temperature danger factors.Socioeconomic statistical data and remotely sensed image data in 2018 are used as the background data to calculate the spatial distribution of high-temperature vulnerability factors and prevention capacity factors,which are then used to compute the high-temperature risk index during different recurrence periods in the Yangtze River Delta urban agglomerations.The results show that the spatial distribution features of high-temperature risk in different return periods are similar.The high-temperature risk index gradually increases from northeast to southwest and from east coast to inland,which has obvious latitude variation characteristics and a relationship with the comprehensive influence of the underlying surface and urban scale.In terms of time variation,the high-temperature risk index and its spatial distribution difference gradually decreases with increasing return period.In different cities,the high-temperature risk in the central area of the city is generally higher than that in the surrounding suburban areas.Jinhua,Hangzhou of Zhejiang Province and Xuancheng of Anhui Province are the top three cities with high-temperature risk in the study area.展开更多
We present recent theoretical results on superconductivity in correlated-electron systems, especially in the two-dimensional Hubbard model and the three-band d-p model. The mechanism of superconductivity in high-tempe...We present recent theoretical results on superconductivity in correlated-electron systems, especially in the two-dimensional Hubbard model and the three-band d-p model. The mechanism of superconductivity in high-temperature superconductors has been extensively studied on the basis of various electronic models and also electron-phonon models. In this study, we investigate the properties of superconductivity in correlated-electron systems by using numerical methods such as the variational Monte Carlo method and the quantum Monte Carlomethod. The Hubbard model is one of basic models for strongly correlated electron systems, and is regarded as the model of cuprate high temperature superconductors. The d-p model is more realistic model for cuprates. The superconducting condensation energy obtained by adopting the Gutzwiller ansatz is in reasonable agreement with the condensation energy estimated for YBa2Cu3O7. We show the phase diagram of the ground state using this method. We have further investigated the stability of striped and checkerboard states in the under-doped region. Holes doped in a half-filled square lattice lead to an incommensurate spin and charge density wave. The relationship of the hole density x and incommensurability δ, δ~x, is satisfied in the lower doping region, as indicated by the variationalMonte Carlocalculations for the two-dimensional Hubbard model. A checkerboard-like charge-density modulation with a roughly period has also been observed by scanning tunneling microscopy experiments in Bi2212 and Na-CCOC compounds. We have performed a variational Monte Carlo simulation on a two-dimensional t-t′-t″- U Hubbard model with a Bi-2212 type band structure and found that the period checkerboard spin modulation, that is characterized by multi Q vectors, is indeed stabilized. We have further performed an investigation by using a quantumMonte Carlomethod, which is a numerical method that can be used to simulate the behavior of correlated electron systems. We present a new algorithm of the quantum Monte Carlo diagonalization that is a method for the evaluation of expectation value without the negative sign problem. We compute pair correlation functions and show that pair correlation is indeed enhanced with hole doping.展开更多
A novel, high-temperature, mechano-chemical（HTMC） method was developed to synthesise singlephase Sr_2CeO_4：Eu^（3＋）phosphor. Phosphors were characterised by X-ray diffraction（XRD）, scanning electron microscopy...A novel, high-temperature, mechano-chemical（HTMC） method was developed to synthesise singlephase Sr_2CeO_4：Eu^（3＋）phosphor. Phosphors were characterised by X-ray diffraction（XRD）, scanning electron microscopy（SEM）, and luminescence spectra. Compared with phosphors prepared by the traditional hightemperature solid state method and citric acid gel method, single-phase Sr_2CeO_4：Eu^（3＋）powders by using the HTMC method, with small average particle sizes of about 5 μm, a narrow size distribution range and uniform dispersion, were prepared at 800 ℃, and reached their maximum luminescent intensity at 900 ℃.Under ultraviolet excitation at 298 nm, the sample showed good luminescence with the strongest red light of 616 nm. However, Sr_2CeO_4：Eu^（3＋）was prepared at the higher temperature of 1100 ℃ by solid state method and citric acid gel method. The particle size was too large and uneven with phosphor agglomeration by high-temperature solid state method. The luminescent intensity reached a maximum for Sr_2CeO_4：Eu^（3＋）phosphor at a synthesis temperature of 1100 ℃ by using the high-temperature solid state method, and at 1200 ℃ by both citric acid gel and chemical precipitation methods. Furthermore, the advantages of the Sr_2CeO_4：Eu^（3＋）powder prepared by HTMC method were discussed compared with that prepared using traditional high-temperature solid state and citric acid gel methods.展开更多
Using polymer-derived technology, continuous high-temperature resistant Si-Al-C fibers were prepared by one step method, which included melt-spinning of polyaluminocarbosilane (PACS), curing of continuous PACS fibers,...Using polymer-derived technology, continuous high-temperature resistant Si-Al-C fibers were prepared by one step method, which included melt-spinning of polyaluminocarbosilane (PACS), curing of continuous PACS fibers, and sintering of the cured products. The results show that the average diameter and tensile strength of continuous Si-Al-C fibers are 11 to 12 μm and 1.8 to 2.0 GPa, respectively. The chemical formula of Si-Al-C fibers is SiC1.01O0.0400Al0.024, which is nearly stoichometric. The fibers are mainly composed of β-SiC crystalline, small amount of α-SiC, and amorphous SiC. Continuous Si-Al-C fibers exhibit excellent thermal stability. When the fibers were exposed in argon for 1 h, the tensile strength did not decrease until 1500°C. After heat treatment at 1800°C in argon for 1 h, the fibers maintained about 80% of the initial strength. It was higher than that of Nicalon and Hi-Nicalon fibers.展开更多
There is a critical need to develop advanced high-temperature thermal storage systems to improve efficiencies and reduce the costs of solar thermal storage system.In this work,two typical systems composed with Cu as m...There is a critical need to develop advanced high-temperature thermal storage systems to improve efficiencies and reduce the costs of solar thermal storage system.In this work,two typical systems composed with Cu as matrix and Sn as the phase change material(PCM)are explored,namely,the 3-deimentional(3D)structure system by embedding Sn particles into Cu matrix and the 2-deimentional(2D)structure system by embedding Sn wires into Cu matrix.Given the thermophysical properties of a nanomaterial could be importantly different from that of a bulk one,we thus firstly derive the thermophysical properties of PCM and matrix theoretically,like the thermal conductivity by kinetic method and the specific heat capacity based on Lindemann’s criterion.And then,these properties are utilized to estimate the energy storage ability in both 3D and 2D structure system,and the influence of structure on heat transfer efficiency is theoretically investigated in both 3D and 2D structure system.Results turn out that 3D structure system is a better choice than a 2D structure system,because of larger specific surface area,a larger sensitive heat capacity and a larger thermal conductivity.When the feature size of the PCM decreases to be less than a critical value which is about 500 nm for Sn,the thermal conductivity of the system decreases exponentially while the heat storage capacity increases lineally.Moreover,when the feature size of Sn geometry is less than a critical value,which is 15 nm for 3D structure system and 25 nm for 2D structure,the Cu matrix can’t play a role in improving the effective thermal conductivity of the whole system.展开更多
Single-atom catalysts(SACs),as the rising stars in the field of catalytic science,are leading catalytic technology into an un-precedented new era.However,the synthe-sis of high-performance SACs with well-de-fined acti...Single-atom catalysts(SACs),as the rising stars in the field of catalytic science,are leading catalytic technology into an un-precedented new era.However,the synthe-sis of high-performance SACs with well-de-fined active sites and high loadings under precise control has become a hotly debated topic in scientific research.Metal-organic frameworks(MOFs),with their exceptional properties such as ultrahigh specific surface areas,precisely controllable structural de-signs,and highly flexible functional cus-tomization capabilities,are regarded as one of the ideal matrices for supporting and sta-bilizing SACs.This review provides an in-sightful overview of the diverse preparation strategies for MOFs-derived SACs.It comprehen-sively analyzes the unique advantages and challenges of each method in achieving efficient synthesis of SACs,emphasizing the crucial role of optimized processes in unlocking the antici-pated performance of SACs.Furthermore,this review delves into a series of advanced charac-terization techniques,including aberration-corrected scanning transmission electron mi-croscopy(AC-STEM),electron energy loss spectroscopy(EELS),X-ray absorption spec-troscopy(XAS),and infrared absorption spectroscopy(IRAS),offering valuable insights into the atomic-scale fine structures and properties of SACs,significantly advancing the under-standing of SAC mechanisms.Moreover,this review focuses on exploring the potential appli-cations of MOFs-derived SACs in electrocatalysis frontier fields.This comprehensive exami-nation lays a solid theoretical foundation and provides a directional guidance for the rational design and controllable synthesis of high-performance MOFs-derived SACs.展开更多
Complex phase transitions occur in P2-type materials during charging and discharging.A high-entropy structure can effectively inhibit the structural phase transition of a P2-type layered material.In this study,a hight...Complex phase transitions occur in P2-type materials during charging and discharging.A high-entropy structure can effectively inhibit the structural phase transition of a P2-type layered material.In this study,a hightemperature solid-phase method is used to synthesize the P2-type high-entropy fluorine oxide(HEFO)Na_(0.7)Li_(0.08)Mn(Ⅳ)_(0.21)Mn(Ⅲ)_(0.43)Mg_(0.11)Ni_(0.11)W_(0.04)Nb_(0.02)O_(1.9)F_(0.1)[■-NLM(Ⅳ)0.21M(Ⅲ)0.43F(■=NMNWO)],with a superlattice structure and Na_(2)WO_(4)coating.Na_(2)WO_(4)can effectively inhibit the complex phase transition to improve the structural stability of the material and overcome the limitations of P2-type Na_(x)TMO_(2)(TM=transition metal)via additional charge compensation.Adjusting the Mn^(3+)/Mn^(4+)ratio to increase the average valence state of Mn and introducing F^(-)and Li^(+)to inhibit the Jahn-Teller effect suppress the complex phase transition during charging and discharging.The material exhibits a good multiplicative performance(discharge specific capacity of 88.4 mAh g^(-1)at a multiplicative rate of 10C)and capacity retention(99.22%after 200 cycles at 1C in the potential window of 1.5-4.3 V).The structural stabilities of HEFO are effectively demonstrated using electrochemical in situ X-ray diffraction and ex situ X-ray photoelectron spectroscopy.Theoretical calculations reveal that the high-entropy structure effectively improves the electronic structure and charge distribution of the layered oxide material.This study provides new concepts for use in developing novel energy batteries.展开更多
A series of Dy^(3+)/Eu^(3+) single doped and co-doped SrLaAlO_(4) phosphors was synthesized by the traditional high-temperature solid-state method,and their structure,morphology and optical properties were characteriz...A series of Dy^(3+)/Eu^(3+) single doped and co-doped SrLaAlO_(4) phosphors was synthesized by the traditional high-temperature solid-state method,and their structure,morphology and optical properties were characterized.The X-ray diffraction(XRD) shows a small amount of doping with Dy^(3+) and Eu^(3+) does not change the crystal structure of the matrix SrLaAlO_(4) and the best synthesis temperature is 1450℃.The scanning electron microscopy(SEM) indicates the particle size directly ranges from 1 to 5μm roughly and the energy dispersive spectroscopy(EDS) patterns show that SrLaAlO_(4):Dy^(3+) phosphor and SrLaAlO_(4):Dy^(3+),Eu^(3+) phosphor were successfully synthesized.SrLaAlO_(4):Dy^(3+) phosphor can be effectively excited by near-ultraviolet light,producing two strong emission lights at 483 nm(blue light) and 579 nm(yellow light),presenting a cold white light;SrLaAlO_(4):Eu^(3+) phosphor can be effectively excited by nearultraviolet light,producing red lights at 622 nm;the characteristic emission peaks of Dy^(3+) and Eu^(3+)can be shown simultaneously under the same excitation wavelength in SrLaAlO_(4):Dy^(3+), Eu^(3+) phosphor.By changing the relative doping concentration ratio of Dy^(3+) and Eu^(3+),the modulation of SrLaAlO_(4):Dy^(3+),Eu3+phosphor from cold white to warm white light can be achieved.In addition,the study of the luminescent mechanism and lifetime shows that there is energy transfer between Dy^(3+) and Eu^(3+) in SrLaAlO_(4):Dy^(3+),Eu^(3+) phosphor.展开更多
This paper describes a simple, rapid and sensitive liquid chromatography tandem mass spectrometry assay for the determination of duloxetine in human plasma. A duloxetine stable labeled isotope （duloxetine ds） was us...This paper describes a simple, rapid and sensitive liquid chromatography tandem mass spectrometry assay for the determination of duloxetine in human plasma. A duloxetine stable labeled isotope （duloxetine ds） was used as an internal standard. Analyte and the internal standard were extracted from 100 btL of human plasma via solid phase extraction technique using Oasis HLB cartridges. The chromatographic separation was achieved on a Cl8 column by using a mixture of acetonitrile 5 mM ammonium acetate buffer （83：17, v/v） as the mobile phase at a flow rate of 0.9 mL/min. The calibration curve obtained was linear （r2≥0.99） over the concentration range of 0.05 101 ng/mL. Multiple-reaction monitoring mode （MRM） was used for quantification of ion transitions at rn/z 298.3/154.1 and 303.3/159.1 for the drug and the internal standard, respectively. Method validation was performed as per FDA guidelines and the results met the acceptance criteria. A run time of 2.5 min for each sample made it possible to analyze more than 300 plasma samples per day. The proposed method was found to be applicable to clinical studies.展开更多
Jiaozi Steamed Bread(JSB)has a unique aroma as a traditional staple food in China.The volatile compounds in JSBwere extracted by simultaneous distillation and extraction(SDE)and headspace solid-phasemicroextraction(HS...Jiaozi Steamed Bread(JSB)has a unique aroma as a traditional staple food in China.The volatile compounds in JSBwere extracted by simultaneous distillation and extraction(SDE)and headspace solid-phasemicroextraction(HS-SPME).These volatile substances were analyzed by gas chromatography-mass spectrometry(GC-MS)and gas chromatographyolfactometry-mass spectrometry(GC-O-MS).The results demonstrated that 61 volatile compounds were identified totally in samples,of which 15 were confirmed as potent aroma compounds with odor active values(OAVs)>1.The 15 potent aroma compounds were ethanol,1-butanol,1-pentanol,1-hexanol,heptanol,1-octen-3-ol,3-methyl-1-butanol,hexanal,heptanal,nonanal,(E)-2-heptenal,benzaldehyde,(E,E)-2,4-decadienal,2-pentylfuran and naphthalene.The SDEmethod had better linearity with coefficients of determination(R2)equal to or higher than 0.9991.Furthermore,the SDE method also achieved lower sensitivity and better repeatability and recovery than HS-SPME.This work provides reference method and parameters for future research on the flavor of JSB for commercial products.展开更多
文摘This study investigated the physicochemical properties,enzyme activities,volatile flavor components,microbial communities,and sensory evaluation of high-temperature Daqu(HTD)during the maturation process,and a standard system was established for comprehensive quality evaluation of HTD.There were obvious changes in the physicochemical properties,enzyme activities,and volatile flavor components at different storage periods,which affected the sensory evaluation of HTD to a certain extent.The results of high-throughput sequencing revealed significant microbial diversity,and showed that the bacterial community changed significantly more than did the fungal community.During the storage process,the dominant bacterial genera were Kroppenstedtia and Thermoascus.The correlation between dominant microorganisms and quality indicators highlighted their role in HTD quality.Lactococcus,Candida,Pichia,Paecilomyces,and protease activity played a crucial role in the formation of isovaleraldehyde.Acidic protease activity had the greatest impact on the microbial community.Moisture promoted isobutyric acid generation.Furthermore,the comprehensive quality evaluation standard system was established by the entropy weight method combined with multi-factor fuzzy mathematics.Consequently,this study provides innovative insights for comprehensive quality evaluation of HTD during storage and establishes a groundwork for scientific and rational storage of HTD and quality control of sauce-flavor Baijiu.
基金supported by the Scientific Research Foundation for High-level Talents of Anhui University of Science and Technology(2023yjrc51)the National Natural Science Foundation of China(22172184)+2 种基金the Foundation of State Key Laboratory of Coal Conversion(J24-25-603)the Fundamental Research Project of ICC-CAS(SCJC-DT-2023-01)Weiqiao-UCAS Special Projects on Low-Carbon Technology Development(GYY-DTFZ-2022-015)。
文摘This study explores the controllable synthesis of CuAlO_(2) using copper hydroxide and pseudo-boehmite powders as raw materials via a simple solid-phase ball milling method,along with its catalytic performance investigation in methanol steam reforming(MSR).Various catalysts were prepared under different conditions,such as calcination temperature,calcination atmosphere,and heating rate.Characterization techniques including BET,XRD,XPS,SEM and H2-TPR were employed to analyze the samples.The results revealed significant effects of calcination temperature on the phase compositions,specific surface area,reduction performance,and surface properties of the CA-T catalysts.Based on the findings,a synthesis route of CuAlO_(2) via the solid-phase method was proposed,highlighting the importance of high calcination temperature,nitrogen atmosphere,and low heating rate for CuAlO_(2) formation.Catalytic evaluation data demonstrated that CuAlO_(2) could catalyze MSR without pre-reduction,with the catalytic performance of CA-T catalysts being notably influenced by calcination temperature.Among the prepared catalysts,the CA-1100 catalyst exhibited the highest catalytic activity and stability.The findings of this study might be useful for the further study of the catalytic material for sustained release catalysis,including the synthesis of catalytic materials and the regulation of sustained release catalytic performance.
基金supported by the National Natural Science Foundation of China(No.U19A2099)the CAS Key Laboratory of Carbon Materials,China(No.KLCMKFJJ2005)the Fund of Aerospace Research Institute of Material and Processing Technology,China(No.6142906200108).
文摘To investigate the thermal stability of ceramic-matrix composites,three kinds of C/C−ZrC−SiC composites with different Zr/Si molar ratios were synthesized by reactive melt infiltration.Employing region labeling method,the high-temperature thermal stability of the composites was systematically studied by changing the temperature and holding time of thermal treatment.Results show that the mass loss rate of low Si composites has a growth trend with increasing temperature,and a crystal transformation from β-SiC toα-SiC occurs in the composites.In the calibrated area,SiC phase experiences Ostwald ripening and volume change with location migration,while ZrC phase experiences a re-sintering process with diffusion.Moreover,it is found that increasing temperature has a more obvious effect on the thermal stability than extending holding time,which is mainly attributed to the faster diffusion rate of atoms.
文摘The new catalytic kinetic spectrophotometric method for Au（III） determination was developed and validated. It was based on the catalytic effect of gold on the oxidation of sudan red III by ammonium peroxodisulfate （（NH4）2S2O8） with nitrilo triacetic acid as an activator in microemulsion and H2SO4 medium. Under optimum conditions, there was the linearity of the calibration curve in the concentration range from 0 to 20 μg/L Au（Ⅲ） at 520 nm. The relative standard deviation was 3.0% with a correlation coefficient of 0.9986. The detection limit achieved was 9.75 × 10^-5 μg/mL. A new method using a column packed with sulfhydryl dextrose gel （SDG） as a solid-phase extractant has been developed for the preconcentration and separation of Au（Ⅲ） ions. The method has been applied to the determination of trace gold with satisfactory results.
基金Project supported by the National Natural Science Foundation of China (Nos. 90505015 and10702035)
文摘High-temperature oxidation is an important property to evaluate thermal protection materials. However, since oxidation is a complex process involving microstructure evolution, its quantitative analysis has always been a challenge. In this work, a phase field method （PFM） based on the thermodynamics theory is developed to simulate the oxidation behavior and oxidation induced growth stress. It involves microstructure evolution and solves the problem of quantitatively computational analysis for the oxidation behavior and growth stress. Employing this method, the diffusion process, oxidation performance, and stress evolution axe predicted for Fe-Cr-A1-Y alloys. The numerical results agree well with the experimental data. The linear relationship between the maximum growth stress and the environment oxygen concentration is found. PFM provides a powerful tool to investigate high-temperature oxidation in complex environments.
基金This work was financially supported by the Natural Science Foundation of Shaanxi Province, China (No.2004E107)
文摘The mechanism of self-propagating high-temperature synthesis （SHS） of TiC-Cu cermets was studied using a combustion front quenching method. Microstructural evolution in the quenched sample was observed using scanning electron microscope （SEM） with energy dispersive X-ray （EDX） spectrometry, and the combustion temperature was measured. The results showed that the combustion reaction started with local formation of Ti-Cu melt and could be described with the dissolution-precipitation mechanism, namely, Ti, Cu, and C particles dissolved into the Ti-Cu solution and TiC particles precipitated in the saturated Ti-Cu-C liquid solution. The local formation of Ti-Cu melt resulted from the solid diffusion between Ti and Cu particles.
文摘Valve-regulated-lead-acid (VRLA) battery charging performed in high-temperature environments is extremely risky under overcharge conditions, and may lead to a subsequent thermal runaway. A new pressure-controlled charging method was adopted and the charging characteristics of the pressure-controlled VRLA battery in high-temperature environments were ex-perimentally studied. The concept was tested in a large temperature gradient to obtain more details about the effects of users' accustomed charging and discharging modes on battery capacity. The premature capacity loss (PCL) phenomenon under high temperature exposure was analyzed. The results showed that the capacity loss could be recovered by charging using a large current.
基金Project supported by the National Natural Science Foundation of China(Nos.11932008 and 12272156)the Fundamental Research Funds for the Central Universities(No.lzujbky-2022-kb06)+1 种基金the Gansu Science and Technology ProgramLanzhou City’s Scientific Research Funding Subsidy to Lanzhou University of China。
文摘Second-generation high-temperature superconducting(HTS)conductors,specifically rare earth-barium-copper-oxide(REBCO)coated conductor(CC)tapes,are promising candidates for high-energy and high-field superconducting applications.With respect to epoxy-impregnated REBCO composite magnets that comprise multilayer components,the thermomechanical characteristics of each component differ considerably under extremely low temperatures and strong electromagnetic fields.Traditional numerical models include homogenized orthotropic models,which simplify overall field calculation but miss detailed multi-physics aspects,and full refinement(FR)ones that are thorough but computationally demanding.Herein,we propose an extended multi-scale approach for analyzing the multi-field characteristics of an epoxy-impregnated composite magnet assembled by HTS pancake coils.This approach combines a global homogenization(GH)scheme based on the homogenized electromagnetic T-A model,a method for solving Maxwell's equations for superconducting materials based on the current vector potential T and the magnetic field vector potential A,and a homogenized orthotropic thermoelastic model to assess the electromagnetic and thermoelastic properties at the macroscopic scale.We then identify“dangerous regions”at the macroscopic scale and obtain finer details using a local refinement(LR)scheme to capture the responses of each component material in the HTS composite tapes at the mesoscopic scale.The results of the present GH-LR multi-scale approach agree well with those of the FR scheme and the experimental data in the literature,indicating that the present approach is accurate and efficient.The proposed GH-LR multi-scale approach can serve as a valuable tool for evaluating the risk of failure in large-scale HTS composite magnets.
基金Supported by the National Natural Science Foundation of China(29977014)
文摘Chitosan was prepared with stressing method by blending chitin and solid alkali in a single-screw extruder at given temperature and characterized by potentiometric titration,gel permeation chromatography(GPC),infrared spectrum(IR)and carbon-13 magnetic resonance sperctroscopy(^(13)C NMR).Chitosan with a deacetylation degree(DD)of 76.1%was obtained at a mass ratio 0.2∶1∶1 for H_2 O/chitin/NaOH at 160℃for 12 min.Compared to conventional solution method(usually 1∶10 for chitin/NaOH),the alkali assumption greatly decreased.Molecular weight of chitosan obtained by solid-phase method(S3,M_w1.54×10^(5))was lower than that obtained by suspension method(Y2,M_w3.34×10^(5)).During deacetylation,molecular weight decreased with high reaction temperature and long reaction time but remained same at different initial ratios of NaOH/chitin.It might be concluded that degradation of chitosan was caused by breakout of the main chain of the oxidized chitosan catalyzed by alkali during the deactylation.IR and^(13)C NMR showed that structures of chitosans prepared by solid-phase method were not changed.
基金financially supported by the National Key R&D Program of China(No.2022YFC2906100).
文摘For the rational manipulation of the production quality of high-temperature metallurgical engineering,there are many challenges in understanding the processes involved because of the black box chemical/electrochemical reactors.To overcome this issue,various in-situ characterization methods have been recently developed to analyze the interactions between the composition,microstructure,and solid-liquid interface of high-temperature electrochemical electrodes and molten salts.In this review,recent progress of in-situ hightemperature characterization techniques is discussed to summarize the advances in understanding the processes in metallurgical engineering.In-situ high-temperature technologies and analytical methods mainly include synchrotron X-ray diffraction(s-XRD),laser scanning confocal microscopy,and X-ray computed microtomography(X-rayμ-CT),which are important platforms for analyzing the structure and morphology of the electrodes to reveal the complexity and variability of their interfaces.In addition,laser-induced breakdown spectroscopy,high-temperature Raman spectroscopy,and ultraviolet-visible absorption spectroscopy provide microscale characterizations of the composition and structure of molten salts.More importantly,the combination of X-rayμ-CT and s-XRD techniques enables the investigation of the chemical reaction mechanisms at the two-phase interface.Therefore,these in-situ methods are essential for analyzing the chemical/electrochemical kinetics of high-temperature reaction processes and establishing the theoretical principles for the efficient and stable operation of chemical/electrochemical metallurgical processes.
基金Under the auspices of National Key R&D Program of China(No.2019YFC1510203)National Natural Science Foundation of China(No.42171101,41871028)。
文摘Against the background of global warming,research on the spatial distribution of high-temperature risk is of great significance to effectively prevent the adverse effects of high temperatures.By using air temperature data from 1951 to 2018 measured by meteorological stations located in the Yangtze River Delta urban agglomeration,the daily maximum air temperature distribution is interpolated at a resolution of 1 km based on the local thin disk smooth spline function;the high-temperature threshold for return periods of 5,10,20 and 30 yr are then calculated by using the generalized extreme value method.The yearly average high-temperature intensity and high-temperature days are finally calculated as high-temperature danger factors.Socioeconomic statistical data and remotely sensed image data in 2018 are used as the background data to calculate the spatial distribution of high-temperature vulnerability factors and prevention capacity factors,which are then used to compute the high-temperature risk index during different recurrence periods in the Yangtze River Delta urban agglomerations.The results show that the spatial distribution features of high-temperature risk in different return periods are similar.The high-temperature risk index gradually increases from northeast to southwest and from east coast to inland,which has obvious latitude variation characteristics and a relationship with the comprehensive influence of the underlying surface and urban scale.In terms of time variation,the high-temperature risk index and its spatial distribution difference gradually decreases with increasing return period.In different cities,the high-temperature risk in the central area of the city is generally higher than that in the surrounding suburban areas.Jinhua,Hangzhou of Zhejiang Province and Xuancheng of Anhui Province are the top three cities with high-temperature risk in the study area.
文摘We present recent theoretical results on superconductivity in correlated-electron systems, especially in the two-dimensional Hubbard model and the three-band d-p model. The mechanism of superconductivity in high-temperature superconductors has been extensively studied on the basis of various electronic models and also electron-phonon models. In this study, we investigate the properties of superconductivity in correlated-electron systems by using numerical methods such as the variational Monte Carlo method and the quantum Monte Carlomethod. The Hubbard model is one of basic models for strongly correlated electron systems, and is regarded as the model of cuprate high temperature superconductors. The d-p model is more realistic model for cuprates. The superconducting condensation energy obtained by adopting the Gutzwiller ansatz is in reasonable agreement with the condensation energy estimated for YBa2Cu3O7. We show the phase diagram of the ground state using this method. We have further investigated the stability of striped and checkerboard states in the under-doped region. Holes doped in a half-filled square lattice lead to an incommensurate spin and charge density wave. The relationship of the hole density x and incommensurability δ, δ~x, is satisfied in the lower doping region, as indicated by the variationalMonte Carlocalculations for the two-dimensional Hubbard model. A checkerboard-like charge-density modulation with a roughly period has also been observed by scanning tunneling microscopy experiments in Bi2212 and Na-CCOC compounds. We have performed a variational Monte Carlo simulation on a two-dimensional t-t′-t″- U Hubbard model with a Bi-2212 type band structure and found that the period checkerboard spin modulation, that is characterized by multi Q vectors, is indeed stabilized. We have further performed an investigation by using a quantumMonte Carlomethod, which is a numerical method that can be used to simulate the behavior of correlated electron systems. We present a new algorithm of the quantum Monte Carlo diagonalization that is a method for the evaluation of expectation value without the negative sign problem. We compute pair correlation functions and show that pair correlation is indeed enhanced with hole doping.
文摘A novel, high-temperature, mechano-chemical（HTMC） method was developed to synthesise singlephase Sr_2CeO_4：Eu^（3＋）phosphor. Phosphors were characterised by X-ray diffraction（XRD）, scanning electron microscopy（SEM）, and luminescence spectra. Compared with phosphors prepared by the traditional hightemperature solid state method and citric acid gel method, single-phase Sr_2CeO_4：Eu^（3＋）powders by using the HTMC method, with small average particle sizes of about 5 μm, a narrow size distribution range and uniform dispersion, were prepared at 800 ℃, and reached their maximum luminescent intensity at 900 ℃.Under ultraviolet excitation at 298 nm, the sample showed good luminescence with the strongest red light of 616 nm. However, Sr_2CeO_4：Eu^（3＋）was prepared at the higher temperature of 1100 ℃ by solid state method and citric acid gel method. The particle size was too large and uneven with phosphor agglomeration by high-temperature solid state method. The luminescent intensity reached a maximum for Sr_2CeO_4：Eu^（3＋）phosphor at a synthesis temperature of 1100 ℃ by using the high-temperature solid state method, and at 1200 ℃ by both citric acid gel and chemical precipitation methods. Furthermore, the advantages of the Sr_2CeO_4：Eu^（3＋）powder prepared by HTMC method were discussed compared with that prepared using traditional high-temperature solid state and citric acid gel methods.
基金the National Natural Science Foundation of China (Grant No. 59972042)
文摘Using polymer-derived technology, continuous high-temperature resistant Si-Al-C fibers were prepared by one step method, which included melt-spinning of polyaluminocarbosilane (PACS), curing of continuous PACS fibers, and sintering of the cured products. The results show that the average diameter and tensile strength of continuous Si-Al-C fibers are 11 to 12 μm and 1.8 to 2.0 GPa, respectively. The chemical formula of Si-Al-C fibers is SiC1.01O0.0400Al0.024, which is nearly stoichometric. The fibers are mainly composed of β-SiC crystalline, small amount of α-SiC, and amorphous SiC. Continuous Si-Al-C fibers exhibit excellent thermal stability. When the fibers were exposed in argon for 1 h, the tensile strength did not decrease until 1500°C. After heat treatment at 1800°C in argon for 1 h, the fibers maintained about 80% of the initial strength. It was higher than that of Nicalon and Hi-Nicalon fibers.
基金supported by the Fundamental Research Funds for the Central Universities(2020ZDPY0215)。
文摘There is a critical need to develop advanced high-temperature thermal storage systems to improve efficiencies and reduce the costs of solar thermal storage system.In this work,two typical systems composed with Cu as matrix and Sn as the phase change material(PCM)are explored,namely,the 3-deimentional(3D)structure system by embedding Sn particles into Cu matrix and the 2-deimentional(2D)structure system by embedding Sn wires into Cu matrix.Given the thermophysical properties of a nanomaterial could be importantly different from that of a bulk one,we thus firstly derive the thermophysical properties of PCM and matrix theoretically,like the thermal conductivity by kinetic method and the specific heat capacity based on Lindemann’s criterion.And then,these properties are utilized to estimate the energy storage ability in both 3D and 2D structure system,and the influence of structure on heat transfer efficiency is theoretically investigated in both 3D and 2D structure system.Results turn out that 3D structure system is a better choice than a 2D structure system,because of larger specific surface area,a larger sensitive heat capacity and a larger thermal conductivity.When the feature size of the PCM decreases to be less than a critical value which is about 500 nm for Sn,the thermal conductivity of the system decreases exponentially while the heat storage capacity increases lineally.Moreover,when the feature size of Sn geometry is less than a critical value,which is 15 nm for 3D structure system and 25 nm for 2D structure,the Cu matrix can’t play a role in improving the effective thermal conductivity of the whole system.
基金supported by Henan Province Key Research and Development and Promotion of Science and Technology Project(No.25A150001)the National Natural Science Foundation of China(Nos.22409171,22125303,92361302,and 92061203).
文摘Single-atom catalysts(SACs),as the rising stars in the field of catalytic science,are leading catalytic technology into an un-precedented new era.However,the synthe-sis of high-performance SACs with well-de-fined active sites and high loadings under precise control has become a hotly debated topic in scientific research.Metal-organic frameworks(MOFs),with their exceptional properties such as ultrahigh specific surface areas,precisely controllable structural de-signs,and highly flexible functional cus-tomization capabilities,are regarded as one of the ideal matrices for supporting and sta-bilizing SACs.This review provides an in-sightful overview of the diverse preparation strategies for MOFs-derived SACs.It comprehen-sively analyzes the unique advantages and challenges of each method in achieving efficient synthesis of SACs,emphasizing the crucial role of optimized processes in unlocking the antici-pated performance of SACs.Furthermore,this review delves into a series of advanced charac-terization techniques,including aberration-corrected scanning transmission electron mi-croscopy(AC-STEM),electron energy loss spectroscopy(EELS),X-ray absorption spec-troscopy(XAS),and infrared absorption spectroscopy(IRAS),offering valuable insights into the atomic-scale fine structures and properties of SACs,significantly advancing the under-standing of SAC mechanisms.Moreover,this review focuses on exploring the potential appli-cations of MOFs-derived SACs in electrocatalysis frontier fields.This comprehensive exami-nation lays a solid theoretical foundation and provides a directional guidance for the rational design and controllable synthesis of high-performance MOFs-derived SACs.
基金financially supported by the Guizhou Provincial Basic Research Program(Natural Science)(No.QKHJC-ZK[2023]YB051)the Natural Science Special Foundation of Guizhou University(No.GDTGH[2022]33)+2 种基金the Natural Science Research project of the Education Department of Guizhou Province(No.QJJ[2022]001)the National Natural Science Foundation of China(No.52161029)the Science and Technology Innovation Team of Education Agency in Guizhou Province(No.Qian Jiao Ji[2023]056)
文摘Complex phase transitions occur in P2-type materials during charging and discharging.A high-entropy structure can effectively inhibit the structural phase transition of a P2-type layered material.In this study,a hightemperature solid-phase method is used to synthesize the P2-type high-entropy fluorine oxide(HEFO)Na_(0.7)Li_(0.08)Mn(Ⅳ)_(0.21)Mn(Ⅲ)_(0.43)Mg_(0.11)Ni_(0.11)W_(0.04)Nb_(0.02)O_(1.9)F_(0.1)[■-NLM(Ⅳ)0.21M(Ⅲ)0.43F(■=NMNWO)],with a superlattice structure and Na_(2)WO_(4)coating.Na_(2)WO_(4)can effectively inhibit the complex phase transition to improve the structural stability of the material and overcome the limitations of P2-type Na_(x)TMO_(2)(TM=transition metal)via additional charge compensation.Adjusting the Mn^(3+)/Mn^(4+)ratio to increase the average valence state of Mn and introducing F^(-)and Li^(+)to inhibit the Jahn-Teller effect suppress the complex phase transition during charging and discharging.The material exhibits a good multiplicative performance(discharge specific capacity of 88.4 mAh g^(-1)at a multiplicative rate of 10C)and capacity retention(99.22%after 200 cycles at 1C in the potential window of 1.5-4.3 V).The structural stabilities of HEFO are effectively demonstrated using electrochemical in situ X-ray diffraction and ex situ X-ray photoelectron spectroscopy.Theoretical calculations reveal that the high-entropy structure effectively improves the electronic structure and charge distribution of the layered oxide material.This study provides new concepts for use in developing novel energy batteries.
基金Project supported by Outstanding Young and Middle-aged Scientific Innovation Team of Colleges and Universities of Hubei Province(T2020008)。
文摘A series of Dy^(3+)/Eu^(3+) single doped and co-doped SrLaAlO_(4) phosphors was synthesized by the traditional high-temperature solid-state method,and their structure,morphology and optical properties were characterized.The X-ray diffraction(XRD) shows a small amount of doping with Dy^(3+) and Eu^(3+) does not change the crystal structure of the matrix SrLaAlO_(4) and the best synthesis temperature is 1450℃.The scanning electron microscopy(SEM) indicates the particle size directly ranges from 1 to 5μm roughly and the energy dispersive spectroscopy(EDS) patterns show that SrLaAlO_(4):Dy^(3+) phosphor and SrLaAlO_(4):Dy^(3+),Eu^(3+) phosphor were successfully synthesized.SrLaAlO_(4):Dy^(3+) phosphor can be effectively excited by near-ultraviolet light,producing two strong emission lights at 483 nm(blue light) and 579 nm(yellow light),presenting a cold white light;SrLaAlO_(4):Eu^(3+) phosphor can be effectively excited by nearultraviolet light,producing red lights at 622 nm;the characteristic emission peaks of Dy^(3+) and Eu^(3+)can be shown simultaneously under the same excitation wavelength in SrLaAlO_(4):Dy^(3+), Eu^(3+) phosphor.By changing the relative doping concentration ratio of Dy^(3+) and Eu^(3+),the modulation of SrLaAlO_(4):Dy^(3+),Eu3+phosphor from cold white to warm white light can be achieved.In addition,the study of the luminescent mechanism and lifetime shows that there is energy transfer between Dy^(3+) and Eu^(3+) in SrLaAlO_(4):Dy^(3+),Eu^(3+) phosphor.
文摘This paper describes a simple, rapid and sensitive liquid chromatography tandem mass spectrometry assay for the determination of duloxetine in human plasma. A duloxetine stable labeled isotope （duloxetine ds） was used as an internal standard. Analyte and the internal standard were extracted from 100 btL of human plasma via solid phase extraction technique using Oasis HLB cartridges. The chromatographic separation was achieved on a Cl8 column by using a mixture of acetonitrile 5 mM ammonium acetate buffer （83：17, v/v） as the mobile phase at a flow rate of 0.9 mL/min. The calibration curve obtained was linear （r2≥0.99） over the concentration range of 0.05 101 ng/mL. Multiple-reaction monitoring mode （MRM） was used for quantification of ion transitions at rn/z 298.3/154.1 and 303.3/159.1 for the drug and the internal standard, respectively. Method validation was performed as per FDA guidelines and the results met the acceptance criteria. A run time of 2.5 min for each sample made it possible to analyze more than 300 plasma samples per day. The proposed method was found to be applicable to clinical studies.
基金This project was supported by the National Natural Science Foundation of China(No.31701635)the Key Laboratory of Staple Grain Processing,Ministry of Agriculture(No.DZLS201703)the Henan University of Technology High-level Talents Fund(No.2015BS009).
文摘Jiaozi Steamed Bread(JSB)has a unique aroma as a traditional staple food in China.The volatile compounds in JSBwere extracted by simultaneous distillation and extraction(SDE)and headspace solid-phasemicroextraction(HS-SPME).These volatile substances were analyzed by gas chromatography-mass spectrometry(GC-MS)and gas chromatographyolfactometry-mass spectrometry(GC-O-MS).The results demonstrated that 61 volatile compounds were identified totally in samples,of which 15 were confirmed as potent aroma compounds with odor active values(OAVs)>1.The 15 potent aroma compounds were ethanol,1-butanol,1-pentanol,1-hexanol,heptanol,1-octen-3-ol,3-methyl-1-butanol,hexanal,heptanal,nonanal,(E)-2-heptenal,benzaldehyde,(E,E)-2,4-decadienal,2-pentylfuran and naphthalene.The SDEmethod had better linearity with coefficients of determination(R2)equal to or higher than 0.9991.Furthermore,the SDE method also achieved lower sensitivity and better repeatability and recovery than HS-SPME.This work provides reference method and parameters for future research on the flavor of JSB for commercial products.
