A high-performance liquid chromatography(HPLC)method has been developed using a CAPCELL PAK ADME(150 mm×4.6 mm,5μm)as analytical column and a gradient elution with 15 min using acetonitrile and 0.1%(in volume fr...A high-performance liquid chromatography(HPLC)method has been developed using a CAPCELL PAK ADME(150 mm×4.6 mm,5μm)as analytical column and a gradient elution with 15 min using acetonitrile and 0.1%(in volume fraction)phosphoric acid water(pH=2.2)as the mobile phase.Three active substances in cosmetics were quantitatively detected simultaneously at a detection wavelength of 265 nm.The linear ranges of β-nicotinamide mononucleotides,ergothioneine and nicotinamide are 10~200 mg/L,5~100 mg/L and 5~100 mg/L respectively and the detection limits of three components are 3.0 mg/L,1.5 mg/L and 1.5 mg/L respectively.The recovery rate is 97.1~104.9%,with RSD≤2.0%.The method was applied to quantitative analysis of five samples of cosmetics toner,lotion,cream,essence and gel and three samples of raw materials.The results showed that the results of β-nicotinamide mononucleotide and ergothioneine in five cosmetics were consistent with the product label,while nicotinamide was inconsistent with the label.The purity of the three raw material samples was 99.5%,99.7% and 100.8%respectively.This method offers high precision,accuracy and short analysis time,making it a reliable approach for studying three active ingredients in cosmetics and suitable for quality control of related functional ingredients.展开更多
Anode active materials involving transition metal oxides and sulfides are of great significance for high energy density lithium-ion batteries(LIBs),but the huge volume expansion and inferior electronic conductivity up...Anode active materials involving transition metal oxides and sulfides are of great significance for high energy density lithium-ion batteries(LIBs),but the huge volume expansion and inferior electronic conductivity upon cycling critically constrain their further application.Herein,from a new perspective,a highly conductive and stable 3D flexible composite current collector is rationally designed by facilely electrodepositing metallic Ni thin layer onto the carbon cloth(CC/Ni),which endows the supported active materials with exceptional electronic conductivity and structural stability.In addition,the homogeneously distributed metallic Ni protrusions external CC can strongly bond with the active components,ensuring the structural integrity of electrodes upon cycling.More importantly,the 3D network structure with large specific surface area provides abundant space to alleviate the volume expansion and more active sites for electrochemical reactions.Therefore,taking Ni_(3)S_(2)nanosheet(Ni_(3)S_(2)NS)anode as an example,the prepared Ni_(3)S_(2)NS@CC/Ni electrode shows a high specific capacity of 2.32 mAh/cm^(2)at 1mA/cm^(2)and high capacity retention of 1.68 mAh/cm^(2)at a high rate of 8mA/cm^(2).This study provides a universal approach to obtain highly conductive and stable 3D flexible current collectors towards high performance metal-ion batteries beyond LIBs.展开更多
This study aims to assess the comprehensive strengthening effect of a steel-ultra high performance concrete(UHPC)composite strengthening method.The axial force-moment interaction curve(N-M curve)was calculated in a no...This study aims to assess the comprehensive strengthening effect of a steel-ultra high performance concrete(UHPC)composite strengthening method.The axial force-moment interaction curve(N-M curve)was calculated in a novel way,using cross-sectional strains at ultimate states as well as real-time stress measurements for each material.The enclosed area of the N-M curve was defined as a comprehensive performance index for the system.We validate our approach with comparisons to numerical modeling and full-scale four-point bending experiments.Additionally,strengthening effects were compared for different sagging and hogging moments based on material stress responses,and the impact of various strengthening parameters was analyzed.We find that the N-M curve of the strengthened cross-section envelops that of the un-strengthened cross-section.Notably,improvements in flexural capacity are greater under sagging moments during the large eccentric failure stage,and greater under hogging moments during the small eccentric failure stage.This discrepancy is attributed to the strength utilization of strengthening materials.These findings provide a reference for understanding the strengthening effects and parameters of steel-UHPC composite.展开更多
In this study, an optimized high performance liquid chromatography-fluorescence detector (HPLC-FL) method for the determination of benzo[a]pyrene in edible oil was established. HPLC was performed with Thermo Fisher Sc...In this study, an optimized high performance liquid chromatography-fluorescence detector (HPLC-FL) method for the determination of benzo[a]pyrene in edible oil was established. HPLC was performed with Thermo Fisher Scientific C18 column (250 mm×4.6 mm, 5 μm) as the chromatographic column and acetonitrile and water as the mobile phase, and the excitation wavelength and emission wavelength of fluorescence detector were 286 and 430 nm, respectively. The response was high, and the linear range was 0.5-10.0 ng/ml. The lowest limit of detection was 0.11 ng/ml, and the average recovery was 92.5%. This method is suitable for quantitative analysis of benzo[a]pyrene content in edible oil.展开更多
Influences of admixtures on the workability and strength of high performance concrete （HPC） are in- vestigated. The types of investigated admixtures include naphthalene series high range water reducing agent, polyca...Influences of admixtures on the workability and strength of high performance concrete （HPC） are in- vestigated. The types of investigated admixtures include naphthalene series high range water reducing agent, polycarboxlic series high range water reduce agent and sodium sulfate hardening accelerating agent. Two kinds of curing condition, namely steam curing condition and standard curing condition, are adopted. The result shows that HPC, added with polycarboxlic series of high performance water reducer, has high workability and strength, while sodium sulfate accelerating agent causes poor workability and low strength. Thus for vapor-cured HPC and its formulations, naphthalene series high range water reducing agent with less sodium sulfate should be given pri- ority. Therefore, the differences of curing conditions should be considered when selecting HPC admixtures.展开更多
Due to their biological and physiological importance,flavonoids receive considerable attention in the literature. Nowadays,high performance liquid chromatography（HPLC）is the most widely used analytical method.In thi...Due to their biological and physiological importance,flavonoids receive considerable attention in the literature. Nowadays,high performance liquid chromatography（HPLC）is the most widely used analytical method.In this review,we summarize the principle of the choice of HPLC column and mobile phase,discuss and compare the features of various detections such as UV,fluorescence detection,electrochemical detection,chemilummescence detection,UV-MS etc.Recent developments in HPLC including ultra-LC and miniaturization of LC（micro-LC,capillary-LC,and nano-LC）,are also discussed.展开更多
The ginkgo terpenoids including bilobalide and ginkgolides are the main pharmaceutical components in the leaves or extracts of Ginkgo biloba L. In this paper, the analysis of bilobalide and ginkgolides in leaves of Gi...The ginkgo terpenoids including bilobalide and ginkgolides are the main pharmaceutical components in the leaves or extracts of Ginkgo biloba L. In this paper, the analysis of bilobalide and ginkgolides in leaves of Ginkgo biloba L. by high performance liquid chromatography (HPLC)-electrospray ionization (ESI)-mass spectrometry (MS) was carried out. The separation was performed on Inertsil ODS3 column with methanol-water (36:64) as mobile phase, with 1 mL·min -1 of flow rate at 35℃. Then the mass spectrum analysis was conducted by ZMD micromass electrospray ionization (ESI)-mass spectrometer (MS). The HPLC total ion chromatogram and selected ion chromatogram (with 325, 407, 423, 439 of m/z) of the sample and ESI-/MS mass spectra of the peaks in the chromatograms were obtained. So bilobalide, ginkgolide A, B, C and J in Ginkgo biloba L. leaves were identified. The method is easy and rapid, with a good accuracy.展开更多
A high performance 70nm CMOS device has been demonstrated for the first time in the continent, China. Some innovations in techniques are applied to restrain the short channel effect and improve the driving ability, ...A high performance 70nm CMOS device has been demonstrated for the first time in the continent, China. Some innovations in techniques are applied to restrain the short channel effect and improve the driving ability, such as 3nm nitrided oxide, dual poly Si gate electrode, novel super steep retrograde channel doping by heavy ion implantation, ultra shallow S/D extension formed by Ge PAI(Pre Amorphism Implantation) plus LEI(Low Energy Implantation), thin and low resistance Ti SALICIDE by Ge PAI and special cleaning, etc. The shortest channel length of the CMOS device is 70nm. The threshold voltages, G m and off current are 0 28V,490mS·mm -1 and 0 08nA/μm for NMOS and -0 3V,340mS·mm -1 and 0 2nA/μm for PMOS, respectively. Delays of 23 5ps/stage at 1 5V, 17 5ps/stage at 2 0V and 12 5ps/stage at 3V are achieved in the 57 stage unloaded 100nm CMOS ring oscillator circuits.展开更多
An improved high fan-in domino circuit is proposed. The nMOS pull-down network of the circuit is divided into several blocks to reduce the capacitance of the dynamic node and each block only needs a small keeper trans...An improved high fan-in domino circuit is proposed. The nMOS pull-down network of the circuit is divided into several blocks to reduce the capacitance of the dynamic node and each block only needs a small keeper transistor to maintain the noise margin. Because we omit the footer transistor, the circuit has better performance than the standard domino circuit. A 64-input OR-gate implemented with the structure is simulated using HSPICE under typical conditions of 0.13μm CMOS technology. The average delay of the circuit is 63.9ps, the average power dissipation is 32.4μW, and the area is l15μm^2. Compared to compound domino logic, the proposed circuit can reduce delay and power dissipation by 55% and 38%, respectively.展开更多
To develop a sensitive high performance liquid chromatography （HPLC） assay for the determination of trans-resveratrol in mouse liver. The whole liver of a mouse was removed from the body, homogenated, and extracted ...To develop a sensitive high performance liquid chromatography （HPLC） assay for the determination of trans-resveratrol in mouse liver. The whole liver of a mouse was removed from the body, homogenated, and extracted by ethyl acetate. The organic layer was isolated and evaporated to dryness, the residue was reconstituted in 0.2 mL mobile phase for centrifugation, and 50 uL of the supernatant was injected into the/-IPLC instrument. The sample was separated on a Shimadzu ODS column （150 mm × 4.6 mm, 5 um） at 35 ℃ and detected by ultraviolet （UV） detector at the wavelength of 305 nm. The mobile phase consisted of methanol and 0.1 mol/L acetic acid （4：6, v/v） with the flow-rote at 1 mL/min. The limit of detection was 3.0 ng/g in liver homogenate with a signal/noise ratio of 3：1. The linear range of the calibration curve was 5.0-120.0 ng/g. The mean recoveries at the concentrations of 6, 10 and 80 ng/g were 102%, 96.0% and 91.5%, respectively. The RSDs for inter- and intra-day assays were less than 5%. Compared with other reported methods, this method was faster and more sensitive. It was also proved to be of good linearity, selectivity, accuracy and precision, and can be efficiently applied to the pharmacoldnetic study of trans-resveratrol in mouse liver.展开更多
Objective High performance liquid chromatography(HPLC)and liquid chromatography-mass spectrometry(LC/MS)methods were developed for the determination of ganciclovir and its related substances.Methods A Hypersil ODS2 co...Objective High performance liquid chromatography(HPLC)and liquid chromatography-mass spectrometry(LC/MS)methods were developed for the determination of ganciclovir and its related substances.Methods A Hypersil ODS2 column(4.6 mm×250 mm,5 μm)was used with a mobile phase of 0.02 M potassium dihydrogen phosphate buffer(pH 6.0)-methanol(92∶8)at a flow rate of 1.0 mL/min,and UV detector set at 254 nm was used for monitoring the eluents.Results The method was simple,rapid,selective and capable of separating all related substances at trace level with a detection limit of 0.04 μg/mL.It has been validated with respect to accuracy,precision,linearity,and limits of detection and quantification.The linearity range was 10.2-153.0 μg/mL with r=0.9998.The percentage recoveries ranged from 96.7% to 101.6%,and RSD was 1.24%-1.96%(n=5).Conclusion The method was found to be suitable not only for monitoring the reactions during the process development but also for quality control of ganciclovir.For identification of related substances,LC/MS was used.The mainly related substances of ganciclovir active pharmaceutical ingredients(API)were determined as guanine,(1,3-dioxolan-4-yl)methyl acetate,and diacetyl guanine.展开更多
The influence of glycol,the main composition of the most frequently used aircraft dicer,on the freeze-thaw durability of high performance concrete（HPC）is investigated.Freeze-thaw durability of HPC is tested by accel...The influence of glycol,the main composition of the most frequently used aircraft dicer,on the freeze-thaw durability of high performance concrete（HPC）is investigated.Freeze-thaw durability of HPC is tested by accelerated freeze-thaw test.Four kinds of the solution,i.e.,tap water,3.5% NaCl solution,glycol solutions,and a LBR-A type commercial aircraft deicer are employed.Results show that freeze-thaw durability of HPC exposed to glycol solutions is closely related to the solution concentrations.The failure of HPC exposed to 3.5% glycol solution is similar to that of those exposed to 3.5% NaCl solution,i.e.,serious surface scaling.While the damage of HPC exposed to 12.5%—25% glycol solutions is postponed.Compared with glycol solution,the commercial aircraft deicer has much more negative effects on HPC freeze-thaw durability compared with 3.5% NaCl solution.In the presence of commercial aircraft deicer for HPC subjected to freeze-thaw cycles,the deterioration is mainly due to scaling and spalling.展开更多
Among pharmaceuticals and personal care products released into the aquatic environment, antibiotics are of particular concern, because of their ubiquity and health effects. Although scientists have recently paid more ...Among pharmaceuticals and personal care products released into the aquatic environment, antibiotics are of particular concern, because of their ubiquity and health effects. Although scientists have recently paid more attention to the threat of antibiotics to coastal ecosystems, researchers have often focused on relatively few antibiotics, because of the absence of suitable analytical methods. We have therefore developed a method for the rapid detection of 36 antibiotic residues in coastal waters, including tetracyclines （TCs）, sulfanilamides （SAs）, and quinolones （QLs）. The method consists of solid-phase extraction （SPE） and liquid chromatography-tandem mass spectrometry （LC-MS/MS） analysis, using electrospray ionization （ESI） in positive mode. The SPE was performed with Oasis HLB and Oasis MCX cartridges. Chromatographic separation on a Cr8 column was achieved using a binary eluent containing methanol and water with 0.1% formic acid. Typical recoveries of the analytes ranged from 67.4% to 109.3% at a fortification level of 100 ng/L. The precision of the method, calculated as relative standard deviation （RSD）, was below 14.6% for all the compounds. The limits of detection （LODs） varied from 0.45 pg to 7.97 pg. The method was applied to detemaine the target analytes in coastal waters of the Yellow Sea in Liaoning, China. Among the tested antibiotics, 31 were found in coastal ＇waters, with their concentrations between the LOD and 212.5 ng/L. These data indicate that this method is valid for analysis of antibiotics in coastal waters. The study first reports such a large number of antibiotics along the Yellow Sea coast of Liaoning, and should facilitate future comprehensive evaluation of antibiotics in coastal ecosystems展开更多
A novel method for the determination of five carbamate pesticides （metolcarb, carbofuran, carbaryl, isoprocard and diethofencard） in water samples was developed by dispersive liquid-liquid microextraction （DLLME） ...A novel method for the determination of five carbamate pesticides （metolcarb, carbofuran, carbaryl, isoprocard and diethofencard） in water samples was developed by dispersive liquid-liquid microextraction （DLLME） coupled with high performance liquid chromatography-diode array detector （HPLC-DAD）. Some experimental parameters that influence the extraction efficiency were studied and optimized to obtain the best extraction results. Under the optimum conditions for the method, the calibration curve was linear in the concentration range from 5 to 1000 ng mL^-1 for all the five carbamate pesticides, with the correlation coefficients （r^2） varying from 0.9984 to 0.9994. Good enrichment factors were achieved ranging from 80 to 177- fold, depending on the compound. The limits of detection （LODs） （S/N = 3） were ranged from 0.1 to 0.5 ng mL^-1. The method has been successfully applied to the analysis of the pesticide residues in environmental water samples.展开更多
The impact properties of normal concrete (NC) and reinforced concrete (RC) specimens,steel fibre reinforced concrete (SFRC) specimens and RC+SFRC specimens with different steel fibre dosages were investigated with the...The impact properties of normal concrete (NC) and reinforced concrete (RC) specimens,steel fibre reinforced concrete (SFRC) specimens and RC+SFRC specimens with different steel fibre dosages were investigated with the drop-weight impact test recommended by ACI Committee 544.The results indicate that the number of blows to final failure is greatly increased by addition of steel fibres.Moreover,the combination of steel fibres and steel rebars demonstrates a significant positive composite effect on the impact resistance,which results in the improvement in impact toughness of concrete specimens.In the view of variation of impact test results,the two-parameter Weibull distribution was adopted to analyze the experimental data.It is proved that the probabilistic distributions of the blows to first crack and to final failure of six types of samples approximately follow two-parameter Weibull distribution.展开更多
Based on an extensive experimental program,the paper studies the behavior of HPFRCC under triaxial compression. The experimental parameters are lateral confining pressure and PVA fiber content by volume. The test resu...Based on an extensive experimental program,the paper studies the behavior of HPFRCC under triaxial compression. The experimental parameters are lateral confining pressure and PVA fiber content by volume. The test results indicate that ultimate strength and peak strain are significantly improved with the increases of confining pressure. The confining effect introduced by the fibers becomes minor in triaxial compression tests,where there is relatively high external confining pressure. The axial stress-strain curves with different confining pressure and different PVA fiber content by volume are obtained. Lateral confining pressure constraints the lateral expansion of HPFRCC,so there is a big plastic deformation with its ultimate strength improved. At lower confining pressure,PVA fiber content by volume has some effect on the decreased section of stress-strain curve. According to test results,the paper establishes formula of confining pressure with ultimate strength and axial peak strain respectively.展开更多
It is expected that in the new century, to cope with developments of new high temperature technologies , a new generation of high performance refractory ceramics will e-merge and flourish which should include the foll...It is expected that in the new century, to cope with developments of new high temperature technologies , a new generation of high performance refractory ceramics will e-merge and flourish which should include the following (1) oxide and nonoxide composites characterized by a unique combination of high hot strength , high thermal shock resistance and high corrosion resistance ; (2) free CaO bearing basic refractories capable of purifying molten metal for improving cleanliness and of absorbing contaminants from waste gases for reducing environmental pollution ; (3) free flowing zero cement castables with improved thermome-chanical properties , thermal shock resistance and corrosion resistance and gradient castables with varying matrix composition and varying texture.展开更多
A rapid and accurate high performance liquid chromatography tandem mass spectrometry（HPLS-MS） method was established for quantification of chlorpromazine in pork. The porcine samples were pretreated with acetonitril...A rapid and accurate high performance liquid chromatography tandem mass spectrometry（HPLS-MS） method was established for quantification of chlorpromazine in pork. The porcine samples were pretreated with acetonitrile to precipitate proteins and followed by extraction with tert--butyl methyl ether（TBME）. The separation was performed on a 5 μm Agilent XDB--C18 column with gradient elution. The mobile phase A was 0.01 mol/L ammonium formate in water and mobile phase B was acetonitrile. The flow rate was at 0.8 mL/min. Quantification was performed on a triple-quadrupole tandem mass spectrometer using the multiple selected reaction monitoring（MRM） mode. Transition of m/z ＋319.1 to 58.1 was used for the quantification of chlorpromazine. The method was validated at the concentration range of 0.4040 μg/kg to 8.080 μg/kg for chlorpromazine with correlation coefficient of 0.9999. The spiked recoveries were more than 80.0% and the limit of detection（LOD） was 0.052 μg/kg. The developed method, which offers advantages of convenience, rapid, specificity and higher sensitivity, can be used for determination of chlorpromazine hydrochloride in porcine muscles.展开更多
AIM： To observe the effect of protocatechuic aldchyde on the proliferation of hepatic stellate cells （HSCs）. METHODS： Liver fibrosis was induced in rats by carbon tetrachloride （CCh）. Then normal and fibrotic dr...AIM： To observe the effect of protocatechuic aldchyde on the proliferation of hepatic stellate cells （HSCs）. METHODS： Liver fibrosis was induced in rats by carbon tetrachloride （CCh）. Then normal and fibrotic drug sera were extracted from rats. The effects of protocatechuic aldchyde, raw Radix Salvia miltiorrhiza and drug sera of Salvia miltiorrhiza on HSC growth were determined by CCKoS. The protocatechuic aldchyde was separated by high performance liquid chromatography （HPLC） in a AIItima C18 column （250 mm × 4.6 mm, 5 μm） with a mobile phase of acetonitrile-4% glacial acetic acid solution （gradient elution） at the wavelength of 281 nm. RESULTS： Protocatechuic aldchyde, raw Radix Salvia miltiorrhiza and drug sera of Salvia miltiorrhiza were found to have inhibitory effects on proliferation of rat HSCs. Raw Radix Salvia miltiorrhiza had a stronger inhibitory effect than the drug sera. The fibrotic drug sera showed a higher suppressive effect than the normal drug sera （P 〈 0.05）. Protocatechuic aldchyde was found in crude materials of both Radix Salvia miltiorrhiza and its corresponding drug sera. The average recovery （n = 6） was 110.5% for raw Salvia miltiorrhiza Bge, 102% for normal drug sera and 105.2% for fibrotic drug sera. The relative standard devitation （RSD） was 0.37%, 1.96% and 1.51%, respectively （n=6）. The contents of protocatechuic aldchyde were 0.22%, 0.15% and 0.19%, respectively （n = 6） （P〈 0.05）. The RSD was 0.33%, 0.75% and 1.24% （n=6） for raw material of Radix Salvia miltiorrhiza, normal drug sera and fibrotic drug sera, respectively. The samples were stable for 6 d. CONCLUSION： Protocatechuic aldchyde can inhibit the growth of HSCs. HPLC is suitable for the determination of virtual bioactive components of Chinese herbal medicines in vitro.展开更多
Methods for determining nine low molecular weight organic acids in root exudates were developed by using reversed phase high performance liquid chromatography with UV (ultraviolet) detection at 214 nm. The mobile ph...Methods for determining nine low molecular weight organic acids in root exudates were developed by using reversed phase high performance liquid chromatography with UV (ultraviolet) detection at 214 nm. The mobile phase was 18 mmol L -1 kH 2PO 4 adjusted to pH 2.25 with phosphoric acid and the flow rate was 0.3 mL min -1 . The analytical column was a reversed phase silica based C 18 column (Shim pack CLC ODS). The root exudates were collected through submerging the whole root system into aerated deionized water for 2 hours. The filtered exudate solutions were concentrated to dryness by rotary evaporation at 40 °C, dissolved in 10 mL mobile phase. The chromatographic conditions of organic acid determination were analyzed. The results showed that there was a high selectivity and sensitivity in the organic acid determination by reversed phase high performance liquid chromatography. Coefficients of variation for organic acid determination were lower than 10% except lactic acid. The recoveries were consistently between 80.1% to 108.3%. Detection limits were approximately 0.05 to 4.5 mg L -1 for organic acids except succinic acid with the detection limit of 7.0 mg L -1 . Phosphorus deficiency may contribute to the release of organic acids in soybean root exudates especially malic, lactic and citric acids.展开更多
文摘A high-performance liquid chromatography(HPLC)method has been developed using a CAPCELL PAK ADME(150 mm×4.6 mm,5μm)as analytical column and a gradient elution with 15 min using acetonitrile and 0.1%(in volume fraction)phosphoric acid water(pH=2.2)as the mobile phase.Three active substances in cosmetics were quantitatively detected simultaneously at a detection wavelength of 265 nm.The linear ranges of β-nicotinamide mononucleotides,ergothioneine and nicotinamide are 10~200 mg/L,5~100 mg/L and 5~100 mg/L respectively and the detection limits of three components are 3.0 mg/L,1.5 mg/L and 1.5 mg/L respectively.The recovery rate is 97.1~104.9%,with RSD≤2.0%.The method was applied to quantitative analysis of five samples of cosmetics toner,lotion,cream,essence and gel and three samples of raw materials.The results showed that the results of β-nicotinamide mononucleotide and ergothioneine in five cosmetics were consistent with the product label,while nicotinamide was inconsistent with the label.The purity of the three raw material samples was 99.5%,99.7% and 100.8%respectively.This method offers high precision,accuracy and short analysis time,making it a reliable approach for studying three active ingredients in cosmetics and suitable for quality control of related functional ingredients.
基金financially supported by the National Natural Science Foundation of China(Nos.52075351,51604177)the National Key Research and Development Program of China(No.2019YFA0705701)+4 种基金the National Funded Postdoctoral Researcher Program(No.GZC20231762)the Major S&T Infrastructure Construction Project of Sichuan Province(No.2020-510000-73-01441847)the International S&T Innovation Cooperation Program of Sichuan Province(No.2020YFH0039)the Chengdu International S&T Cooperation Funded Project(Nos.2020-GH02-00006HZ,2022-GH02-00027-HZ)the“1000 Talents Plan”of Sichuan Province,and the Talent Introduction Program of Sichuan University(No.YJ201410)。
文摘Anode active materials involving transition metal oxides and sulfides are of great significance for high energy density lithium-ion batteries(LIBs),but the huge volume expansion and inferior electronic conductivity upon cycling critically constrain their further application.Herein,from a new perspective,a highly conductive and stable 3D flexible composite current collector is rationally designed by facilely electrodepositing metallic Ni thin layer onto the carbon cloth(CC/Ni),which endows the supported active materials with exceptional electronic conductivity and structural stability.In addition,the homogeneously distributed metallic Ni protrusions external CC can strongly bond with the active components,ensuring the structural integrity of electrodes upon cycling.More importantly,the 3D network structure with large specific surface area provides abundant space to alleviate the volume expansion and more active sites for electrochemical reactions.Therefore,taking Ni_(3)S_(2)nanosheet(Ni_(3)S_(2)NS)anode as an example,the prepared Ni_(3)S_(2)NS@CC/Ni electrode shows a high specific capacity of 2.32 mAh/cm^(2)at 1mA/cm^(2)and high capacity retention of 1.68 mAh/cm^(2)at a high rate of 8mA/cm^(2).This study provides a universal approach to obtain highly conductive and stable 3D flexible current collectors towards high performance metal-ion batteries beyond LIBs.
基金supported by the National Natural Science Foundation of China(Nos.51938005,52090082,and 52378395)the National Key Research and Development Program of China(No.2023YFB2604402).
文摘This study aims to assess the comprehensive strengthening effect of a steel-ultra high performance concrete(UHPC)composite strengthening method.The axial force-moment interaction curve(N-M curve)was calculated in a novel way,using cross-sectional strains at ultimate states as well as real-time stress measurements for each material.The enclosed area of the N-M curve was defined as a comprehensive performance index for the system.We validate our approach with comparisons to numerical modeling and full-scale four-point bending experiments.Additionally,strengthening effects were compared for different sagging and hogging moments based on material stress responses,and the impact of various strengthening parameters was analyzed.We find that the N-M curve of the strengthened cross-section envelops that of the un-strengthened cross-section.Notably,improvements in flexural capacity are greater under sagging moments during the large eccentric failure stage,and greater under hogging moments during the small eccentric failure stage.This discrepancy is attributed to the strength utilization of strengthening materials.These findings provide a reference for understanding the strengthening effects and parameters of steel-UHPC composite.
文摘In this study, an optimized high performance liquid chromatography-fluorescence detector (HPLC-FL) method for the determination of benzo[a]pyrene in edible oil was established. HPLC was performed with Thermo Fisher Scientific C18 column (250 mm×4.6 mm, 5 μm) as the chromatographic column and acetonitrile and water as the mobile phase, and the excitation wavelength and emission wavelength of fluorescence detector were 286 and 430 nm, respectively. The response was high, and the linear range was 0.5-10.0 ng/ml. The lowest limit of detection was 0.11 ng/ml, and the average recovery was 92.5%. This method is suitable for quantitative analysis of benzo[a]pyrene content in edible oil.
基金Supported by the National Basic Research Programe of China("973"Program)(2009CB623203)the Construction Department of Zhejiang Province Foundation(1006)+1 种基金the Education Department of Zhejiang Province Foundation(Y200909029)the Doctoral Innovation Foundation of Nanjing University of Aeronautics andAstronautics(BCXJ07-04)~~
文摘Influences of admixtures on the workability and strength of high performance concrete （HPC） are in- vestigated. The types of investigated admixtures include naphthalene series high range water reducing agent, polycarboxlic series high range water reduce agent and sodium sulfate hardening accelerating agent. Two kinds of curing condition, namely steam curing condition and standard curing condition, are adopted. The result shows that HPC, added with polycarboxlic series of high performance water reducer, has high workability and strength, while sodium sulfate accelerating agent causes poor workability and low strength. Thus for vapor-cured HPC and its formulations, naphthalene series high range water reducing agent with less sodium sulfate should be given pri- ority. Therefore, the differences of curing conditions should be considered when selecting HPC admixtures.
基金Administration Bureau of Traditional Chinese Medicine(2007-2008)for Scientific Research Program of TCM (Grant No.HL07057)
文摘Due to their biological and physiological importance,flavonoids receive considerable attention in the literature. Nowadays,high performance liquid chromatography（HPLC）is the most widely used analytical method.In this review,we summarize the principle of the choice of HPLC column and mobile phase,discuss and compare the features of various detections such as UV,fluorescence detection,electrochemical detection,chemilummescence detection,UV-MS etc.Recent developments in HPLC including ultra-LC and miniaturization of LC（micro-LC,capillary-LC,and nano-LC）,are also discussed.
文摘The ginkgo terpenoids including bilobalide and ginkgolides are the main pharmaceutical components in the leaves or extracts of Ginkgo biloba L. In this paper, the analysis of bilobalide and ginkgolides in leaves of Ginkgo biloba L. by high performance liquid chromatography (HPLC)-electrospray ionization (ESI)-mass spectrometry (MS) was carried out. The separation was performed on Inertsil ODS3 column with methanol-water (36:64) as mobile phase, with 1 mL·min -1 of flow rate at 35℃. Then the mass spectrum analysis was conducted by ZMD micromass electrospray ionization (ESI)-mass spectrometer (MS). The HPLC total ion chromatogram and selected ion chromatogram (with 325, 407, 423, 439 of m/z) of the sample and ESI-/MS mass spectra of the peaks in the chromatograms were obtained. So bilobalide, ginkgolide A, B, C and J in Ginkgo biloba L. leaves were identified. The method is easy and rapid, with a good accuracy.
文摘A high performance 70nm CMOS device has been demonstrated for the first time in the continent, China. Some innovations in techniques are applied to restrain the short channel effect and improve the driving ability, such as 3nm nitrided oxide, dual poly Si gate electrode, novel super steep retrograde channel doping by heavy ion implantation, ultra shallow S/D extension formed by Ge PAI(Pre Amorphism Implantation) plus LEI(Low Energy Implantation), thin and low resistance Ti SALICIDE by Ge PAI and special cleaning, etc. The shortest channel length of the CMOS device is 70nm. The threshold voltages, G m and off current are 0 28V,490mS·mm -1 and 0 08nA/μm for NMOS and -0 3V,340mS·mm -1 and 0 2nA/μm for PMOS, respectively. Delays of 23 5ps/stage at 1 5V, 17 5ps/stage at 2 0V and 12 5ps/stage at 3V are achieved in the 57 stage unloaded 100nm CMOS ring oscillator circuits.
基金the National High-Tech Research and Development Program of China(No.2005AA110020)~~
文摘An improved high fan-in domino circuit is proposed. The nMOS pull-down network of the circuit is divided into several blocks to reduce the capacitance of the dynamic node and each block only needs a small keeper transistor to maintain the noise margin. Because we omit the footer transistor, the circuit has better performance than the standard domino circuit. A 64-input OR-gate implemented with the structure is simulated using HSPICE under typical conditions of 0.13μm CMOS technology. The average delay of the circuit is 63.9ps, the average power dissipation is 32.4μW, and the area is l15μm^2. Compared to compound domino logic, the proposed circuit can reduce delay and power dissipation by 55% and 38%, respectively.
基金Postdoctoral Scientific Research Station of Gansu Yasheng Groups.
文摘To develop a sensitive high performance liquid chromatography （HPLC） assay for the determination of trans-resveratrol in mouse liver. The whole liver of a mouse was removed from the body, homogenated, and extracted by ethyl acetate. The organic layer was isolated and evaporated to dryness, the residue was reconstituted in 0.2 mL mobile phase for centrifugation, and 50 uL of the supernatant was injected into the/-IPLC instrument. The sample was separated on a Shimadzu ODS column （150 mm × 4.6 mm, 5 um） at 35 ℃ and detected by ultraviolet （UV） detector at the wavelength of 305 nm. The mobile phase consisted of methanol and 0.1 mol/L acetic acid （4：6, v/v） with the flow-rote at 1 mL/min. The limit of detection was 3.0 ng/g in liver homogenate with a signal/noise ratio of 3：1. The linear range of the calibration curve was 5.0-120.0 ng/g. The mean recoveries at the concentrations of 6, 10 and 80 ng/g were 102%, 96.0% and 91.5%, respectively. The RSDs for inter- and intra-day assays were less than 5%. Compared with other reported methods, this method was faster and more sensitive. It was also proved to be of good linearity, selectivity, accuracy and precision, and can be efficiently applied to the pharmacoldnetic study of trans-resveratrol in mouse liver.
文摘Objective High performance liquid chromatography(HPLC)and liquid chromatography-mass spectrometry(LC/MS)methods were developed for the determination of ganciclovir and its related substances.Methods A Hypersil ODS2 column(4.6 mm×250 mm,5 μm)was used with a mobile phase of 0.02 M potassium dihydrogen phosphate buffer(pH 6.0)-methanol(92∶8)at a flow rate of 1.0 mL/min,and UV detector set at 254 nm was used for monitoring the eluents.Results The method was simple,rapid,selective and capable of separating all related substances at trace level with a detection limit of 0.04 μg/mL.It has been validated with respect to accuracy,precision,linearity,and limits of detection and quantification.The linearity range was 10.2-153.0 μg/mL with r=0.9998.The percentage recoveries ranged from 96.7% to 101.6%,and RSD was 1.24%-1.96%(n=5).Conclusion The method was found to be suitable not only for monitoring the reactions during the process development but also for quality control of ganciclovir.For identification of related substances,LC/MS was used.The mainly related substances of ganciclovir active pharmaceutical ingredients(API)were determined as guanine,(1,3-dioxolan-4-yl)methyl acetate,and diacetyl guanine.
基金Supported by the National Basic Research Program of China("973"Program)(2009CB623203)the China Postdoctoral Science Foundation(20070421036)+1 种基金the Natural Science Foundation of Jiangsu Province(BK2005216)the Research Foundation of Nanjing University of Aeronautics and Astronautics(NS2010015)~~
文摘The influence of glycol,the main composition of the most frequently used aircraft dicer,on the freeze-thaw durability of high performance concrete（HPC）is investigated.Freeze-thaw durability of HPC is tested by accelerated freeze-thaw test.Four kinds of the solution,i.e.,tap water,3.5% NaCl solution,glycol solutions,and a LBR-A type commercial aircraft deicer are employed.Results show that freeze-thaw durability of HPC exposed to glycol solutions is closely related to the solution concentrations.The failure of HPC exposed to 3.5% glycol solution is similar to that of those exposed to 3.5% NaCl solution,i.e.,serious surface scaling.While the damage of HPC exposed to 12.5%—25% glycol solutions is postponed.Compared with glycol solution,the commercial aircraft deicer has much more negative effects on HPC freeze-thaw durability compared with 3.5% NaCl solution.In the presence of commercial aircraft deicer for HPC subjected to freeze-thaw cycles,the deterioration is mainly due to scaling and spalling.
基金Supported by Young Scientists Research Program (No. 2009507)the Key Laboratory of Marine Bioactive Substances and Modern Analytical Techniques (No. MBSMAT-2010-04),SOA of China
文摘Among pharmaceuticals and personal care products released into the aquatic environment, antibiotics are of particular concern, because of their ubiquity and health effects. Although scientists have recently paid more attention to the threat of antibiotics to coastal ecosystems, researchers have often focused on relatively few antibiotics, because of the absence of suitable analytical methods. We have therefore developed a method for the rapid detection of 36 antibiotic residues in coastal waters, including tetracyclines （TCs）, sulfanilamides （SAs）, and quinolones （QLs）. The method consists of solid-phase extraction （SPE） and liquid chromatography-tandem mass spectrometry （LC-MS/MS） analysis, using electrospray ionization （ESI） in positive mode. The SPE was performed with Oasis HLB and Oasis MCX cartridges. Chromatographic separation on a Cr8 column was achieved using a binary eluent containing methanol and water with 0.1% formic acid. Typical recoveries of the analytes ranged from 67.4% to 109.3% at a fortification level of 100 ng/L. The precision of the method, calculated as relative standard deviation （RSD）, was below 14.6% for all the compounds. The limits of detection （LODs） varied from 0.45 pg to 7.97 pg. The method was applied to detemaine the target analytes in coastal waters of the Yellow Sea in Liaoning, China. Among the tested antibiotics, 31 were found in coastal ＇waters, with their concentrations between the LOD and 212.5 ng/L. These data indicate that this method is valid for analysis of antibiotics in coastal waters. The study first reports such a large number of antibiotics along the Yellow Sea coast of Liaoning, and should facilitate future comprehensive evaluation of antibiotics in coastal ecosystems
基金supported both by the Natural Science Foundations of Hebei(No.B2008000210)the Scientific Research Foundation of Agricultural University of Hebei.
文摘A novel method for the determination of five carbamate pesticides （metolcarb, carbofuran, carbaryl, isoprocard and diethofencard） in water samples was developed by dispersive liquid-liquid microextraction （DLLME） coupled with high performance liquid chromatography-diode array detector （HPLC-DAD）. Some experimental parameters that influence the extraction efficiency were studied and optimized to obtain the best extraction results. Under the optimum conditions for the method, the calibration curve was linear in the concentration range from 5 to 1000 ng mL^-1 for all the five carbamate pesticides, with the correlation coefficients （r^2） varying from 0.9984 to 0.9994. Good enrichment factors were achieved ranging from 80 to 177- fold, depending on the compound. The limits of detection （LODs） （S/N = 3） were ranged from 0.1 to 0.5 ng mL^-1. The method has been successfully applied to the analysis of the pesticide residues in environmental water samples.
基金Project(50578026) supported by the National Natural Science Foundation of ChinaProject supported by FCT (SFRH/BPD/22680/2005)and Research Center of Mathematics of the University of Minho through the FCT Pluriannual Funding Program
文摘The impact properties of normal concrete (NC) and reinforced concrete (RC) specimens,steel fibre reinforced concrete (SFRC) specimens and RC+SFRC specimens with different steel fibre dosages were investigated with the drop-weight impact test recommended by ACI Committee 544.The results indicate that the number of blows to final failure is greatly increased by addition of steel fibres.Moreover,the combination of steel fibres and steel rebars demonstrates a significant positive composite effect on the impact resistance,which results in the improvement in impact toughness of concrete specimens.In the view of variation of impact test results,the two-parameter Weibull distribution was adopted to analyze the experimental data.It is proved that the probabilistic distributions of the blows to first crack and to final failure of six types of samples approximately follow two-parameter Weibull distribution.
基金support from the youth science fund project of China (50908187)Henan provincial natural science research project ( 2010B560006 )Shanxi provinces youth fund project(2009JQ7013)
文摘Based on an extensive experimental program,the paper studies the behavior of HPFRCC under triaxial compression. The experimental parameters are lateral confining pressure and PVA fiber content by volume. The test results indicate that ultimate strength and peak strain are significantly improved with the increases of confining pressure. The confining effect introduced by the fibers becomes minor in triaxial compression tests,where there is relatively high external confining pressure. The axial stress-strain curves with different confining pressure and different PVA fiber content by volume are obtained. Lateral confining pressure constraints the lateral expansion of HPFRCC,so there is a big plastic deformation with its ultimate strength improved. At lower confining pressure,PVA fiber content by volume has some effect on the decreased section of stress-strain curve. According to test results,the paper establishes formula of confining pressure with ultimate strength and axial peak strain respectively.
文摘It is expected that in the new century, to cope with developments of new high temperature technologies , a new generation of high performance refractory ceramics will e-merge and flourish which should include the following (1) oxide and nonoxide composites characterized by a unique combination of high hot strength , high thermal shock resistance and high corrosion resistance ; (2) free CaO bearing basic refractories capable of purifying molten metal for improving cleanliness and of absorbing contaminants from waste gases for reducing environmental pollution ; (3) free flowing zero cement castables with improved thermome-chanical properties , thermal shock resistance and corrosion resistance and gradient castables with varying matrix composition and varying texture.
文摘A rapid and accurate high performance liquid chromatography tandem mass spectrometry（HPLS-MS） method was established for quantification of chlorpromazine in pork. The porcine samples were pretreated with acetonitrile to precipitate proteins and followed by extraction with tert--butyl methyl ether（TBME）. The separation was performed on a 5 μm Agilent XDB--C18 column with gradient elution. The mobile phase A was 0.01 mol/L ammonium formate in water and mobile phase B was acetonitrile. The flow rate was at 0.8 mL/min. Quantification was performed on a triple-quadrupole tandem mass spectrometer using the multiple selected reaction monitoring（MRM） mode. Transition of m/z ＋319.1 to 58.1 was used for the quantification of chlorpromazine. The method was validated at the concentration range of 0.4040 μg/kg to 8.080 μg/kg for chlorpromazine with correlation coefficient of 0.9999. The spiked recoveries were more than 80.0% and the limit of detection（LOD） was 0.052 μg/kg. The developed method, which offers advantages of convenience, rapid, specificity and higher sensitivity, can be used for determination of chlorpromazine hydrochloride in porcine muscles.
文摘AIM： To observe the effect of protocatechuic aldchyde on the proliferation of hepatic stellate cells （HSCs）. METHODS： Liver fibrosis was induced in rats by carbon tetrachloride （CCh）. Then normal and fibrotic drug sera were extracted from rats. The effects of protocatechuic aldchyde, raw Radix Salvia miltiorrhiza and drug sera of Salvia miltiorrhiza on HSC growth were determined by CCKoS. The protocatechuic aldchyde was separated by high performance liquid chromatography （HPLC） in a AIItima C18 column （250 mm × 4.6 mm, 5 μm） with a mobile phase of acetonitrile-4% glacial acetic acid solution （gradient elution） at the wavelength of 281 nm. RESULTS： Protocatechuic aldchyde, raw Radix Salvia miltiorrhiza and drug sera of Salvia miltiorrhiza were found to have inhibitory effects on proliferation of rat HSCs. Raw Radix Salvia miltiorrhiza had a stronger inhibitory effect than the drug sera. The fibrotic drug sera showed a higher suppressive effect than the normal drug sera （P 〈 0.05）. Protocatechuic aldchyde was found in crude materials of both Radix Salvia miltiorrhiza and its corresponding drug sera. The average recovery （n = 6） was 110.5% for raw Salvia miltiorrhiza Bge, 102% for normal drug sera and 105.2% for fibrotic drug sera. The relative standard devitation （RSD） was 0.37%, 1.96% and 1.51%, respectively （n=6）. The contents of protocatechuic aldchyde were 0.22%, 0.15% and 0.19%, respectively （n = 6） （P〈 0.05）. The RSD was 0.33%, 0.75% and 1.24% （n=6） for raw material of Radix Salvia miltiorrhiza, normal drug sera and fibrotic drug sera, respectively. The samples were stable for 6 d. CONCLUSION： Protocatechuic aldchyde can inhibit the growth of HSCs. HPLC is suitable for the determination of virtual bioactive components of Chinese herbal medicines in vitro.
文摘Methods for determining nine low molecular weight organic acids in root exudates were developed by using reversed phase high performance liquid chromatography with UV (ultraviolet) detection at 214 nm. The mobile phase was 18 mmol L -1 kH 2PO 4 adjusted to pH 2.25 with phosphoric acid and the flow rate was 0.3 mL min -1 . The analytical column was a reversed phase silica based C 18 column (Shim pack CLC ODS). The root exudates were collected through submerging the whole root system into aerated deionized water for 2 hours. The filtered exudate solutions were concentrated to dryness by rotary evaporation at 40 °C, dissolved in 10 mL mobile phase. The chromatographic conditions of organic acid determination were analyzed. The results showed that there was a high selectivity and sensitivity in the organic acid determination by reversed phase high performance liquid chromatography. Coefficients of variation for organic acid determination were lower than 10% except lactic acid. The recoveries were consistently between 80.1% to 108.3%. Detection limits were approximately 0.05 to 4.5 mg L -1 for organic acids except succinic acid with the detection limit of 7.0 mg L -1 . Phosphorus deficiency may contribute to the release of organic acids in soybean root exudates especially malic, lactic and citric acids.
