An experimental platform of a pulse detonation engine(PDE) was established to study the effect of different K_2 CO_3 ionized seed mass contents on the detonation process.The pressure and ion concentration were detecte...An experimental platform of a pulse detonation engine(PDE) was established to study the effect of different K_2 CO_3 ionized seed mass contents on the detonation process.The pressure and ion concentration were detected in the detonation process of the PDE with different contents of ionized seeds.The initiation process of the PDE at different ignition frequencies was studied.The results show that the gas conductivity in the detonation process increased by adding ionized seeds to the PDE tube,and the conductivity increased with the increase in ionized seed mass content.With the increase in ionized seed mass content,the range of the conductivity decreased.The PDE was successfully ignited and formed a stable detonation wave at ignition frequencies of 5 Hz and 10 Hz,and the peak pressure of the stable detonation with the ignition frequency of 5 Hz was 17% higher than that with an ignition frequency of 10 Hz.The detonation wave intensity was weake ned and dege nerated to a shock wave that propagated in the tube without the fuel filled at the ignition frequency of 20 Hz.展开更多
The reverse magnetohydrodynamic(MHD)energy bypass technology is a promising energy redis⁃tribution technology in the scramjet system,in augmented with a power generation equipment to supply the neces⁃sary long-distanc...The reverse magnetohydrodynamic(MHD)energy bypass technology is a promising energy redis⁃tribution technology in the scramjet system,in augmented with a power generation equipment to supply the neces⁃sary long-distance flight airframe power.In this paper,a computational model of the scramjet magnetohydrody⁃namic channel is developed and verified by using the commercial software Fluent.It is found that when the mag⁃netic induction intensity is 1,2,3,4 T,the power generation efficiency is 22.5%,22.3%,22.0%,21.5%,and decreases with the increase of the magnetic induction intensity,and the enthalpy extraction rate is 0.026%,0.1%,0.21%,0.34%,and increases with the increase of the magnetic induction intensity.The deceleration ef⁃fect of electromagnetic action on the airflow in the power channel increases with the increase of magnetic induc⁃tion intensity.The stronger the magnetic field intensity,the more obvious the decreasing effect of fluid Mach num⁃ber in the channel.The power generation efficiency decreases as the magnetic induction intensity increases and the enthalpy extraction rate is reversed.As the local currents gathering at inlet and outlet of the power generation area,total temperature and enthalpy along the flow direction do not vary linearly,and there are maximum and minimum values at inlet and outlet.Increasing the number of electrodes can effectively regulate the percentage of Joule heat dissipation,which can improve the power generation efficiency.展开更多
In order to achieve a wider range of ionizing radiations detection,novel fluorescence sensing materials have been developed that utilize the fluorescence enhancement phenomenon caused by the intramolecular photoinduce...In order to achieve a wider range of ionizing radiations detection,novel fluorescence sensing materials have been developed that utilize the fluorescence enhancement phenomenon caused by the intramolecular photoinduced electron transfer(PET)effect.Two perylene diimide isomers PDI-P and PDI-B were designed and synthesized,and their molecular structures were characterized by high-resolution Fourier transform mass spectrometry(HRMS),nuclear magnetic resonance hydrogen and carbon spectroscopy(~1H and~(13)C NMR).The interaction between ionizing radiation and fluorescent molecules was simulated by HCl titration.The results show that combining PDIs and HCl can improve fluorescence through the retro-PET process.Despite the similarities in chemical structures,the fluorescent enhancement multiple of PDI-B with aromatic amine as electron donor is much higher than that of PDI-P with alkyl amine.In the direct irradiation experiments of ionizing radiation,the emission enhancement multiples of PDI-P and PDI-B are 2.01 and 45.4,respectively.Furthermore,density functional theory(DFT)and time-dependent density functional theory(TDDFT)calculations indicate that the HOMO and HOMO-1 energy ranges of PDI-P and PDI-B are 0.54 e V and 1.13 e V,respectively.A wider energy range has a stronger driving force on electrons,which is conducive to fluorescence quenching.Both femtosecond transient absorption spectroscopy(fs-TAS)and transient fluorescence spectroscopy(TFS)tests show that PDI-B has shorter charge separation lifetime and higher electron transfer rate constant.Although both isomers can significantly reduce LOD during PET process,PDI-B with aromatic amine has a wider detection range of 0.118—240 Gy due to its larger emission enhancement,which is a leap of three orders of magnitude.It breaks through the detection range of gamma radiation reported in existing studies,and provides theoretical support for the further study of sensitive and effective new materials for ionizing radiation detection.展开更多
A GC-NCI-MS method was developed for the determination of chlorfenapyr residues in eggplant and soil sample.The sample was extracted by the mixture solvent of acetone-dichloromethane(4 ∶3,by volume),and cleaned up by...A GC-NCI-MS method was developed for the determination of chlorfenapyr residues in eggplant and soil sample.The sample was extracted by the mixture solvent of acetone-dichloromethane(4 ∶3,by volume),and cleaned up by chromatographic column of aluminum oxide-graphitized carbon black.The analysis of extract was performed by gas chromatography-negative chemical ionization-mass spectrometry(GC-NCI-MS).The recoveries of chlorfenapyr at the spiked concentration levels of 0.1,1.0,10.0 mg/kg were 100%-116% for eggplant sample with RSD of 2.0%-6.2%,and 83%-116% for the soil sample with RSD of 1.1%-4.5%,respectively.展开更多
A direct determination method for the atrazine residue on the vegetable was developed by using desorption electrospray ionization mass spectrometry (DESI MS) without any sample pretreatment.Acetonitrile-water (1:1,v/v...A direct determination method for the atrazine residue on the vegetable was developed by using desorption electrospray ionization mass spectrometry (DESI MS) without any sample pretreatment.Acetonitrile-water (1:1,v/v),which contained 0.1% formic acid,was used as the spray solvent.The working conditions,such as ESI gas inlet pressure,ESI flow rate,ESI spray voltage,spray-to-sample distance,spray-to-cone-hole distance and the collision induced dissociation (CID) voltage for MS/MS,were optimized for both DESI and esquires 6 000 mass spectrometer.The linear range of atrazine on cabbage leaves was 25.25-2 525 pg/mm2,the R2 was 0.991 6,and the relative standard deviations were between 3.37% and 26.17%.The LOD of atrazine calculated by S/N=3 was 2.50 pg/mm2.展开更多
Technique of lutetium isotopic analysis by laser resonance ionization mass spectrometry(LRIMS) was developed in the presence of isobaric interference. In the case of real sample, the elemental selectivity was better t...Technique of lutetium isotopic analysis by laser resonance ionization mass spectrometry(LRIMS) was developed in the presence of isobaric interference. In the case of real sample, the elemental selectivity was better than 8×105, and the detection efficiency was 8.3×10-5. The technique of wavelength scanning method was set up in order that the accurate isotopic ratio could be determined. And the numerical computational method was provided to calculate the correct factor of isotopic ratio. Using this technique, the isotopic ratio measured by LRIMS is in good agreement with standard value measured by TIMS.展开更多
Puerarin,an isoflavone compound,is the bioactive component of traditional Chinese medicine.A novel dialkyl puerarin-7-yl phosphate was synthesized and investigated by positive ion electrospray ionization ion trap mass...Puerarin,an isoflavone compound,is the bioactive component of traditional Chinese medicine.A novel dialkyl puerarin-7-yl phosphate was synthesized and investigated by positive ion electrospray ionization ion trap mass spectrometry (ESI MS)in conjunction with tandem mass spectrometry.The fragmentation pathways of dialkyl puerarin-7-yl phosphates were investigated.展开更多
采用气相色谱-氢火焰离子化检测器法(gas chromatography with hydrogen flame ionization detection,GCFID)、顶空固相微萃取-气相色谱-质谱(headspace solid-phase microextraction coupled with gas chromatography-mass spectrometr...采用气相色谱-氢火焰离子化检测器法(gas chromatography with hydrogen flame ionization detection,GCFID)、顶空固相微萃取-气相色谱-质谱(headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry,HS-SPME-GC-MS)和电子鼻技术分析6种果酒中的挥发性成分,评价果酒风味轮廓特征的差异性。结果表明,GC-FID定量测定樱桃李酒,其中异戊醇、活性戊醇、β-苯乙醇含量最高,乙酸乙酯含量最低;木瓜酒中正丙醇、2,3-丁二醇、癸酸乙酯、乙酸含量最高; 3-羟基-2-丁酮含量在樱桃李酒中最高,山楂酒、甜橙酒中最少。HP-SPME-GC-MS鉴定果酒中挥发性物质94种,其中醇类23种,酯类43种,醛酮类10种,酸类8种,酚类2种,苯环类5种,烷烃类3种。山楂酒、菠萝酒、木瓜酒、甜橙酒、无花果酒和樱桃李酒中香气物质数量分别为34、44、45、45、33、47种。其中山楂酒、木瓜酒和无花果酒中未检出酚类、烷烃类物质。电子鼻对不同果酒香气的区分效果无重叠,W5S传感器区分果酒香气能力最强。比较而言,菠萝酒和樱桃李酒的口感更圆润,香气更愉悦,感官得分最高。展开更多
As the transmission line corridors become more and more rare in China,it is now inevitable for people to construct HVAC-HVDC hybrid transmission lines.The research on the electric field around the transmission lines p...As the transmission line corridors become more and more rare in China,it is now inevitable for people to construct HVAC-HVDC hybrid transmission lines.The research on the electric field around the transmission lines plays an important role in evaluating the electromagnetic environment nearby.However,few existing research now considered the mutual effect of HVAC-HVDC hybrid transmission lines.Thus,this research designed a program based on windows,which calculated the surface voltage gradient on the transmission lines and the electric field at ground level respectively.This research calculated the surface voltage gradient on the transmission lines by applying the improved method of successive images.For the electric field at ground level under AC transmission line,simulation charge method is used,while for the electric field at the ground level under DC transmission lines,deutsch assumption method is used.Comparing the results generated by the calculation with those in published literature,the program is reliable.Taking 500 kV transmission lines as an example,when considering the mutual effect of the HVAC-HVDC lines,the amplitude of the surface voltage gradient will increase by about 10%and the amplitude of the electric field at ground level will increase by about 8%,making the mutual effect of the AC and DC lines unneglectable. Larger part of the electric field at ground level under hybrid lines is produced by the DC line.Thus,in order to control the electric field at ground level under hybrid lines,it should pay more attention on that produced by the DC line.展开更多
The method of isotope dilution thermal ionization mass spectrometry able to trace to SI was developed to accurately measure trace amount of cadmium in the rice powder sample from CCQM-K24 international key comparison ...The method of isotope dilution thermal ionization mass spectrometry able to trace to SI was developed to accurately measure trace amount of cadmium in the rice powder sample from CCQM-K24 international key comparison organized by CCQM(Comité Consultatif pour la Quantité de Matière, Paris). By comparison with our previous work, there was much improvement in aspects of digestion of the rice powder sample, separation of cadmium from the sample and dry-mass correction. As a result, the blank of this procedure was reduced and the measurement precisions of isotopic ratios of cadmium were increased. In addition, the uncertainty evaluation of the entire process of measurement was profoundly studied. The analytical result of this work (14.53±0.15) nmol/g was in agreement with the certified value.展开更多
Positive electrospray ionization tandem mass spectrometry was applied to study four newly synthesized(12-aminodehydroabietylamine)acetamide-substituted salicylidene Schiff bases(ADASSSB).The results showed that the MS...Positive electrospray ionization tandem mass spectrometry was applied to study four newly synthesized(12-aminodehydroabietylamine)acetamide-substituted salicylidene Schiff bases(ADASSSB).The results showed that the MSn characteristics of ADASSSB can be used for their qualitative and quantitative analysis.展开更多
建立了一种可用于水产品及食用油中氟乐灵残留量分析的分散型固相萃取-气相色谱-负化学离子源质谱方法。水产品及食用油经乙腈提取，4℃冷藏后，采用分散型固相萃取法净化，由气相色谱-负化学离子源质谱选择离子监测技术进行测定与确证...建立了一种可用于水产品及食用油中氟乐灵残留量分析的分散型固相萃取-气相色谱-负化学离子源质谱方法。水产品及食用油经乙腈提取，4℃冷藏后，采用分散型固相萃取法净化，由气相色谱-负化学离子源质谱选择离子监测技术进行测定与确证，同位素内标法定量。在1～40μg / L 范围内氟乐灵农药的线性关系良好；方法定量限（LOQ）为0.02μg / kg；对鳗鱼、烤鳗、梭子蟹、小龙虾、猪油和橄榄油等6种复杂基质进行1.0、2.0和3.0μg / kg 等3个水平的添加回收试验，平均回收率均处于80％～100％之间，RSD≤10.3％；无干扰现象出现。该方法可作为水产品及食用油中氟乐灵残留检测的确证方法。展开更多
A simple, sensitive and reproducible high performance liquid chromatography-mass spectrometry coupled with electrospray ionization method for simultaneous separation and determination of adenine, adenosine and （urid...A simple, sensitive and reproducible high performance liquid chromatography-mass spectrometry coupled with electrospray ionization method for simultaneous separation and determination of adenine, adenosine and （uridine） was developed. The analytical column is a 2.0 mm×150 mm Shimadzu VP-ODS column and volume fraction of the mobile phase is （86.5%）water, 12.0%methanol and 1.5%formic acid. 2-chloroadenosine was used as internal standard. Selective ion monitoring mode and selective ion monitoring ions at ratio of mass to electric charge of 136 for adenine, 268 for adenosine and 267 for uridine were chosen for quantitative analysis of the three active components. The results show that the regression equations and linear range are Y=0.062X+（0.005） and 2.0140.0 (μg·mL-1)for adenine, Y=0.049X+0.004 and 4.0115.0 μg·mL-1 for uridine, （Y=0.154X）+0.014 and （1.0125.0） μg·mL-1 for adenosine. The limits of detection are 0.6 μg·mL-1 for adenine, 1.0 μg·mL-1for uridine and (0.2 μg·mL-1) for adenosine. The recoveries of the three constituents are from 96.6% to 103.2%.展开更多
A simple, reliable and rapid isocratic liquid chromatography(LC)-mass spectrometric detection(MS) coupled with electrospray ionization(ESI) method for simultaneous separation and determination of calycosin-7-O-β-D-gl...A simple, reliable and rapid isocratic liquid chromatography(LC)-mass spectrometric detection(MS) coupled with electrospray ionization(ESI) method for simultaneous separation and determination of calycosin-7-O-β-D-glucoside, ononin, calycosin and formonometin in Astragali Radix was developed. After the samples were extracted with ethanol, the optimum separation conditions for these analytes were achieved using water and acetonitrile(70:30, v/v) containing 0.2%(v/v) acetic acid as a mobile phase and a 2.0 mm×150 mm Hypersil-Keystone C18 column. Selective ion monitoring(SIM) mode and [M+H]+ ions at m/z 447, 431, 285 and 269 were used for quantitative analysis of four main active components above mentioned. The calibration curves were linear in the range of 0.4-175.0 μg/mL for calycosin-7-O-β-D-glucoside, 0.2-146.0 μg/m L for ononin, 0.4-210.0 μg/mL for calycosin and 0.5-217.0 μg/mL for formonetion, respectively. The limits of quantification(LOQ) and detection(LOD) were 0.4 μg/mL and 0.08 μg/m L for calycosin-7-O-β-D-glucoside, 0.2 μg/mL and 0.06 μg/m L for ononin, 0.4 μg/mL and 0.1 μg/mL for calycosin, 0.5 μg/m L and 0.1 μg/m L formonetion, respectively. The standard recoveries were in the range of 96.5%-104.7%. The developed method has successfully been used for the determination of four main flavonoids in Astragali Radix from various sources and can be used for identification, differentiation and quality evaluation of Astragali Radix.展开更多
基金supported by the National Natural Science Foundation of China(No.11802039,No.51605046)the Jiangsu Natural Science Foundation of China(No.BK20160406)。
文摘An experimental platform of a pulse detonation engine(PDE) was established to study the effect of different K_2 CO_3 ionized seed mass contents on the detonation process.The pressure and ion concentration were detected in the detonation process of the PDE with different contents of ionized seeds.The initiation process of the PDE at different ignition frequencies was studied.The results show that the gas conductivity in the detonation process increased by adding ionized seeds to the PDE tube,and the conductivity increased with the increase in ionized seed mass content.With the increase in ionized seed mass content,the range of the conductivity decreased.The PDE was successfully ignited and formed a stable detonation wave at ignition frequencies of 5 Hz and 10 Hz,and the peak pressure of the stable detonation with the ignition frequency of 5 Hz was 17% higher than that with an ignition frequency of 10 Hz.The detonation wave intensity was weake ned and dege nerated to a shock wave that propagated in the tube without the fuel filled at the ignition frequency of 20 Hz.
文摘The reverse magnetohydrodynamic(MHD)energy bypass technology is a promising energy redis⁃tribution technology in the scramjet system,in augmented with a power generation equipment to supply the neces⁃sary long-distance flight airframe power.In this paper,a computational model of the scramjet magnetohydrody⁃namic channel is developed and verified by using the commercial software Fluent.It is found that when the mag⁃netic induction intensity is 1,2,3,4 T,the power generation efficiency is 22.5%,22.3%,22.0%,21.5%,and decreases with the increase of the magnetic induction intensity,and the enthalpy extraction rate is 0.026%,0.1%,0.21%,0.34%,and increases with the increase of the magnetic induction intensity.The deceleration ef⁃fect of electromagnetic action on the airflow in the power channel increases with the increase of magnetic induc⁃tion intensity.The stronger the magnetic field intensity,the more obvious the decreasing effect of fluid Mach num⁃ber in the channel.The power generation efficiency decreases as the magnetic induction intensity increases and the enthalpy extraction rate is reversed.As the local currents gathering at inlet and outlet of the power generation area,total temperature and enthalpy along the flow direction do not vary linearly,and there are maximum and minimum values at inlet and outlet.Increasing the number of electrodes can effectively regulate the percentage of Joule heat dissipation,which can improve the power generation efficiency.
基金financial support from the National Natural Science Foundation of China(Grant No.21801016)the Science and Technology on Applied Physical Chemistry Laboratory(Grant No.6142602220304)。
文摘In order to achieve a wider range of ionizing radiations detection,novel fluorescence sensing materials have been developed that utilize the fluorescence enhancement phenomenon caused by the intramolecular photoinduced electron transfer(PET)effect.Two perylene diimide isomers PDI-P and PDI-B were designed and synthesized,and their molecular structures were characterized by high-resolution Fourier transform mass spectrometry(HRMS),nuclear magnetic resonance hydrogen and carbon spectroscopy(~1H and~(13)C NMR).The interaction between ionizing radiation and fluorescent molecules was simulated by HCl titration.The results show that combining PDIs and HCl can improve fluorescence through the retro-PET process.Despite the similarities in chemical structures,the fluorescent enhancement multiple of PDI-B with aromatic amine as electron donor is much higher than that of PDI-P with alkyl amine.In the direct irradiation experiments of ionizing radiation,the emission enhancement multiples of PDI-P and PDI-B are 2.01 and 45.4,respectively.Furthermore,density functional theory(DFT)and time-dependent density functional theory(TDDFT)calculations indicate that the HOMO and HOMO-1 energy ranges of PDI-P and PDI-B are 0.54 e V and 1.13 e V,respectively.A wider energy range has a stronger driving force on electrons,which is conducive to fluorescence quenching.Both femtosecond transient absorption spectroscopy(fs-TAS)and transient fluorescence spectroscopy(TFS)tests show that PDI-B has shorter charge separation lifetime and higher electron transfer rate constant.Although both isomers can significantly reduce LOD during PET process,PDI-B with aromatic amine has a wider detection range of 0.118—240 Gy due to its larger emission enhancement,which is a leap of three orders of magnitude.It breaks through the detection range of gamma radiation reported in existing studies,and provides theoretical support for the further study of sensitive and effective new materials for ionizing radiation detection.
文摘A GC-NCI-MS method was developed for the determination of chlorfenapyr residues in eggplant and soil sample.The sample was extracted by the mixture solvent of acetone-dichloromethane(4 ∶3,by volume),and cleaned up by chromatographic column of aluminum oxide-graphitized carbon black.The analysis of extract was performed by gas chromatography-negative chemical ionization-mass spectrometry(GC-NCI-MS).The recoveries of chlorfenapyr at the spiked concentration levels of 0.1,1.0,10.0 mg/kg were 100%-116% for eggplant sample with RSD of 2.0%-6.2%,and 83%-116% for the soil sample with RSD of 1.1%-4.5%,respectively.
文摘A direct determination method for the atrazine residue on the vegetable was developed by using desorption electrospray ionization mass spectrometry (DESI MS) without any sample pretreatment.Acetonitrile-water (1:1,v/v),which contained 0.1% formic acid,was used as the spray solvent.The working conditions,such as ESI gas inlet pressure,ESI flow rate,ESI spray voltage,spray-to-sample distance,spray-to-cone-hole distance and the collision induced dissociation (CID) voltage for MS/MS,were optimized for both DESI and esquires 6 000 mass spectrometer.The linear range of atrazine on cabbage leaves was 25.25-2 525 pg/mm2,the R2 was 0.991 6,and the relative standard deviations were between 3.37% and 26.17%.The LOD of atrazine calculated by S/N=3 was 2.50 pg/mm2.
文摘Technique of lutetium isotopic analysis by laser resonance ionization mass spectrometry(LRIMS) was developed in the presence of isobaric interference. In the case of real sample, the elemental selectivity was better than 8×105, and the detection efficiency was 8.3×10-5. The technique of wavelength scanning method was set up in order that the accurate isotopic ratio could be determined. And the numerical computational method was provided to calculate the correct factor of isotopic ratio. Using this technique, the isotopic ratio measured by LRIMS is in good agreement with standard value measured by TIMS.
文摘Puerarin,an isoflavone compound,is the bioactive component of traditional Chinese medicine.A novel dialkyl puerarin-7-yl phosphate was synthesized and investigated by positive ion electrospray ionization ion trap mass spectrometry (ESI MS)in conjunction with tandem mass spectrometry.The fragmentation pathways of dialkyl puerarin-7-yl phosphates were investigated.
文摘采用气相色谱-氢火焰离子化检测器法(gas chromatography with hydrogen flame ionization detection,GCFID)、顶空固相微萃取-气相色谱-质谱(headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry,HS-SPME-GC-MS)和电子鼻技术分析6种果酒中的挥发性成分,评价果酒风味轮廓特征的差异性。结果表明,GC-FID定量测定樱桃李酒,其中异戊醇、活性戊醇、β-苯乙醇含量最高,乙酸乙酯含量最低;木瓜酒中正丙醇、2,3-丁二醇、癸酸乙酯、乙酸含量最高; 3-羟基-2-丁酮含量在樱桃李酒中最高,山楂酒、甜橙酒中最少。HP-SPME-GC-MS鉴定果酒中挥发性物质94种,其中醇类23种,酯类43种,醛酮类10种,酸类8种,酚类2种,苯环类5种,烷烃类3种。山楂酒、菠萝酒、木瓜酒、甜橙酒、无花果酒和樱桃李酒中香气物质数量分别为34、44、45、45、33、47种。其中山楂酒、木瓜酒和无花果酒中未检出酚类、烷烃类物质。电子鼻对不同果酒香气的区分效果无重叠,W5S传感器区分果酒香气能力最强。比较而言,菠萝酒和樱桃李酒的口感更圆润,香气更愉悦,感官得分最高。
文摘As the transmission line corridors become more and more rare in China,it is now inevitable for people to construct HVAC-HVDC hybrid transmission lines.The research on the electric field around the transmission lines plays an important role in evaluating the electromagnetic environment nearby.However,few existing research now considered the mutual effect of HVAC-HVDC hybrid transmission lines.Thus,this research designed a program based on windows,which calculated the surface voltage gradient on the transmission lines and the electric field at ground level respectively.This research calculated the surface voltage gradient on the transmission lines by applying the improved method of successive images.For the electric field at ground level under AC transmission line,simulation charge method is used,while for the electric field at the ground level under DC transmission lines,deutsch assumption method is used.Comparing the results generated by the calculation with those in published literature,the program is reliable.Taking 500 kV transmission lines as an example,when considering the mutual effect of the HVAC-HVDC lines,the amplitude of the surface voltage gradient will increase by about 10%and the amplitude of the electric field at ground level will increase by about 8%,making the mutual effect of the AC and DC lines unneglectable. Larger part of the electric field at ground level under hybrid lines is produced by the DC line.Thus,in order to control the electric field at ground level under hybrid lines,it should pay more attention on that produced by the DC line.
文摘The method of isotope dilution thermal ionization mass spectrometry able to trace to SI was developed to accurately measure trace amount of cadmium in the rice powder sample from CCQM-K24 international key comparison organized by CCQM(Comité Consultatif pour la Quantité de Matière, Paris). By comparison with our previous work, there was much improvement in aspects of digestion of the rice powder sample, separation of cadmium from the sample and dry-mass correction. As a result, the blank of this procedure was reduced and the measurement precisions of isotopic ratios of cadmium were increased. In addition, the uncertainty evaluation of the entire process of measurement was profoundly studied. The analytical result of this work (14.53±0.15) nmol/g was in agreement with the certified value.
文摘Positive electrospray ionization tandem mass spectrometry was applied to study four newly synthesized(12-aminodehydroabietylamine)acetamide-substituted salicylidene Schiff bases(ADASSSB).The results showed that the MSn characteristics of ADASSSB can be used for their qualitative and quantitative analysis.
文摘建立了一种可用于水产品及食用油中氟乐灵残留量分析的分散型固相萃取-气相色谱-负化学离子源质谱方法。水产品及食用油经乙腈提取，4℃冷藏后，采用分散型固相萃取法净化，由气相色谱-负化学离子源质谱选择离子监测技术进行测定与确证，同位素内标法定量。在1～40μg / L 范围内氟乐灵农药的线性关系良好；方法定量限（LOQ）为0.02μg / kg；对鳗鱼、烤鳗、梭子蟹、小龙虾、猪油和橄榄油等6种复杂基质进行1.0、2.0和3.0μg / kg 等3个水平的添加回收试验，平均回收率均处于80％～100％之间，RSD≤10.3％；无干扰现象出现。该方法可作为水产品及食用油中氟乐灵残留检测的确证方法。
文摘A simple, sensitive and reproducible high performance liquid chromatography-mass spectrometry coupled with electrospray ionization method for simultaneous separation and determination of adenine, adenosine and （uridine） was developed. The analytical column is a 2.0 mm×150 mm Shimadzu VP-ODS column and volume fraction of the mobile phase is （86.5%）water, 12.0%methanol and 1.5%formic acid. 2-chloroadenosine was used as internal standard. Selective ion monitoring mode and selective ion monitoring ions at ratio of mass to electric charge of 136 for adenine, 268 for adenosine and 267 for uridine were chosen for quantitative analysis of the three active components. The results show that the regression equations and linear range are Y=0.062X+（0.005） and 2.0140.0 (μg·mL-1)for adenine, Y=0.049X+0.004 and 4.0115.0 μg·mL-1 for uridine, （Y=0.154X）+0.014 and （1.0125.0） μg·mL-1 for adenosine. The limits of detection are 0.6 μg·mL-1 for adenine, 1.0 μg·mL-1for uridine and (0.2 μg·mL-1) for adenosine. The recoveries of the three constituents are from 96.6% to 103.2%.
基金Project(21472110)supported by the National Natural Science Foundation of ChinaProject(LY15B050008)supported by the Natural Science Foundation of Zhejiang Province,ChinaProject(2013Y003)supported by Quzhou Technology Projects,China
文摘A simple, reliable and rapid isocratic liquid chromatography(LC)-mass spectrometric detection(MS) coupled with electrospray ionization(ESI) method for simultaneous separation and determination of calycosin-7-O-β-D-glucoside, ononin, calycosin and formonometin in Astragali Radix was developed. After the samples were extracted with ethanol, the optimum separation conditions for these analytes were achieved using water and acetonitrile(70:30, v/v) containing 0.2%(v/v) acetic acid as a mobile phase and a 2.0 mm×150 mm Hypersil-Keystone C18 column. Selective ion monitoring(SIM) mode and [M+H]+ ions at m/z 447, 431, 285 and 269 were used for quantitative analysis of four main active components above mentioned. The calibration curves were linear in the range of 0.4-175.0 μg/mL for calycosin-7-O-β-D-glucoside, 0.2-146.0 μg/m L for ononin, 0.4-210.0 μg/mL for calycosin and 0.5-217.0 μg/mL for formonetion, respectively. The limits of quantification(LOQ) and detection(LOD) were 0.4 μg/mL and 0.08 μg/m L for calycosin-7-O-β-D-glucoside, 0.2 μg/mL and 0.06 μg/m L for ononin, 0.4 μg/mL and 0.1 μg/mL for calycosin, 0.5 μg/m L and 0.1 μg/m L formonetion, respectively. The standard recoveries were in the range of 96.5%-104.7%. The developed method has successfully been used for the determination of four main flavonoids in Astragali Radix from various sources and can be used for identification, differentiation and quality evaluation of Astragali Radix.
