A convenient,cost-effective and fast method using dynamic microwave-assisted extraction and liquid phase microextraction based on the solidification of a floating drop was proposed to analyze organochlorine pesticides...A convenient,cost-effective and fast method using dynamic microwave-assisted extraction and liquid phase microextraction based on the solidification of a floating drop was proposed to analyze organochlorine pesticides in grains including rice,maize and millet.Twelve samples can be processed simultaneously in the method.During the extraction process,10%acetonitrile-water solutions containing 110μL of n-hexadecane were used to extract organochlorine pesticides.Subsequently,1.0 g sodium chloride was placed in the extract,and then centrifuged and cooled.The n-hexadecane drops containing the analytes were solidifi ed and transferred for determination by gas chromatography-electron capture detector without any further filtration or cleaning process.Limits of detection for organochlorine pesticides were 0.97–1.01μg/kg and the RSDs were in the range of 2.6%–8.5%.The developed technology has succeeded in analyzing six real grains samples and the recoveries of the organochlorine pesticides were 72.2%–94.3%.Compared with the published extraction methods,the developed method was used to analyze organochlorine pesticides in grains,being more environmentally friendly,which is suitable for the daily determination of organochlorine pesticides.展开更多
The aim of this work was to develop an automated on-line solid phase extraction(SPE)with liquid chromatography-tandem mass spectrometry method for the detection of fifteen sulfonamides in pork and fish samples.Samples...The aim of this work was to develop an automated on-line solid phase extraction(SPE)with liquid chromatography-tandem mass spectrometry method for the detection of fifteen sulfonamides in pork and fish samples.Samples were extracted with 0.2%formic acid acetonitrile solution,purified by on-line SPE device with HLB column,then separated by XBridge C18 column,using 0.1%formic acid solution and acetonitrile as the mobile phase.Mass spectrometric data was acquired under multiple reaction monitoring(MRM)mode using positive ionization electrospray.Internal standard method was used in the quantification,good linear relationship was got in range of 0.1–100 ng/mL and correlation coefficient was higher than 0.9990.The limits of detection were in the range of 0.125–2.00g/kg and the limits of quantitation were in the range of 0.250–5.00g/kg.Recoveries of the method were in range of 78.3%–99.3%,relative standard deviation were lower than 10%.The method was simple,sensitivity,and could be used for routine supervision and analysis of fifteen sulfonamides in pork and fish.展开更多
The analysis of the coupling mechanism of thermal-hydraulic-mechanical(THM)fields,and solid-liquidgas(SLG)phases during gas extraction process is of profound significance to explore its numerical application in the ga...The analysis of the coupling mechanism of thermal-hydraulic-mechanical(THM)fields,and solid-liquidgas(SLG)phases during gas extraction process is of profound significance to explore its numerical application in the gas occurrence regularity and its effective extraction radius.In this study,the Hudi coal mine in Qinshui basin is taken as the research area,the influencing factors of gas occurrence were analyzed,the differences in overburden load for gas pressure distribution and the factors influencing the effective extraction radius were further discussed by using the COMSOL software.The results show that the derivation of mathematical model in gas extraction shows that the process is a process the THM fields restrict each other,and the SLG phases influence each other.The longer the extraction time,the larger the influencing range of borehole,and the better the extraction effect.The larger the diameter of borehole,the larger the effective extraction radius,and the influence on gas extraction effect is smaller in the early stage and larger in the late stage.The borehole arrangement should be flexibly arranged according to the actual extraction situation.The higher the porosity,the higher the permeability,the better the gas extraction effect.The larger the overburden load of reservoir,the stronger the effective stress,which will result in the more severe the strain,and the closure of pore and fracture,which in turn will lead to the decrease of permeability and slow down the gas extraction.The relationship among extraction time,borehole diameter,negative pressure of gas extraction,permeability with effective extraction radius is exponential.This study has important theoretical and practical significance for clarifying and summarizing the gas occurrence regularity and its engineering practice.展开更多
Generally, the phase of the cold-atom interferometer is extracted from the atomic interference fringe, which can be obtained by scanning the chirp rate of the Raman lasers at a given interrogation time T. If mapping t...Generally, the phase of the cold-atom interferometer is extracted from the atomic interference fringe, which can be obtained by scanning the chirp rate of the Raman lasers at a given interrogation time T. If mapping the phase shift for each T with a series of measurements, the extraction time is limited by the protocol of each T measurement, and therefore increases dramatically when doing fine mapping with a small step of T. Here we present a new method for rapid extraction of the phase shift via phase demodulation. By using this method, the systematic shifts can be mapped though the whole interference area. This method enables quick diagnostics of the potential cause of the phase shift in specific time. We demonstrate experimentally that this method is effective for the evaluation of the systematic errors of the cold atomic gravimeter. The systematic phase error induced by the quadratic Zeeman effect in the free-falling region is extracted by this method. The measured results correspond well with the theoretic prediction and also agree with the results obtained by the fringe fitting method for each T.展开更多
The identification features of composite pseudocode phase modulation and carry frequency modulation signal include pseudocode and modulation frequency. In this paper,PWD is used to extract these features. First,the fe...The identification features of composite pseudocode phase modulation and carry frequency modulation signal include pseudocode and modulation frequency. In this paper,PWD is used to extract these features. First,the feature of pseudocode is extracted using the amplitude output of PWD and the correlation filter technology. Then the feature of frequency modulation is extracted by way of PWD analysis on the signal processed by anti-phase operation according to the extracted feature of pseudo code,i.e. position information of changed abruptly point of phase. The simulation result shows that both the features of frequency modulation and phase change position caused by the pseudocode phase modulation can be extracted effectively for SNR=3 dB.展开更多
A phase-derived velocity measurement method is proposed in a wideband coherent system,based on a precise echo model considering the inner pulse Doppler effect caused by fast moving targets.The Cramer-Rao low band of v...A phase-derived velocity measurement method is proposed in a wideband coherent system,based on a precise echo model considering the inner pulse Doppler effect caused by fast moving targets.The Cramer-Rao low band of velocity measurement precision is deduced,demonstrating the high precision of the proposed method.Simulations and out-field experiments further validate the effectiveness of the proposed method in high-precision measurement and micro-motion extraction for targets with weak reflection intensity.Compared with the long-time integration approaches for velocity measurement,the phase-derived method is easy to implement and meets the requirement for high data rate,which makes it suitable for micro-motion feature extraction in wideband systems.展开更多
The pore structure and oil content of shales have an important influence on the oil mobility and enrichment.In this study,the lacustrine shale samples from the Qingshankou Formation(Q1)of Songliao Basin were selected....The pore structure and oil content of shales have an important influence on the oil mobility and enrichment.In this study,the lacustrine shale samples from the Qingshankou Formation(Q1)of Songliao Basin were selected.TOC,pyrolysis,XRD and nitrogen adsorption were performed on the original and extracted shale samples.Then the influence of mineral composition and organic matter(OM)on the development of nano-scale pore,the oil phase states and mobility were analyzed.The Q1 shale samples can be sub-divided into three types according to the isotherm characteristics.Type A samples are characterized by high kerogen content,with oil mainly existing in the free phase state.Type B samples are characterized by medium kerogen content,oil mainly exists in the absorbed phase state.Type C samples are characterized by low kerogen content,with trace oil found in the absorbed phase state.Nano-scale organic pores are well developed in the Q1 Formation.Oil is primarily found in the pore spaces with diameters less than 10 nm,this being the pore size threshold for mobile shale oil.When TOC>2.0 wt%and EOM>1.0 wt%,Q1 Formation shale oil mobility is high,resulting in prospective drilling targets.展开更多
A highly sensitive SPE-liquid/liquid extraction RPLC method has been developed for the analysis of 6β-hydroxycortisol and cortisol in the urine of cancer patients. Methods： After SPE column purification and liquid-l...A highly sensitive SPE-liquid/liquid extraction RPLC method has been developed for the analysis of 6β-hydroxycortisol and cortisol in the urine of cancer patients. Methods： After SPE column purification and liquid-liquid extraction, the sample test solutions were analyzed with RPLC using a C18 analytical column. This improved analytical method has been validated for linearity, accuracy （recovery from urine）, repeatability （within-day and between-day precision）, specificity, sensitivity, and stability. This SPE-liquid/liquid extraction-RPLC is rapid, simple, accurate and reproducible. The technique is particularly useful for monitoring the CYP3A activity of cancer patients in clinical settings. The results are expressed as the ratio of 6β-hydroxycortisol to cortisol. Results： The CYP3A activity from a total of 153 samples was measured using this improved method. Considerable variation in the CYP3A activity of different cancer patients has been documented. Thus, personalized medical treatment based on the individual metabolic enzyme activity level is necessary. Conclusion： This new analytical method facilitates such individualized medical treatments.展开更多
With the vigorous development of national infrastructure construction and public information construction,video surveillance systems have gradually penetrated various fields.The current key frame extraction technology...With the vigorous development of national infrastructure construction and public information construction,video surveillance systems have gradually penetrated various fields.The current key frame extraction technology has inadequate target details and inaccurate judgment of local actions.Addressing this problem,a key frame extraction method based on fractional Fourier transform is proposed.This method obtained the phase spectra information of different orders by performing fractional Fourier transform on the surveillance video frames.Next,the method designed an adaptive algorithm based on the golden section point to select the transformation order.Then,the phase spectrum information of two adjacent frames was used to characterize the changes in the global and local motion states of the target.The final step was to extract key frames based on this.Experimental results show that,compared with the previous methods,the key frames extracted by the method proposed in this paper can correctly capture the changes in the global and local motion states of the target.展开更多
The mass transfer between heavy oil and liquid carbon dioxide and the changes of the heavy phase(mixture of heavy oil and CO_2) and light phase(pure CO_2) in the mixture were tested in lab with heavy oil samples from ...The mass transfer between heavy oil and liquid carbon dioxide and the changes of the heavy phase(mixture of heavy oil and CO_2) and light phase(pure CO_2) in the mixture were tested in lab with heavy oil samples from Russia. The experimental results showed that the heavy oil hardly expanded when the concentration of carbon dioxide in the mixture was 10%. When the concentration of carbon dioxide was higher than 26%, the volume of the heavy phase decreased, and the viscosity of the heavy phase increased exponentially as the light components extracted from the heavy oil exceeded the carbon dioxide saturated in the heavy oil. When the concentration of carbon dioxide in the mixture was 26%, the effect of viscosity reducing to the heavy phase was the strongest. The density of the light and heavy phases, volume factor, and solubility of gas and flash viscosity of heavy phase all increased with the rise of carbon dioxide concentration in the mixture. The best concentration of carbon dioxide in the mixture was 26%, when the heavy oil expanded the most and the viscosity of the heavy phase was the lowest. When the concentration of carbon dioxide in the mixture was between 10% and 26%, the volume of the light phase was the smallest and the oil displacement effect was the best.展开更多
建立了液相色谱-串联质谱(LC-MS/MS)手性拆分和测定水产品中奥沙西泮和替马西泮对映体残留量的分析方法。样品经乙腈提取2次,40℃条件下氮气浓缩至近干,残渣加入2 mL 50%乙腈-水溶液溶解,采用分散固相萃取净化,LC-MS/MS测定。使用Enanti...建立了液相色谱-串联质谱(LC-MS/MS)手性拆分和测定水产品中奥沙西泮和替马西泮对映体残留量的分析方法。样品经乙腈提取2次,40℃条件下氮气浓缩至近干,残渣加入2 mL 50%乙腈-水溶液溶解,采用分散固相萃取净化,LC-MS/MS测定。使用EnantioPAK■Y1-R(5μm,150 mm×4.6 mm)手性色谱柱,乙腈和0.1%甲酸-5 mmol/L乙酸铵溶液作为流动相,采用等度洗脱方式实现奥沙西泮和替马西泮手性对映体的拆分。目标对映体采用电喷雾正离子(ESI^(+))模式电离,多反应监测(MRM)模式下,内标法测定。目标对映体在0.5~50μg/L质量浓度范围内线性关系良好,相关系数(r^(2))均不低于0.9990。水产品中对映体的检出限和定量下限分别为0.2μg/kg和0.5μg/kg。在5种空白基质中添加低、中、高浓度水平的目标对映体,样品平均加标回收率为82.6%~107%,相对标准偏差(RSD,n=6)为1.6%~9.2%。该方法灵敏可靠、适用性强,可用于不同水产品中奥沙西泮和替马西泮对映体的分析。展开更多
基金The study was financially supported by the National Science and Technology Support Program of China(Grant No.2013BAD16B08).
文摘A convenient,cost-effective and fast method using dynamic microwave-assisted extraction and liquid phase microextraction based on the solidification of a floating drop was proposed to analyze organochlorine pesticides in grains including rice,maize and millet.Twelve samples can be processed simultaneously in the method.During the extraction process,10%acetonitrile-water solutions containing 110μL of n-hexadecane were used to extract organochlorine pesticides.Subsequently,1.0 g sodium chloride was placed in the extract,and then centrifuged and cooled.The n-hexadecane drops containing the analytes were solidifi ed and transferred for determination by gas chromatography-electron capture detector without any further filtration or cleaning process.Limits of detection for organochlorine pesticides were 0.97–1.01μg/kg and the RSDs were in the range of 2.6%–8.5%.The developed technology has succeeded in analyzing six real grains samples and the recoveries of the organochlorine pesticides were 72.2%–94.3%.Compared with the published extraction methods,the developed method was used to analyze organochlorine pesticides in grains,being more environmentally friendly,which is suitable for the daily determination of organochlorine pesticides.
基金This work was supported by“National Key Research and Development Program of China”(Project No.2018YFC1603400)Science and Technology Program of Hebei Province(Project No.19225503D).
文摘The aim of this work was to develop an automated on-line solid phase extraction(SPE)with liquid chromatography-tandem mass spectrometry method for the detection of fifteen sulfonamides in pork and fish samples.Samples were extracted with 0.2%formic acid acetonitrile solution,purified by on-line SPE device with HLB column,then separated by XBridge C18 column,using 0.1%formic acid solution and acetonitrile as the mobile phase.Mass spectrometric data was acquired under multiple reaction monitoring(MRM)mode using positive ionization electrospray.Internal standard method was used in the quantification,good linear relationship was got in range of 0.1–100 ng/mL and correlation coefficient was higher than 0.9990.The limits of detection were in the range of 0.125–2.00g/kg and the limits of quantitation were in the range of 0.250–5.00g/kg.Recoveries of the method were in range of 78.3%–99.3%,relative standard deviation were lower than 10%.The method was simple,sensitivity,and could be used for routine supervision and analysis of fifteen sulfonamides in pork and fish.
基金financially supported by the University Synergy Innovation Program of Anhui Province(No.GXXT-2021-018)the National Natural Science Foundation of China(No.42102217)+3 种基金the Natural Science Research Project of Anhui University(Nos.KJ2020A0315,KJ2020A0317)the Institute of Energy,Hefei Comprehensive National Science Center(No.21KZS218)the Natural Science Foundation of Anhui Province(No.2108085MD134)the Foundation of State Key Laboratory of Petroleum Resources and Prospecting,China University of Petroleum,Beijing(No.PRP/open-2005)
文摘The analysis of the coupling mechanism of thermal-hydraulic-mechanical(THM)fields,and solid-liquidgas(SLG)phases during gas extraction process is of profound significance to explore its numerical application in the gas occurrence regularity and its effective extraction radius.In this study,the Hudi coal mine in Qinshui basin is taken as the research area,the influencing factors of gas occurrence were analyzed,the differences in overburden load for gas pressure distribution and the factors influencing the effective extraction radius were further discussed by using the COMSOL software.The results show that the derivation of mathematical model in gas extraction shows that the process is a process the THM fields restrict each other,and the SLG phases influence each other.The longer the extraction time,the larger the influencing range of borehole,and the better the extraction effect.The larger the diameter of borehole,the larger the effective extraction radius,and the influence on gas extraction effect is smaller in the early stage and larger in the late stage.The borehole arrangement should be flexibly arranged according to the actual extraction situation.The higher the porosity,the higher the permeability,the better the gas extraction effect.The larger the overburden load of reservoir,the stronger the effective stress,which will result in the more severe the strain,and the closure of pore and fracture,which in turn will lead to the decrease of permeability and slow down the gas extraction.The relationship among extraction time,borehole diameter,negative pressure of gas extraction,permeability with effective extraction radius is exponential.This study has important theoretical and practical significance for clarifying and summarizing the gas occurrence regularity and its engineering practice.
基金supported by the National Natural Science Foundation of China(Grant Nos.11174249 and 61475139)the Ministry of Science and Technology of China(Grant No.2011AA060504)+1 种基金the National Basic Research Program of China(Grant No.2013CB329501)the Fundamental Research Funds for the Central Universities,China(Grant No.2015FZA3002)
文摘Generally, the phase of the cold-atom interferometer is extracted from the atomic interference fringe, which can be obtained by scanning the chirp rate of the Raman lasers at a given interrogation time T. If mapping the phase shift for each T with a series of measurements, the extraction time is limited by the protocol of each T measurement, and therefore increases dramatically when doing fine mapping with a small step of T. Here we present a new method for rapid extraction of the phase shift via phase demodulation. By using this method, the systematic shifts can be mapped though the whole interference area. This method enables quick diagnostics of the potential cause of the phase shift in specific time. We demonstrate experimentally that this method is effective for the evaluation of the systematic errors of the cold atomic gravimeter. The systematic phase error induced by the quadratic Zeeman effect in the free-falling region is extracted by this method. The measured results correspond well with the theoretic prediction and also agree with the results obtained by the fringe fitting method for each T.
文摘The identification features of composite pseudocode phase modulation and carry frequency modulation signal include pseudocode and modulation frequency. In this paper,PWD is used to extract these features. First,the feature of pseudocode is extracted using the amplitude output of PWD and the correlation filter technology. Then the feature of frequency modulation is extracted by way of PWD analysis on the signal processed by anti-phase operation according to the extracted feature of pseudo code,i.e. position information of changed abruptly point of phase. The simulation result shows that both the features of frequency modulation and phase change position caused by the pseudocode phase modulation can be extracted effectively for SNR=3 dB.
基金Supported by the National Natural Science Foundation of China(61301189)111 Project of China(B14010)
文摘A phase-derived velocity measurement method is proposed in a wideband coherent system,based on a precise echo model considering the inner pulse Doppler effect caused by fast moving targets.The Cramer-Rao low band of velocity measurement precision is deduced,demonstrating the high precision of the proposed method.Simulations and out-field experiments further validate the effectiveness of the proposed method in high-precision measurement and micro-motion extraction for targets with weak reflection intensity.Compared with the long-time integration approaches for velocity measurement,the phase-derived method is easy to implement and meets the requirement for high data rate,which makes it suitable for micro-motion feature extraction in wideband systems.
基金financially supported by the National Natural Science Foundation of China(No.41972156)the Science and Technology Project of Heilongjiang Province(No.2020ZX05A01)
文摘The pore structure and oil content of shales have an important influence on the oil mobility and enrichment.In this study,the lacustrine shale samples from the Qingshankou Formation(Q1)of Songliao Basin were selected.TOC,pyrolysis,XRD and nitrogen adsorption were performed on the original and extracted shale samples.Then the influence of mineral composition and organic matter(OM)on the development of nano-scale pore,the oil phase states and mobility were analyzed.The Q1 shale samples can be sub-divided into three types according to the isotherm characteristics.Type A samples are characterized by high kerogen content,with oil mainly existing in the free phase state.Type B samples are characterized by medium kerogen content,oil mainly exists in the absorbed phase state.Type C samples are characterized by low kerogen content,with trace oil found in the absorbed phase state.Nano-scale organic pores are well developed in the Q1 Formation.Oil is primarily found in the pore spaces with diameters less than 10 nm,this being the pore size threshold for mobile shale oil.When TOC>2.0 wt%and EOM>1.0 wt%,Q1 Formation shale oil mobility is high,resulting in prospective drilling targets.
基金supported by the Shanghai Pharmaceutical Association
文摘A highly sensitive SPE-liquid/liquid extraction RPLC method has been developed for the analysis of 6β-hydroxycortisol and cortisol in the urine of cancer patients. Methods： After SPE column purification and liquid-liquid extraction, the sample test solutions were analyzed with RPLC using a C18 analytical column. This improved analytical method has been validated for linearity, accuracy （recovery from urine）, repeatability （within-day and between-day precision）, specificity, sensitivity, and stability. This SPE-liquid/liquid extraction-RPLC is rapid, simple, accurate and reproducible. The technique is particularly useful for monitoring the CYP3A activity of cancer patients in clinical settings. The results are expressed as the ratio of 6β-hydroxycortisol to cortisol. Results： The CYP3A activity from a total of 153 samples was measured using this improved method. Considerable variation in the CYP3A activity of different cancer patients has been documented. Thus, personalized medical treatment based on the individual metabolic enzyme activity level is necessary. Conclusion： This new analytical method facilitates such individualized medical treatments.
基金supported by the National Natural Science Foundation of China(Nos.61702347,62027801 and 61972267)Natural Science Fund of Hebei Province(No.F2017210161),and Hebei Province Graduate Student Innovation Ability Training Funding Project.
文摘With the vigorous development of national infrastructure construction and public information construction,video surveillance systems have gradually penetrated various fields.The current key frame extraction technology has inadequate target details and inaccurate judgment of local actions.Addressing this problem,a key frame extraction method based on fractional Fourier transform is proposed.This method obtained the phase spectra information of different orders by performing fractional Fourier transform on the surveillance video frames.Next,the method designed an adaptive algorithm based on the golden section point to select the transformation order.Then,the phase spectrum information of two adjacent frames was used to characterize the changes in the global and local motion states of the target.The final step was to extract key frames based on this.Experimental results show that,compared with the previous methods,the key frames extracted by the method proposed in this paper can correctly capture the changes in the global and local motion states of the target.
文摘The mass transfer between heavy oil and liquid carbon dioxide and the changes of the heavy phase(mixture of heavy oil and CO_2) and light phase(pure CO_2) in the mixture were tested in lab with heavy oil samples from Russia. The experimental results showed that the heavy oil hardly expanded when the concentration of carbon dioxide in the mixture was 10%. When the concentration of carbon dioxide was higher than 26%, the volume of the heavy phase decreased, and the viscosity of the heavy phase increased exponentially as the light components extracted from the heavy oil exceeded the carbon dioxide saturated in the heavy oil. When the concentration of carbon dioxide in the mixture was 26%, the effect of viscosity reducing to the heavy phase was the strongest. The density of the light and heavy phases, volume factor, and solubility of gas and flash viscosity of heavy phase all increased with the rise of carbon dioxide concentration in the mixture. The best concentration of carbon dioxide in the mixture was 26%, when the heavy oil expanded the most and the viscosity of the heavy phase was the lowest. When the concentration of carbon dioxide in the mixture was between 10% and 26%, the volume of the light phase was the smallest and the oil displacement effect was the best.
