Chinese herbal compound is playing an important role on curing human diseases.And it has been a trend that Chinese herbal compound is being used all over the world in 21 century.However,our Chinese herbal compound is ...Chinese herbal compound is playing an important role on curing human diseases.And it has been a trend that Chinese herbal compound is being used all over the world in 21 century.However,our Chinese herbal compound is facing serious challenge for the lack of canonical system of quality criterion for Chinese herbal compound so it has been a urgent problem to set up the quality control standards and reveal therapeutic basis of Chinese herbal compound.In order to give full play to the advantages of Chinese herbal compound,modern scientific and technological is used to research of Chinese herbal compound,especially the high performance liquid chromatography tandem mass spectrometry(HPLC-MS),because it is high sensitive,rapid,and obtain more information.It is very necessary that HPLC-MS is uesed to elucidate the effective components of basic substances of Chinese Herbal Compound,and endow traditional Chinese medicine with modern scientific connotation.展开更多
建立高效液相色谱检测桦褐孔菌粗提物中原儿茶酸、原儿茶醛和紫萁酮3种化合物含量的方法,对比评价超声辅助提取法、回流提取法、微波辅助提取法、酶解提取法4种不同提取方法对桦褐孔菌粗提物中活性成分含量的影响。结果表明,该检测方法...建立高效液相色谱检测桦褐孔菌粗提物中原儿茶酸、原儿茶醛和紫萁酮3种化合物含量的方法,对比评价超声辅助提取法、回流提取法、微波辅助提取法、酶解提取法4种不同提取方法对桦褐孔菌粗提物中活性成分含量的影响。结果表明,该检测方法精密度较高,3种化合物的精密度的相对标准偏差(relative standard deviation,RSD)分别为0.14%、0.06%、0.20%;重复性RSD分别为1.67%、1.98%、2.22%;在24 h内稳定性较好,其RSD分别为0.20%、0.61%、0.25%。对比不同提取方法对3种化合物的影响,发现采用超声辅助提取法得到的目标化合物产量较高,适用于桦褐孔菌中主要活性成分的提取。该研究建立的HPLC法检测桦褐孔菌粗提物中原儿茶酸、原儿茶醛和紫萁酮含量的结果准确。展开更多
Lemon oils are broadly used as flavoring agents in beverages,foods,cosmetics and pharmaceuticals,yet the adulteration of natural,particularly cold pressed lemon oils is very common in the industry due to its unmet dem...Lemon oils are broadly used as flavoring agents in beverages,foods,cosmetics and pharmaceuticals,yet the adulteration of natural,particularly cold pressed lemon oils is very common in the industry due to its unmet demand and high cost.Nowadays,most quality control(QC)analysis of lemon oils is conducted by gas chromatography(GC)analysis,which is far from a reliable method.Oxygen heterocyclic compounds(OHCs)in non-volatile fraction are gaining increasing attention in authentication process because of the nearly finger-printing profiles of OHCs in cold pressed citrus essential oils.Our goal in this study was to identify OHCs using high performance liquid chromatography(HPLC)in lemon oils,establish OHC profiles,perform stepwise logistic regression analysis(SLRA)and build effective predicting model and further determine adulterated lemon oils by referencing the OHC profiles and established models.After HPLC analyses,profiling and SLRA modeling of 154 OHCs samples of industrial lemon oils,we found that the combination of isopimpinellin and total OHC concentration are essential and robust predictors to differentiate authentic samples from adulterated lemon oils with a success rate of 98%from the 5-fold cross validation.This study provided a reliable and efficient method in determining the authenticity of lemon oils.展开更多
In this experiment,a liquid chromatography tandem mass spectrometry method was built to determine 15 pesticide residues in Chinese cabbage and cucumber samples based on online turbulent flow chromatography purificatio...In this experiment,a liquid chromatography tandem mass spectrometry method was built to determine 15 pesticide residues in Chinese cabbage and cucumber samples based on online turbulent flow chromatography purification.After modified quick,easy,cheap,effective,rugged,and safe(QuEChERS)extraction,extracts were directly injected to the TLX(TurboFlow Liquid Xcalibur)system and brought to TurboFlow™columns for on-line purification and then transferred to analytical column for further separation and analysis.TurboFlow™columns types,transfer flow rate,and transfer time were optimized.Limits of detection and limits of quantification of the method obtained for 15 pesticide residues were ranged between 0.2–1.0μg/kg and 0.5–2.0μg/kg in Chinese cabbage and cucumber samples.Recoveries of pesticide residues were in range of 75.3%–103.7%.Matrix effects for 15 pesticides were in range of 5.6%–106.6%.The developed method has been successfully used for the determination of 15 pesticide residues in real samples.展开更多
The novel pulsed liquid chromatography radionuclide separation method presented here provides a new and promising strategy for the extraction of uranium from seawater.In this study,a new chromatographic separation met...The novel pulsed liquid chromatography radionuclide separation method presented here provides a new and promising strategy for the extraction of uranium from seawater.In this study,a new chromatographic separation method was proposed,and a pulsed nuclide automated separation device was developed,alongside a new chromatographic column.The length of this chromatographic column was 10 m,with an internal warp of 3 mm and a packing size of 1 mm,while the total separation units of the column reached 12,250.The most favorable conditions for the separation of nuclides were then obtained through optimizing the separation conditions of the device:Sample pH in the column=2,sample injection flow rate=5.698 mL/min,chromatographic column heating temperature=60℃.Separation experiments were also carried out for uranium,europium,and sodium ions in mixed solutions;uranium and sodium ions in water samples from the Ganjiang River;and uranium,sodium,and magnesium ions from seawater samples.The separation factors between the different nuclei were then calculated based on the experimental data,and a formula for the separation level was derived.The experimental results showed that the separation factor in the mixed solution of uranium and europium(1:1)was 1.088,while achieving the initial separation of uranium and europium theoretically required a 47-stage separation.Considering the separation factor of 1.50for the uranium and sodium ions in water samples from the Ganjiang River,achieving the initial separation of uranium and sodium ions would have theoretically required at least a 21-stage separation.Furthermore,for the seawater sample separation experiments,the separation factor of uranium and sodium ions was 1.2885;therefore,more than 28 stages of sample separation would be required to achieve uranium extraction from seawater.The novel pulsed liquid chromatography method proposed in this study was innovative in terms of uranium separation and enrichment,while expanding the possibilities of extracting uranium from seawater through chromatography.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
An isocratic reversed-phase liquid chromatographic (LC) method is described for the determination of epalrestat and its three stereoisomers (degradation impurities) in drug substance. The LC separation system consiste...An isocratic reversed-phase liquid chromatographic (LC) method is described for the determination of epalrestat and its three stereoisomers (degradation impurities) in drug substance. The LC separation system consisted of a Hypersil C18 column (250 mm×4.6 mm, 5 μm) with a mobile phase comprising methanol, acetonitrile and water (volume ratio 60∶1∶50, pH 4.5) delivered at a flow rate of 1.6 mL/min and UV detection at 280 nm. The proposed LC method is simple and selective for the determination of the stereoisomers of epalrestat in the drug substance with a limit of detection and quantification of 3.9 μg/mL and 4.9 μg/mL, respectively. The stereoisomers were identified by liquid chromatography-mass spectrometry (LC-MS).展开更多
文摘Chinese herbal compound is playing an important role on curing human diseases.And it has been a trend that Chinese herbal compound is being used all over the world in 21 century.However,our Chinese herbal compound is facing serious challenge for the lack of canonical system of quality criterion for Chinese herbal compound so it has been a urgent problem to set up the quality control standards and reveal therapeutic basis of Chinese herbal compound.In order to give full play to the advantages of Chinese herbal compound,modern scientific and technological is used to research of Chinese herbal compound,especially the high performance liquid chromatography tandem mass spectrometry(HPLC-MS),because it is high sensitive,rapid,and obtain more information.It is very necessary that HPLC-MS is uesed to elucidate the effective components of basic substances of Chinese Herbal Compound,and endow traditional Chinese medicine with modern scientific connotation.
文摘建立高效液相色谱检测桦褐孔菌粗提物中原儿茶酸、原儿茶醛和紫萁酮3种化合物含量的方法,对比评价超声辅助提取法、回流提取法、微波辅助提取法、酶解提取法4种不同提取方法对桦褐孔菌粗提物中活性成分含量的影响。结果表明,该检测方法精密度较高,3种化合物的精密度的相对标准偏差(relative standard deviation,RSD)分别为0.14%、0.06%、0.20%;重复性RSD分别为1.67%、1.98%、2.22%;在24 h内稳定性较好,其RSD分别为0.20%、0.61%、0.25%。对比不同提取方法对3种化合物的影响,发现采用超声辅助提取法得到的目标化合物产量较高,适用于桦褐孔菌中主要活性成分的提取。该研究建立的HPLC法检测桦褐孔菌粗提物中原儿茶酸、原儿茶醛和紫萁酮含量的结果准确。
文摘Lemon oils are broadly used as flavoring agents in beverages,foods,cosmetics and pharmaceuticals,yet the adulteration of natural,particularly cold pressed lemon oils is very common in the industry due to its unmet demand and high cost.Nowadays,most quality control(QC)analysis of lemon oils is conducted by gas chromatography(GC)analysis,which is far from a reliable method.Oxygen heterocyclic compounds(OHCs)in non-volatile fraction are gaining increasing attention in authentication process because of the nearly finger-printing profiles of OHCs in cold pressed citrus essential oils.Our goal in this study was to identify OHCs using high performance liquid chromatography(HPLC)in lemon oils,establish OHC profiles,perform stepwise logistic regression analysis(SLRA)and build effective predicting model and further determine adulterated lemon oils by referencing the OHC profiles and established models.After HPLC analyses,profiling and SLRA modeling of 154 OHCs samples of industrial lemon oils,we found that the combination of isopimpinellin and total OHC concentration are essential and robust predictors to differentiate authentic samples from adulterated lemon oils with a success rate of 98%from the 5-fold cross validation.This study provided a reliable and efficient method in determining the authenticity of lemon oils.
基金National Key Research and Development Program of China(Project No.2018YFC1603400)Science and Technology Program of Hebei Province(Project No.19225503D)Technical Support Project of State Administration for Market Regulation(Project No.2019YJ009).
文摘In this experiment,a liquid chromatography tandem mass spectrometry method was built to determine 15 pesticide residues in Chinese cabbage and cucumber samples based on online turbulent flow chromatography purification.After modified quick,easy,cheap,effective,rugged,and safe(QuEChERS)extraction,extracts were directly injected to the TLX(TurboFlow Liquid Xcalibur)system and brought to TurboFlow™columns for on-line purification and then transferred to analytical column for further separation and analysis.TurboFlow™columns types,transfer flow rate,and transfer time were optimized.Limits of detection and limits of quantification of the method obtained for 15 pesticide residues were ranged between 0.2–1.0μg/kg and 0.5–2.0μg/kg in Chinese cabbage and cucumber samples.Recoveries of pesticide residues were in range of 75.3%–103.7%.Matrix effects for 15 pesticides were in range of 5.6%–106.6%.The developed method has been successfully used for the determination of 15 pesticide residues in real samples.
基金the Natural Science Foundation of Jiangxi Province,China(No.20202BABL203004)the Opening Project of the State Key Laboratory of Nuclear Resources and Environment(East China University of Technology)(No.2022NRE23)the Opening Project of Jiangxi Province Key Laboratory of Polymer Micro/Nano Manufacturing and Devices(No.PMND202101).
文摘The novel pulsed liquid chromatography radionuclide separation method presented here provides a new and promising strategy for the extraction of uranium from seawater.In this study,a new chromatographic separation method was proposed,and a pulsed nuclide automated separation device was developed,alongside a new chromatographic column.The length of this chromatographic column was 10 m,with an internal warp of 3 mm and a packing size of 1 mm,while the total separation units of the column reached 12,250.The most favorable conditions for the separation of nuclides were then obtained through optimizing the separation conditions of the device:Sample pH in the column=2,sample injection flow rate=5.698 mL/min,chromatographic column heating temperature=60℃.Separation experiments were also carried out for uranium,europium,and sodium ions in mixed solutions;uranium and sodium ions in water samples from the Ganjiang River;and uranium,sodium,and magnesium ions from seawater samples.The separation factors between the different nuclei were then calculated based on the experimental data,and a formula for the separation level was derived.The experimental results showed that the separation factor in the mixed solution of uranium and europium(1:1)was 1.088,while achieving the initial separation of uranium and europium theoretically required a 47-stage separation.Considering the separation factor of 1.50for the uranium and sodium ions in water samples from the Ganjiang River,achieving the initial separation of uranium and sodium ions would have theoretically required at least a 21-stage separation.Furthermore,for the seawater sample separation experiments,the separation factor of uranium and sodium ions was 1.2885;therefore,more than 28 stages of sample separation would be required to achieve uranium extraction from seawater.The novel pulsed liquid chromatography method proposed in this study was innovative in terms of uranium separation and enrichment,while expanding the possibilities of extracting uranium from seawater through chromatography.
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.
文摘An isocratic reversed-phase liquid chromatographic (LC) method is described for the determination of epalrestat and its three stereoisomers (degradation impurities) in drug substance. The LC separation system consisted of a Hypersil C18 column (250 mm×4.6 mm, 5 μm) with a mobile phase comprising methanol, acetonitrile and water (volume ratio 60∶1∶50, pH 4.5) delivered at a flow rate of 1.6 mL/min and UV detection at 280 nm. The proposed LC method is simple and selective for the determination of the stereoisomers of epalrestat in the drug substance with a limit of detection and quantification of 3.9 μg/mL and 4.9 μg/mL, respectively. The stereoisomers were identified by liquid chromatography-mass spectrometry (LC-MS).
