A carbon paste electrode modified with electropolymerized fills of isonicotinic acid was developed. The modified electrode shows excellent electrocatalytic activity toward the oxidation of both dopamine (DA) and epi...A carbon paste electrode modified with electropolymerized fills of isonicotinic acid was developed. The modified electrode shows excellent electrocatalytic activity toward the oxidation of both dopamine (DA) and epinephrine (EP). Separation of the reduction peak potentials for dopamine and epinephrine was about 357 mV in pH 5.3 phosphate buffer solution (PBS) and the character was used for the detection DA and EP simultaneously. The peak currents increase linearly with DA and EP concentration over the range of 8.0×10^-5 to 7.0×10^-4 mol/L and 5.0×10^-6 to 1.0×10^-4 mol/L with detection limits of 2×10^-5 and 1×10^-6 mol/L, respectively. The interference studies showed that the modified electrode exhibits excellent selectivity in the presence of large excess of ascorbic acid (AA).展开更多
To establish an analytical method for determination of four bisphenols (BPA, BPB, BPF, and BPS) and two alkylphenols (4-n-OP, 4-n-NP) in water by ultra performance liquid chromatography- tandem mass spectrometry ...To establish an analytical method for determination of four bisphenols (BPA, BPB, BPF, and BPS) and two alkylphenols (4-n-OP, 4-n-NP) in water by ultra performance liquid chromatography- tandem mass spectrometry (UPLC/MS/MS). The water samples were extracted and condensed with solid-phase extraction (SPE) using C18 cartridges and eluted by acetonitrile. Separation was carried out with Acquity BEH C8 column and detection were performed by UPLC/MS/MS. Quantification was calculated by using the internal standard BPA-d16 and 4-n-NP-d8. The linear correlation coefficients of these compounds in the range of 1.0-100.0μg/L were all over 0.999. The minimum detectable concentrations were 0.75-1.0 ng/L, and the recoveries ranged from 87.0% to 106.9%.展开更多
A novel technique of Moveable Reduction Bed Hydride Generator(MRBHG)was applied tohe hydride generation or cold vapor generation of As,Se,Ge,and Hg existing In TraditionalChinese Medicinal Material(TCM).The si...A novel technique of Moveable Reduction Bed Hydride Generator(MRBHG)was applied tohe hydride generation or cold vapor generation of As,Se,Ge,and Hg existing In TraditionalChinese Medicinal Material(TCM).The simultaneous determination of the multi-elements wasperformed with ICP-MS.A solid reduction system involving the use of potassiumtetraborohydride and tartaric acid was applied to generating metal hydride or cold vaporefficiently.The factors affecting the metal cold vapor generation were studied.The mainadvantage of the technique is that only a 4μL volume of sample was required for the cold vapor展开更多
Stable isotopes in tree-ring cellulose provide important data in ecological,archaeological,and paleoenvironmental researches,thereby,the demand for stable isotope analyses is increasing rapidly.Simultaneous measuremen...Stable isotopes in tree-ring cellulose provide important data in ecological,archaeological,and paleoenvironmental researches,thereby,the demand for stable isotope analyses is increasing rapidly.Simultaneous measurement of cellulose δC and δO values from tree rings would reduce the cost of isotopic commodities and improve the analytical efficiency compared with conventional separate measurement.In this study,we compared the δC and δO values of tree-ringα-cellulose from Tianshan spruce(Picea schrenkiana)in an arid site in the drainage basin of the Urumqi River in Xinjiang of northwestern China based on separate and simultaneous measurements,using the combustion method(at1050°C)and the high-temperature pyrolysis method(at 1350°C and 1400°C).We verified the results of simultaneous measurement using the outputs from separate measurement and found that both methods(separate and simultaneous)produced similar δC values.The two-point calibrated method improved the results(range and variation)of δC and δO values.The mean values,standard deviations,and trends of the tree-ring δC obtained by the combustion method were similar to those by the pyrolysis method followed by two-point calibration.The simultaneously measured δO from the pyrolysis method at 1400°C had a nearly constant offset with that the pyrolysis method at 1350°C due to isotopic-dependence on the reaction temperature.However,they showed similar variations in the time series.The climate responses inferred from simultaneously and separately measured δC and δO did not differ between the two methods.The tree-ring δC and δO values were negatively correlated with standardized precipitation evapotranspiration index from May to August.In addition,the δO was significantly correlated with temperature(positive),precipitation(negative),and relative humidity(negative)from May to August.The tree-ring δC and δO values determined simultaneously through the high-temperature pyrolysis method could produce acceptable and reliable stable isotope series.The simultaneous isotopic measurement can greatly reduce the cost and time requirement compared with the separate isotopic measurement.These results are consistent with the previous studies at humid sites,suggesting that the simultaneous determination of δC and δO in tree-ringα-cellulose can be used in wide regions.展开更多
A highly sensitive double artificial neural network (DANN) analysis with flow-injection chemiluminescence (FI-CL) has been developed to simultaneously determine the trace amounts of the gold and platinum in simula...A highly sensitive double artificial neural network (DANN) analysis with flow-injection chemiluminescence (FI-CL) has been developed to simultaneously determine the trace amounts of the gold and platinum in simulated mixed samples, without the boring process.展开更多
As the most commonly used antipyretic and analgesic drug,paracetamol(PA)coexists with neurotransmitter dopamine(DA)in real biological samples.Their simultaneous determination is extremely important for human health,bu...As the most commonly used antipyretic and analgesic drug,paracetamol(PA)coexists with neurotransmitter dopamine(DA)in real biological samples.Their simultaneous determination is extremely important for human health,but they also interfere with each other.In order to improve the conductivity,adsorption affinity,sensitivity,and selectivity of TiO_(2)-based electrochemical sensor,N-doped carbon@-TiO_(2) double-shelled hollow sphere(HeC/N@TiO_(2))is designed and synthesized by simple alcoholic and hydrothermal method,using polystyrene sphere(PS)as a template.Meanwhile,TiO_(2) hollow spheres(H eTiO_(2))or N-doped carbon hollow spheres(HeC/N)are also prepared by the same method.HeC/N@TiO_(2) has good conductivity,charge separation,and the highly enhanced and stable current responses for the detection of PA and DA.The detection limit and linear range are 50.0 nmol/L and 0.3-50 mmol/L for PA,40.0 nmol/L and 0.3e50 mmol/L for DA,respectively,which are better than those of carbon-based sensors.Moreover,this electrochemical sensor,with high selectivity,strong anti-interference,high reliability,and long time durability,can be used for the simultaneous detection of PA and DA in human blood serum and saliva.The high electrochemical performance of HeC/N@TiO_(2) is attributed to the multifunctional combination of different layers,because of good conductivity,absorption and electrons transfer ability from in-situ N-doped carbon and electrocatalytic activity from TiO_(2).展开更多
Simultaneous determination of epinephrine (EP) and dopamine (DA) at 2,3-dimercaptosuccinic acid (DMSA) modified electrode was studied. The oxidation peaks of the mixture of EP and DA appeared at the same potenti...Simultaneous determination of epinephrine (EP) and dopamine (DA) at 2,3-dimercaptosuccinic acid (DMSA) modified electrode was studied. The oxidation peaks of the mixture of EP and DA appeared at the same potential, but the cathodic peak currents were only linear to the concentration of DA, whereas the anodic peak currents were equal to the sum of individual anodic peak currents of EP and DA. Therefore, a novel electrochemical method for the simultaneous determination of EP and DA at a DMSA modified electrode (DMSA/Au electrode) by cyclic voltammetry was established. The DMSA self-assembled electrode showed good sensitivity, selectivity and stability and could be used to determine DA and EP, simultaneously, in the real application with satisfactory results.展开更多
A gas chromatography mass spectrometry (GC-MS) method has been developed and fully validated for the simultaneous determination of natural borneol (NB) and its metabolite, camphor, in rat plasma. Following a singl...A gas chromatography mass spectrometry (GC-MS) method has been developed and fully validated for the simultaneous determination of natural borneol (NB) and its metabolite, camphor, in rat plasma. Following a single liquid-liquid extraction, the analytes were separated using an HP-5MS capillary column (0.25 mm ? 30 m ? 0.25μm) and analyzed by MS in the selected ion monitoring mode. Selected ion monitor (m/z) of borneol, camphor and internal standard was 95, 95 and 128, respectively. Linearity, accuracy, precision and extraction recovery of the analytes were all satisfactory. The method was successfully applied to pharmacokinetic studies of NB after oral administration to Wistar rats.展开更多
A high performance liquid chromatographic assay has been developed for the simultaneous determination of five water soluble vitamins:thimine, riboflavin, niacin, pyridoxine and folic acid in cereal products and fresh ...A high performance liquid chromatographic assay has been developed for the simultaneous determination of five water soluble vitamins:thimine, riboflavin, niacin, pyridoxine and folic acid in cereal products and fresh vegetables. Food samples were hydrolyzed in 0.4 mol/L HCl, autoclaved at 120℃ 15 psi for 20 minutes, using a μ-Bondapak column (3.9×300mm, Waters Co.), a mobile phase of methanol-water (30:70) (0.005 mol/L heptanesulfonic acid) and a flow rate of 1.0 ml/min gave the most satisfactory separation of the five water soluble vitamins. A double channel deteetion was used: four vitamins (B_5, folic acid, B_2, B_1) were detected hy UV spectrophotometry (254 nm) first, pyridoxine (B_6) was detected by fluoromelry (EX 290nm, EM 395 nm) afterwards. Detection limits were 2, 5, 5, 2and 5ng, linear ranges were 5-10ng, 5-50ng, 5-40ng, 5-50ng and 10-50ng for B_1, B_2, B_5, B_6 and folic acid respectively. Recoveries were 92-100%(B_5), 51-52% (folio acid), 103—105% (B_2), 99—100% (B_6) and 91.3—102% (B_1) respectively. In comparison with a reference method and checking with food composition tables, very satisfactory results were obtained by this method.展开更多
In the past ten years the eomplementary tristimulus speetrophotometryll],eTs,has seen its diverse appli-eations{2一61 though most researehes remain in relatively simpe systems,and less work has been involvinkinetie re...In the past ten years the eomplementary tristimulus speetrophotometryll],eTs,has seen its diverse appli-eations{2一61 though most researehes remain in relatively simpe systems,and less work has been involvinkinetie reaetions. An attemPt has been made on the investigation of some comPlieated systems eontainingrare earths and meta一acetylchloroPhosPhonaz展开更多
The behaviour of the complexes of copper,lead,cadmium and antimony with salicylfluorone (SAF) adsorbed on HMDE has been investigated by derivative chronopotentiometry in NH_3/NH_4C1. The dependence of the peak height...The behaviour of the complexes of copper,lead,cadmium and antimony with salicylfluorone (SAF) adsorbed on HMDE has been investigated by derivative chronopotentiometry in NH_3/NH_4C1. The dependence of the peak height on the dt/dE vs E curve on preconcentration time, the pH of solution and the constant reducing current are discussed. This method achieved the simultaneous determination of copper, lead, cadmium and antimony in human hair.展开更多
A method is developed for the simultaneous determination of ephedrine,pseudoephedrine, norephedrine, norpseudoephedrine and methylephedrine in urine on a capillary column using nitrogen-phosphorus detector.Diphenylami...A method is developed for the simultaneous determination of ephedrine,pseudoephedrine, norephedrine, norpseudoephedrine and methylephedrine in urine on a capillary column using nitrogen-phosphorus detector.Diphenylamine is used as the internal standard.Calibration graphs are linear down to 1.30ug/ml urine.展开更多
A high performance liquid chromatographic method for the simultaneous determination of four fat soluble vitamins: retinol (vitamin A), cholecalciferol(vitamin D), tocopherol(vitamin E) and phylloquinone(vitamin K_1) i...A high performance liquid chromatographic method for the simultaneous determination of four fat soluble vitamins: retinol (vitamin A), cholecalciferol(vitamin D), tocopherol(vitamin E) and phylloquinone(vitamin K_1) in fortified milk powders and egg yolk has been developed. The method requires enzymatic hydrolysis of lipid component of the sample as a pretreatment. Several factors which influence the enzymatic hydrolysis were studied-Separation was achieved using μ-Bondapak C-18 column(3.9×300mm), 98% methanol as mobile phase, a double channel detection was selected; vitamins D_3 E_1 K_1 were detected by UV spectrophotometry (265 nm) first, then vitamin A by fluorometry (EX 325nm, EM 480mm). The retention times of vitamin A_1 D_3, E and K_1 4.87, 9.00, 10.58 and 15.45 min respectively. Detection limit were 0.64, 0.25, 0.50 and 0.07 ng; and the recoveries were 90.5%~103.6% 90.0%~95.6%, 91.7%~98.8%, 91.5%~98.6%, respectively. The vitamins A, D_0, E, K_1 contents in foods were determined satisfactorily.展开更多
A new method for the determination of components in mixed acids has been developed.The mathematical model is obtained from samples of known composition and is then used to predict the concentrations of components in u...A new method for the determination of components in mixed acids has been developed.The mathematical model is obtained from samples of known composition and is then used to predict the concentrations of components in unknown sample.The practical utility of this method is demonstrated for simultaneous determination of two systems of ternary mixed acids and the results are satisfactory.展开更多
With derivative spectrophotometric method,the complexes of lanthanides with 2-(5-bromo-2-pyridylazo)-5-diethylaminophen- ol(5-Br-PADAP)in the presence of octylphenol poly(ethyleneg- lycol)ether(TX-100)were studied.It ...With derivative spectrophotometric method,the complexes of lanthanides with 2-(5-bromo-2-pyridylazo)-5-diethylaminophen- ol(5-Br-PADAP)in the presence of octylphenol poly(ethyleneg- lycol)ether(TX-100)were studied.It is found that the maximum absorption of fourth-order derivative spectra of the neodymium complex by 4f electron transitions is at 579(+)nm and 582(-)nm with molar derivative absorptivities of 5.2×10~3 1.mol^(-1).cm^(-1). The maximum absorption of the zero-order derivative spectra of the complexes for neodymium and praseodymium is at 580hm,the molar absorptivities are 1.47×10~5 l.mol^(-1).cm^(-1)for Nd and 1.26 ×10~5 l.mol^(-1).cm^(-1)for Pr.The component ratio of the complex is Nd:5-Br-PADAP=1:4.Beer's law is obeyed in the range of 0-3.75μg of Nd and Pr in 25ml of solution.The method has been used for the simultaneous determination of Nd and Pr in four synthetic samples and the results obtained are satisfactory.展开更多
Rapid simultaneous determination of chlorophyll a and chlorophyll b by reverse variable-angle synchronous spectrofluorimetry has been studied on a laboratory-constructed microcomputer-controlled versatile spectrofluor...Rapid simultaneous determination of chlorophyll a and chlorophyll b by reverse variable-angle synchronous spectrofluorimetry has been studied on a laboratory-constructed microcomputer-controlled versatile spectrofluorimeter.A method in estimation of scan parameters for the determination of two-component system by variable-angle synchronous spectrofluorimetry has been suggested展开更多
Although at different content levels, phytohormones including auxins, gibberellins, cytokinns and ahscisic acid distribute widely over rice tissues. It has
AIM: To develop and validate a high performance liquid chromatography(HPLC) coupled with diode array and evaporative light scattering detectors(DAD-ELSD) method for the quantitative determination and fingerprint analy...AIM: To develop and validate a high performance liquid chromatography(HPLC) coupled with diode array and evaporative light scattering detectors(DAD-ELSD) method for the quantitative determination and fingerprint analysis of ten active constituents in three chemical classes(namely, xanthone glycosides, steroidal saponins, and alkaloids) in Zhimu-Huangbai herb pair(ZB). METHOD: Chromatographic separation was performed on a Diamonsil C18 column(4.6 mm × 250 mm, 5 μm, Dikma) by gradient elution using acetic acid in acetonitrile solution at a flow rate of 1.0 mL·min–1 at 260 nm. The drift tube temperature of ELSD was set to 60 ℃ and nebulizer gas pressure was 4.0 Bar. Method validation was performed to assure its linearity, limits of detection and quantification, precision, repeatability, stability, and accuracy. RESULTS: The HPLC-DAD-ELSD method allowed the quantification of ten compounds(phellodendrine, jatrorrhizine, palmatine, berberine, neomangiferin, mangiferin, timosaponin E-I, timosaponin B-II, timosaponin B, and timosaponin A-III), and was successfully applied to fingerprint analysis for ten batches of ZB samples. CONCLUSION: This was the first time to apply the combination of DAD and ELSD for the simultaneous determination of ten active ingredients in ZB. The results showed that the combination of quantitative analysis for marker ingredients and chemical fingerprint for the TCM herb pair provides a potentially powerful, widely introduced, and internationally accepted strategy for assessment of complex TCM formulas.展开更多
Objective To establish an HPLC method for the determination of seven flavonoids from the aerial part of Artemisia frigida. Methods Hypersil ODS-2 (300 mm × 4.6 mm, 5 μm) column was used, with acetonitril-0.2% ph...Objective To establish an HPLC method for the determination of seven flavonoids from the aerial part of Artemisia frigida. Methods Hypersil ODS-2 (300 mm × 4.6 mm, 5 μm) column was used, with acetonitril-0.2% phosphoric acid (gradient elution) as a mobile phase, and the detection wavelength was at 283 nm with flow rate at 1 mL/min. Results All calibration curves showed good linear regression (r > 0.9990) within the tested range. All average recovery was more than 98.00% and RSD was less than 3.0% (n = 6). Conclusion The method is steady and with good repeatability, and could be used to determine the content of flavonoids in A. frigida from different areas.展开更多
基金supported by Key Scientific Research Program in Colleges and Universities of Ministry of Education of China(No.207151)Foundation of Educational Commission of Shnanxi Province of China(No.08JK322)Youth Foundation of Xi'an University of Architecture and Technology(No.QN0620)
文摘A carbon paste electrode modified with electropolymerized fills of isonicotinic acid was developed. The modified electrode shows excellent electrocatalytic activity toward the oxidation of both dopamine (DA) and epinephrine (EP). Separation of the reduction peak potentials for dopamine and epinephrine was about 357 mV in pH 5.3 phosphate buffer solution (PBS) and the character was used for the detection DA and EP simultaneously. The peak currents increase linearly with DA and EP concentration over the range of 8.0×10^-5 to 7.0×10^-4 mol/L and 5.0×10^-6 to 1.0×10^-4 mol/L with detection limits of 2×10^-5 and 1×10^-6 mol/L, respectively. The interference studies showed that the modified electrode exhibits excellent selectivity in the presence of large excess of ascorbic acid (AA).
基金supported by the Preventive medicine and public health research project of Anhui,China(No.2011Y0103)the Natural Science Foundation of Anhui,China(No.11040606M216)
文摘To establish an analytical method for determination of four bisphenols (BPA, BPB, BPF, and BPS) and two alkylphenols (4-n-OP, 4-n-NP) in water by ultra performance liquid chromatography- tandem mass spectrometry (UPLC/MS/MS). The water samples were extracted and condensed with solid-phase extraction (SPE) using C18 cartridges and eluted by acetonitrile. Separation was carried out with Acquity BEH C8 column and detection were performed by UPLC/MS/MS. Quantification was calculated by using the internal standard BPA-d16 and 4-n-NP-d8. The linear correlation coefficients of these compounds in the range of 1.0-100.0μg/L were all over 0.999. The minimum detectable concentrations were 0.75-1.0 ng/L, and the recoveries ranged from 87.0% to 106.9%.
文摘A novel technique of Moveable Reduction Bed Hydride Generator(MRBHG)was applied tohe hydride generation or cold vapor generation of As,Se,Ge,and Hg existing In TraditionalChinese Medicinal Material(TCM).The simultaneous determination of the multi-elements wasperformed with ICP-MS.A solid reduction system involving the use of potassiumtetraborohydride and tartaric acid was applied to generating metal hydride or cold vaporefficiently.The factors affecting the metal cold vapor generation were studied.The mainadvantage of the technique is that only a 4μL volume of sample was required for the cold vapor
基金funded by the National Natural Science Foundation of China (41501049, 41571196)the Self-determination Project of the State Key Laboratory of Cryospheric Sciences (SKLCS-ZZ-2018)+3 种基金the "Light of West China" Program of the Chinese Academy of Sciencesthe Youth Innovation Promotion Association, Chinese Academy of Sciences (2016372)the Chinese Scholarship Council (201704910171)the Fundamental Research Funds for the Central Universities (GK201801007)
文摘Stable isotopes in tree-ring cellulose provide important data in ecological,archaeological,and paleoenvironmental researches,thereby,the demand for stable isotope analyses is increasing rapidly.Simultaneous measurement of cellulose δC and δO values from tree rings would reduce the cost of isotopic commodities and improve the analytical efficiency compared with conventional separate measurement.In this study,we compared the δC and δO values of tree-ringα-cellulose from Tianshan spruce(Picea schrenkiana)in an arid site in the drainage basin of the Urumqi River in Xinjiang of northwestern China based on separate and simultaneous measurements,using the combustion method(at1050°C)and the high-temperature pyrolysis method(at 1350°C and 1400°C).We verified the results of simultaneous measurement using the outputs from separate measurement and found that both methods(separate and simultaneous)produced similar δC values.The two-point calibrated method improved the results(range and variation)of δC and δO values.The mean values,standard deviations,and trends of the tree-ring δC obtained by the combustion method were similar to those by the pyrolysis method followed by two-point calibration.The simultaneously measured δO from the pyrolysis method at 1400°C had a nearly constant offset with that the pyrolysis method at 1350°C due to isotopic-dependence on the reaction temperature.However,they showed similar variations in the time series.The climate responses inferred from simultaneously and separately measured δC and δO did not differ between the two methods.The tree-ring δC and δO values were negatively correlated with standardized precipitation evapotranspiration index from May to August.In addition,the δO was significantly correlated with temperature(positive),precipitation(negative),and relative humidity(negative)from May to August.The tree-ring δC and δO values determined simultaneously through the high-temperature pyrolysis method could produce acceptable and reliable stable isotope series.The simultaneous isotopic measurement can greatly reduce the cost and time requirement compared with the separate isotopic measurement.These results are consistent with the previous studies at humid sites,suggesting that the simultaneous determination of δC and δO in tree-ringα-cellulose can be used in wide regions.
文摘A highly sensitive double artificial neural network (DANN) analysis with flow-injection chemiluminescence (FI-CL) has been developed to simultaneously determine the trace amounts of the gold and platinum in simulated mixed samples, without the boring process.
基金supported by the National Natural Science Foundation of China(Grant Nos.:22074058 and 21675077)the Project of Industry-University-Research Cooperation of Fujian Province(Grant No.:2019Y4010)the Education-Science Research Project for Young and Middle-aged Teachers of Fujian(Grant No.:JAT200317).
文摘As the most commonly used antipyretic and analgesic drug,paracetamol(PA)coexists with neurotransmitter dopamine(DA)in real biological samples.Their simultaneous determination is extremely important for human health,but they also interfere with each other.In order to improve the conductivity,adsorption affinity,sensitivity,and selectivity of TiO_(2)-based electrochemical sensor,N-doped carbon@-TiO_(2) double-shelled hollow sphere(HeC/N@TiO_(2))is designed and synthesized by simple alcoholic and hydrothermal method,using polystyrene sphere(PS)as a template.Meanwhile,TiO_(2) hollow spheres(H eTiO_(2))or N-doped carbon hollow spheres(HeC/N)are also prepared by the same method.HeC/N@TiO_(2) has good conductivity,charge separation,and the highly enhanced and stable current responses for the detection of PA and DA.The detection limit and linear range are 50.0 nmol/L and 0.3-50 mmol/L for PA,40.0 nmol/L and 0.3e50 mmol/L for DA,respectively,which are better than those of carbon-based sensors.Moreover,this electrochemical sensor,with high selectivity,strong anti-interference,high reliability,and long time durability,can be used for the simultaneous detection of PA and DA in human blood serum and saliva.The high electrochemical performance of HeC/N@TiO_(2) is attributed to the multifunctional combination of different layers,because of good conductivity,absorption and electrons transfer ability from in-situ N-doped carbon and electrocatalytic activity from TiO_(2).
基金supported by the Natural Science Foundation of Hebei Province(No.C2007000813).
文摘Simultaneous determination of epinephrine (EP) and dopamine (DA) at 2,3-dimercaptosuccinic acid (DMSA) modified electrode was studied. The oxidation peaks of the mixture of EP and DA appeared at the same potential, but the cathodic peak currents were only linear to the concentration of DA, whereas the anodic peak currents were equal to the sum of individual anodic peak currents of EP and DA. Therefore, a novel electrochemical method for the simultaneous determination of EP and DA at a DMSA modified electrode (DMSA/Au electrode) by cyclic voltammetry was established. The DMSA self-assembled electrode showed good sensitivity, selectivity and stability and could be used to determine DA and EP, simultaneously, in the real application with satisfactory results.
基金supported by the National Natural Science Foundation of China (Nos. 81173564,81274028 and 81274102)
文摘A gas chromatography mass spectrometry (GC-MS) method has been developed and fully validated for the simultaneous determination of natural borneol (NB) and its metabolite, camphor, in rat plasma. Following a single liquid-liquid extraction, the analytes were separated using an HP-5MS capillary column (0.25 mm ? 30 m ? 0.25μm) and analyzed by MS in the selected ion monitoring mode. Selected ion monitor (m/z) of borneol, camphor and internal standard was 95, 95 and 128, respectively. Linearity, accuracy, precision and extraction recovery of the analytes were all satisfactory. The method was successfully applied to pharmacokinetic studies of NB after oral administration to Wistar rats.
文摘A high performance liquid chromatographic assay has been developed for the simultaneous determination of five water soluble vitamins:thimine, riboflavin, niacin, pyridoxine and folic acid in cereal products and fresh vegetables. Food samples were hydrolyzed in 0.4 mol/L HCl, autoclaved at 120℃ 15 psi for 20 minutes, using a μ-Bondapak column (3.9×300mm, Waters Co.), a mobile phase of methanol-water (30:70) (0.005 mol/L heptanesulfonic acid) and a flow rate of 1.0 ml/min gave the most satisfactory separation of the five water soluble vitamins. A double channel deteetion was used: four vitamins (B_5, folic acid, B_2, B_1) were detected hy UV spectrophotometry (254 nm) first, pyridoxine (B_6) was detected by fluoromelry (EX 290nm, EM 395 nm) afterwards. Detection limits were 2, 5, 5, 2and 5ng, linear ranges were 5-10ng, 5-50ng, 5-40ng, 5-50ng and 10-50ng for B_1, B_2, B_5, B_6 and folic acid respectively. Recoveries were 92-100%(B_5), 51-52% (folio acid), 103—105% (B_2), 99—100% (B_6) and 91.3—102% (B_1) respectively. In comparison with a reference method and checking with food composition tables, very satisfactory results were obtained by this method.
文摘In the past ten years the eomplementary tristimulus speetrophotometryll],eTs,has seen its diverse appli-eations{2一61 though most researehes remain in relatively simpe systems,and less work has been involvinkinetie reaetions. An attemPt has been made on the investigation of some comPlieated systems eontainingrare earths and meta一acetylchloroPhosPhonaz
基金Project is supported by Natural Science Foundation of Shandong Province
文摘The behaviour of the complexes of copper,lead,cadmium and antimony with salicylfluorone (SAF) adsorbed on HMDE has been investigated by derivative chronopotentiometry in NH_3/NH_4C1. The dependence of the peak height on the dt/dE vs E curve on preconcentration time, the pH of solution and the constant reducing current are discussed. This method achieved the simultaneous determination of copper, lead, cadmium and antimony in human hair.
文摘A method is developed for the simultaneous determination of ephedrine,pseudoephedrine, norephedrine, norpseudoephedrine and methylephedrine in urine on a capillary column using nitrogen-phosphorus detector.Diphenylamine is used as the internal standard.Calibration graphs are linear down to 1.30ug/ml urine.
文摘A high performance liquid chromatographic method for the simultaneous determination of four fat soluble vitamins: retinol (vitamin A), cholecalciferol(vitamin D), tocopherol(vitamin E) and phylloquinone(vitamin K_1) in fortified milk powders and egg yolk has been developed. The method requires enzymatic hydrolysis of lipid component of the sample as a pretreatment. Several factors which influence the enzymatic hydrolysis were studied-Separation was achieved using μ-Bondapak C-18 column(3.9×300mm), 98% methanol as mobile phase, a double channel detection was selected; vitamins D_3 E_1 K_1 were detected by UV spectrophotometry (265 nm) first, then vitamin A by fluorometry (EX 325nm, EM 480mm). The retention times of vitamin A_1 D_3, E and K_1 4.87, 9.00, 10.58 and 15.45 min respectively. Detection limit were 0.64, 0.25, 0.50 and 0.07 ng; and the recoveries were 90.5%~103.6% 90.0%~95.6%, 91.7%~98.8%, 91.5%~98.6%, respectively. The vitamins A, D_0, E, K_1 contents in foods were determined satisfactorily.
基金This project is supported by National Natural Science Foundation of China
文摘A new method for the determination of components in mixed acids has been developed.The mathematical model is obtained from samples of known composition and is then used to predict the concentrations of components in unknown sample.The practical utility of this method is demonstrated for simultaneous determination of two systems of ternary mixed acids and the results are satisfactory.
文摘With derivative spectrophotometric method,the complexes of lanthanides with 2-(5-bromo-2-pyridylazo)-5-diethylaminophen- ol(5-Br-PADAP)in the presence of octylphenol poly(ethyleneg- lycol)ether(TX-100)were studied.It is found that the maximum absorption of fourth-order derivative spectra of the neodymium complex by 4f electron transitions is at 579(+)nm and 582(-)nm with molar derivative absorptivities of 5.2×10~3 1.mol^(-1).cm^(-1). The maximum absorption of the zero-order derivative spectra of the complexes for neodymium and praseodymium is at 580hm,the molar absorptivities are 1.47×10~5 l.mol^(-1).cm^(-1)for Nd and 1.26 ×10~5 l.mol^(-1).cm^(-1)for Pr.The component ratio of the complex is Nd:5-Br-PADAP=1:4.Beer's law is obeyed in the range of 0-3.75μg of Nd and Pr in 25ml of solution.The method has been used for the simultaneous determination of Nd and Pr in four synthetic samples and the results obtained are satisfactory.
基金The Project Supported by National Natural Science Foundation of China.
文摘Rapid simultaneous determination of chlorophyll a and chlorophyll b by reverse variable-angle synchronous spectrofluorimetry has been studied on a laboratory-constructed microcomputer-controlled versatile spectrofluorimeter.A method in estimation of scan parameters for the determination of two-component system by variable-angle synchronous spectrofluorimetry has been suggested
文摘Although at different content levels, phytohormones including auxins, gibberellins, cytokinns and ahscisic acid distribute widely over rice tissues. It has
基金supported by the Natural Science Foundation of Shanghai City,China(No.10411969800)the National Nature Science Foundation of China(Nos.81202866 and 81302856)
文摘AIM: To develop and validate a high performance liquid chromatography(HPLC) coupled with diode array and evaporative light scattering detectors(DAD-ELSD) method for the quantitative determination and fingerprint analysis of ten active constituents in three chemical classes(namely, xanthone glycosides, steroidal saponins, and alkaloids) in Zhimu-Huangbai herb pair(ZB). METHOD: Chromatographic separation was performed on a Diamonsil C18 column(4.6 mm × 250 mm, 5 μm, Dikma) by gradient elution using acetic acid in acetonitrile solution at a flow rate of 1.0 mL·min–1 at 260 nm. The drift tube temperature of ELSD was set to 60 ℃ and nebulizer gas pressure was 4.0 Bar. Method validation was performed to assure its linearity, limits of detection and quantification, precision, repeatability, stability, and accuracy. RESULTS: The HPLC-DAD-ELSD method allowed the quantification of ten compounds(phellodendrine, jatrorrhizine, palmatine, berberine, neomangiferin, mangiferin, timosaponin E-I, timosaponin B-II, timosaponin B, and timosaponin A-III), and was successfully applied to fingerprint analysis for ten batches of ZB samples. CONCLUSION: This was the first time to apply the combination of DAD and ELSD for the simultaneous determination of ten active ingredients in ZB. The results showed that the combination of quantitative analysis for marker ingredients and chemical fingerprint for the TCM herb pair provides a potentially powerful, widely introduced, and internationally accepted strategy for assessment of complex TCM formulas.
文摘Objective To establish an HPLC method for the determination of seven flavonoids from the aerial part of Artemisia frigida. Methods Hypersil ODS-2 (300 mm × 4.6 mm, 5 μm) column was used, with acetonitril-0.2% phosphoric acid (gradient elution) as a mobile phase, and the detection wavelength was at 283 nm with flow rate at 1 mL/min. Results All calibration curves showed good linear regression (r > 0.9990) within the tested range. All average recovery was more than 98.00% and RSD was less than 3.0% (n = 6). Conclusion The method is steady and with good repeatability, and could be used to determine the content of flavonoids in A. frigida from different areas.