Fenton/Fenton-like reactions have gained popularity for their remarkable proficiency in decomposing organic pollutants,especially when enhanced by reductants addition for accel-erating the Fe2+regeneration.Nevertheles...Fenton/Fenton-like reactions have gained popularity for their remarkable proficiency in decomposing organic pollutants,especially when enhanced by reductants addition for accel-erating the Fe2+regeneration.Nevertheless,these works predominantly centered on the formation and utilization of hydroxyl radicals(•OH)in the process,neglecting the evolution of oxidant and reductant due to the difficulty in the simultaneous determination of these two components.By employing the quenching-iodometric method,we could simultaneously determine the concentrations of HSO_(3)-and peroxydisulfate(PDS).This method first employed an excess of peroxymonosulfate(PMS)to effectively quench HSO_(3)-,and then used the iodometric spectrophotometry to simultaneously determine the concentrations of PMS and PDS in the reaction system.Finally,through precise stoichiometric relationships,we could accurately calculate the concentration of HSO_(3)-.Based on this method,we achieved concentration measurements that,upon linear fitting,yielded a correlation coefficient(R^(2))surpassing 0.99,unequivocally affirming the method’s accuracy and trustworthiness.In this work,an innovation approach for determining the concentrations of HSO_(3)-(reductant)and PDS(oxidant)was explored.Additionally,the resilience of the method was verified across different pH levels and in the presence of diverse impurity ions.The results ensured precise concentration measure-ments in the real wastewater.This method was characterized by its simplicity,rapid analysis,and environmental friendliness,offering a newanalytical strategy for the determination of PDS and HSO_(3)-in environmental samples.The method enables more meticulous monitoring of chemical usage in water treatment,facilitating optimized dosing strategies and assessments of reductant-enhanced Fenton or Fenton-like system in water purification.展开更多
The objective of the research is to develop a quantitative method by ultra high-performance liquid chromatography/ quadrupole time-of-flight mass spectrometry （UHPLC/Q-TOF MS） for the analysis of seven major steroid...The objective of the research is to develop a quantitative method by ultra high-performance liquid chromatography/ quadrupole time-of-flight mass spectrometry （UHPLC/Q-TOF MS） for the analysis of seven major steroidal saponins （timosaponin N, timosaponin El, timosaponin BII, timosaponin B, anemarrhenasaponin I, anemarrhenasaponin A2, and timosaponin AIII） in Anemarrhena asphodeloides Bge. The complete separation of these seven steroidal saponins was achieved within 18 min with an ACQUITY UPLC HSS T3 column using an acetonitrile-water （contain 0.1% formic acid） gradient system. The limits of quantitation （LOQ）, 0.18-0.75 ng/pL for seven steroidal saponins, were determined experimentally. The limits of detection （LOD） were found to be 0.05-0.22 ng/μL for these saponins. The correlation coefficients （r2） for calibration curves varied from 0.9902 to 0.9979. This method showed good repeatability for the quantification of these saponins in rhizomes ofA. asphodeloides, with intra-day and inter-day variations of less than 5.0% for seven steroidal saponins. The recoveries of seven steroidal saponins were from 97.13% to 101.98%. The validated method was successfully applied to quantifying seven steroidal saponins in various sources ofA. asphodeloides （different collecting places or processing methods） and Zhimu concentrate-granules （ZMCG）.展开更多
We employed high performance liquid chromatography （HPLC） method coupled with diode array detector （DAD） for the determination of seven major bioactive compounds （forsythoside A, specnuezhenide, phillyrin, schisa...We employed high performance liquid chromatography （HPLC） method coupled with diode array detector （DAD） for the determination of seven major bioactive compounds （forsythoside A, specnuezhenide, phillyrin, schisandrin, schisantherin A, deoxyschizandrin and schisandrin B） in Liuwei Wuling tablet （LWWLT）. The HPLC baseline separation was carried out on an Inertsil ODS-3 column （250 mm×4.6 mm, 5 μm） at 25 ℃ with a gradient elution system composed of 0.1% phosphoric acid solution and acetonitrile. The detection wavelength was set at 230 nm. Calibration curves for seven compounds showed good linear regressions, with correlation coefficients exceeding 0,999 within the tested concentration range. The limits of detection and quantification of each compound were in the range of 0.03-0.28 μg/mL and 0.11-0.87μg/mL, respectively. The relative standard deviation values of precision, stability and repeatability were less than 2.34%. The average recovery of all seven constituents ranged from 96.71% to 103.9%. The validated quantification method was successfully applied for the analysis of 10 batches of commercial LWWLT from Shandong Shibo Jindu Pharmaceutical Co., Ltd. These results would make foundations for quality control and the further pharmacology study of LWWLT.展开更多
An HPLC-DAD-ELSD method was developed and validated for the simultaneous quantitation of seven active components（liquiritin, baicalin, wogonoside, baicalein, wogonin, ginsenosides Re and ginsenosides Rb1） in n-butan...An HPLC-DAD-ELSD method was developed and validated for the simultaneous quantitation of seven active components（liquiritin, baicalin, wogonoside, baicalein, wogonin, ginsenosides Re and ginsenosides Rb1） in n-butanol effective fraction of Xiao Chai Hu Tang. A Diamonsil C18（2） column（4.6 mm × 250 mm, 5 μm） was used as the stationary phase and the mobile phase was consisted of acetonitrile and aqueous phosphate acid（0.05%, v/v）. Gradient elution was carried out at the flow rate of 1 m L/min. The detection wavelength was set at 276 nm and an evaporative light scattering detector was also used. Good linearity for all the seven active components was observed. The established method is simple, fast, reliable, and suitable for the quality control of n-butanol effective fraction of Xiao Chai Hu Tang.展开更多
To determine 13 flavonoids and glycyrrhizic acid in licorice （Glycyrrhiza spp.）, several samples from different areas were examined by HPLC-DAD analysisThe analysis was performed on a Zorbax Extend-C18 （250 mm×...To determine 13 flavonoids and glycyrrhizic acid in licorice （Glycyrrhiza spp.）, several samples from different areas were examined by HPLC-DAD analysisThe analysis was performed on a Zorbax Extend-C18 （250 mm× 4.6 mm, 5 μm） column connected with a Zorbax Extend guard column （20 mm × 4.6 mm, 5 μm）. The mobile phase consisted of （A） acetonitrile and （B） 0.026% aqueous H3PO4 （V/V） using a gradient elution of 20%-25% A at 0-20 min, 25%-33% A at 20-30 min, 33%-50% A at 30-55 min, 50%-60% A at 55-65 min, and 60% A between 65 min and 80 min, and peaks were detected at 280 rim. The fourteen compounds were assigned by HPLC-Orbitrap MS methods. The regression coefficient for the linear equations for the 14 compounds ranged between 0.9998 and 1. The limits of detection and quantification lay in the range of 0.032-2.461 and 0.154-8.202 μg·mL^-1, respectively. The relative recovery rates for the 14 compounds were in the range of 93.90%-106.73% with RSDs being less than 5%. Coefficient variations for intra-day and inter-day precisions were in the range of 0.27%-2.38% and 0.31%-3.51%, respectively. In summary, the validated method was applied to the simultaneous determination of the 14 components in 29 different licorice samples and was proven to be suitable for quality evaluation of licorices and their active fractions.展开更多
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
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
A new analytical method using Back-Propagation （BP） artificial neural networks and spectrophotometry for simultaneous determination of calcium and magnesium in tap water, the Yellow River water and seawater is estab...A new analytical method using Back-Propagation （BP） artificial neural networks and spectrophotometry for simultaneous determination of calcium and magnesium in tap water, the Yellow River water and seawater is established. By condition experiment, the optimum analytical conditions for calcium, magnesium and Arsenazo （Ⅲ） color reactions are obtained. Levenberg- Marquart （L-M） algorithm is used for calculation in BP neural network. The topological structure of three-layer BP ANN network architecture is chosen as 11-10-2 （nodes）. The initial value of gradient coefficient μ is fixed at 0.001 and the increase factor and reduction factor of kt take the default values of the system. The data are processed by computers with our own programs written in MATLAB 7.0. The relative standard deviations of the calculated results for calcium and magnesium are 2.31% and 2.14%, respectively. The results of standard addition method show that the recoveries of calcium and magnesium are 103.6% and 100.8% in the tap water, 103.2% and 96.6% in the Yellow River water （Lijin district of Shandong Province）, and 98.8%-103.3% and 98.43%-103.4% in seawater from Jiaozhou Bay of Qingdao. It is found that 14 common cations and anions do not interfere with the determination of calcium and magnesium under the optimum experimental conditions. The comparative experiments do not show any obvious differ- ence between the results obtained by this new method and those obtained by the classical complexometric titration method in seawater medium. This method exhibits good reproducibility and high accuracy in the determination of calcium and magnesium and can be used for the simultaneous determination of Ca^2＋ and Mg^2＋ in tap water and natural water.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
As more attention is being paid to the characteristics of atmospheric amines,there is also an increasing demand for reliable detection technologies.Herein,a method was developed for simultaneous detection of atmospher...As more attention is being paid to the characteristics of atmospheric amines,there is also an increasing demand for reliable detection technologies.Herein,a method was developed for simultaneous detection of atmospheric amines in both gaseous and particulate phases using gas chromatography-mass spectrometry(GC-MS).The amine samples were collected with and without phosphoric acid filters,followed by derivatization with benzenesulfonyl chloride under alkaline condition prior to GC-MS analysis.Furthermore,the method was optimized and validated for determining 14 standard amines.The detection limits ranged from0.0408-0.421μg/mL(for gaseous samples)and 0.163-1.69μg/mL(for particulate samples),respectively.The obtained recoveries ranged from 68.8%-180%and the relative standard deviation was less than 30%,indicating high precision and good reliability of the method.Seven amines were simultaneously detected in gaseous and particulate samples in an industrial park using the developed method successfully.Methylamine,dimethylamine and diethylamine together accounted for 76.7%and 75.6%of particulate and gaseous samples,respectively.By comparing the measured and predicted values of gas-particle partition fractions,it was found that absorption process of aqueous phase played a more important role in the gas-partition of amines than physical adsorption.Moreover,the reaction between unprotonated amines and acid(aq.)in water phase likely promoted water absorption.Higher measured partition fraction of dibutylamine was likely due to the reaction with gaseous HCl.The developed method would help provide a deeper understanding of gas-particle partitioning as well as atmospheric evolution of amines.展开更多
A new analytical method using Back-Propagation (BP) artificial neural network and kinetic spectrophotometry for simultaneous determination of iron and magnesium in tap water, the Yellow River water and seawater is est...A new analytical method using Back-Propagation (BP) artificial neural network and kinetic spectrophotometry for simultaneous determination of iron and magnesium in tap water, the Yellow River water and seawater is established. By conditional experiments, the optimum analytical conditions and parameters are obtained. Levenberg-Marquart (L-M) algorithm is used for calculation in BP neural network. The topological structure of three-layer BP ANN network architecture is chosen as 15-16-2 (nodes). The initial value of gradient coefficient μ is fixed at 0.001 and the increase factor and reduction factor of μ take the default values of the system. The data are processed by computers with our own programs written in MATLAB 7.0. The relative standard deviation of the calculated results for iron and manganese is 2.30% and 2.67% respectively. The results of standard addition method show that for the tap water, the recoveries of iron and manganese are in the ranges of 98.0%-104.3% and 96.5%-104.5%, and the RSD is in the range of 0.23%-0.98%; for the Yellow River water (Lijin district of Shandong Province), the recoveries of iron and manganese are in the ranges of 96.0%-101.0% and 98.7%-104.2%, and the RSD is in the range of 0.13%-2.52%; for the seawater in Qingdao offshore, the recoveries of iron and manganese are in the ranges of 95.3%-104.8% and 95.3%-104.7%, and the RSD is in the range of 0.14%-2.66%. It is found that 21 common cations and anions do not interfere with the determination of iron and manganese under the optimum experimental conditions. This method exhibits good reproducibility and high accuracy in the determination of iron and manganese and can be used for the simultaneous determination of iron and manganese in tap water and natural water. By using the established ANN- catalytic spectrophotometric method, the iron and manganese concentrations of the surface seawater at 11 sites in Qingdao offshore are determined and the level distribution maps of iron and manganese are drawn.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 method for simultaneous determination of particulate inorganic phosphorus (PIP) and particulate organic phosphorus (POP) in seawater was improved. After using cellulose acetate membrane to filter the seawater sample...A method for simultaneous determination of particulate inorganic phosphorus (PIP) and particulate organic phosphorus (POP) in seawater was improved. After using cellulose acetate membrane to filter the seawater samples and washing the membrane with 1mol/L hydrochloric acid, PIP was extracted into hydrochloric acid phase and POP was left on the membrane. POP was oxygenated at 120℃, 0.12MPa with potassium persulphate. Phosphomolybdate blue spectrophotometry was used in the determination. The proper volume of seawater sample for simultaneously determining PIP and POP was 100-150ml, containing PIP≥0.27μg, POP≥0.69μg. Relative Standard Deviation (RSD) of the determination of PIP and POP was 5.8% and 4.3% respectively. This method was used to determine POP and PIP in the surface water of Huiquan Bay, Qingdao, China. PIP content there averaged at 69.0μg/L and POP at 3.3μg/L. PIP is the main form (>93%) of particulate phosphorus (PP). Maximum PIP coincided with flood tide, indicating that PIP mainly originated from disturbance of surface sediments. At the offshore area, maximum of PIP appeared at flood tide and minimum of PIP appeared at ebb-tide. The maximum of POP presented at about 10:00am, which suggests that POP is closely related to biological metabolism. The control factor of POP in seawater was concluded to be biological metabolization.展开更多
dual-standard addition method was proposed and the principle of simultaneous determination for a interfering binary mixtures was discussed. The proposed procedure was applied to spectroscopic analyses for the simultan...dual-standard addition method was proposed and the principle of simultaneous determination for a interfering binary mixtures was discussed. The proposed procedure was applied to spectroscopic analyses for the simultaneous determination of uranium and thorium without prior separation. Various molar ratios of uranium/thorium, from 0.5∶1 to 10∶1, can be determined with satisfactory precision and accuracy. Uranium and thorium content in a phosphate ore and simulated sample were determined, the recoveries were 98.4%～102.5% for uranium and 96.8%～102.3% for thorium, the relative standard deviations (R.S.D) were 1.5%～2.3% for uranium and 2.1%～3.1% for thorium.展开更多
基金supported by National Natural Scienc Foundation of China(No.52400097)the Nanqiang Young Talents Supporting Program from Xiamen University.
文摘Fenton/Fenton-like reactions have gained popularity for their remarkable proficiency in decomposing organic pollutants,especially when enhanced by reductants addition for accel-erating the Fe2+regeneration.Nevertheless,these works predominantly centered on the formation and utilization of hydroxyl radicals(•OH)in the process,neglecting the evolution of oxidant and reductant due to the difficulty in the simultaneous determination of these two components.By employing the quenching-iodometric method,we could simultaneously determine the concentrations of HSO_(3)-and peroxydisulfate(PDS).This method first employed an excess of peroxymonosulfate(PMS)to effectively quench HSO_(3)-,and then used the iodometric spectrophotometry to simultaneously determine the concentrations of PMS and PDS in the reaction system.Finally,through precise stoichiometric relationships,we could accurately calculate the concentration of HSO_(3)-.Based on this method,we achieved concentration measurements that,upon linear fitting,yielded a correlation coefficient(R^(2))surpassing 0.99,unequivocally affirming the method’s accuracy and trustworthiness.In this work,an innovation approach for determining the concentrations of HSO_(3)-(reductant)and PDS(oxidant)was explored.Additionally,the resilience of the method was verified across different pH levels and in the presence of diverse impurity ions.The results ensured precise concentration measure-ments in the real wastewater.This method was characterized by its simplicity,rapid analysis,and environmental friendliness,offering a newanalytical strategy for the determination of PDS and HSO_(3)-in environmental samples.The method enables more meticulous monitoring of chemical usage in water treatment,facilitating optimized dosing strategies and assessments of reductant-enhanced Fenton or Fenton-like system in water purification.
基金Major National Science and Technology Projects (Grant No. 2009ZX09102-106, 2011ZX09102-002-09)National Natural Science Foundation of China (Grant No. 81274053)
文摘The objective of the research is to develop a quantitative method by ultra high-performance liquid chromatography/ quadrupole time-of-flight mass spectrometry （UHPLC/Q-TOF MS） for the analysis of seven major steroidal saponins （timosaponin N, timosaponin El, timosaponin BII, timosaponin B, anemarrhenasaponin I, anemarrhenasaponin A2, and timosaponin AIII） in Anemarrhena asphodeloides Bge. The complete separation of these seven steroidal saponins was achieved within 18 min with an ACQUITY UPLC HSS T3 column using an acetonitrile-water （contain 0.1% formic acid） gradient system. The limits of quantitation （LOQ）, 0.18-0.75 ng/pL for seven steroidal saponins, were determined experimentally. The limits of detection （LOD） were found to be 0.05-0.22 ng/μL for these saponins. The correlation coefficients （r2） for calibration curves varied from 0.9902 to 0.9979. This method showed good repeatability for the quantification of these saponins in rhizomes ofA. asphodeloides, with intra-day and inter-day variations of less than 5.0% for seven steroidal saponins. The recoveries of seven steroidal saponins were from 97.13% to 101.98%. The validated method was successfully applied to quantifying seven steroidal saponins in various sources ofA. asphodeloides （different collecting places or processing methods） and Zhimu concentrate-granules （ZMCG）.
基金State Project for Essential Drug Research and Development(Grant No.2012ZX09J12108-04C)Special Project of Military Health Ministry(Grant No.13ZJZ12-5)
文摘We employed high performance liquid chromatography （HPLC） method coupled with diode array detector （DAD） for the determination of seven major bioactive compounds （forsythoside A, specnuezhenide, phillyrin, schisandrin, schisantherin A, deoxyschizandrin and schisandrin B） in Liuwei Wuling tablet （LWWLT）. The HPLC baseline separation was carried out on an Inertsil ODS-3 column （250 mm×4.6 mm, 5 μm） at 25 ℃ with a gradient elution system composed of 0.1% phosphoric acid solution and acetonitrile. The detection wavelength was set at 230 nm. Calibration curves for seven compounds showed good linear regressions, with correlation coefficients exceeding 0,999 within the tested concentration range. The limits of detection and quantification of each compound were in the range of 0.03-0.28 μg/mL and 0.11-0.87μg/mL, respectively. The relative standard deviation values of precision, stability and repeatability were less than 2.34%. The average recovery of all seven constituents ranged from 96.71% to 103.9%. The validated quantification method was successfully applied for the analysis of 10 batches of commercial LWWLT from Shandong Shibo Jindu Pharmaceutical Co., Ltd. These results would make foundations for quality control and the further pharmacology study of LWWLT.
基金Foundation for Young Scholars of Shanxi Province,China(Grant No.2011021007-2)
文摘An HPLC-DAD-ELSD method was developed and validated for the simultaneous quantitation of seven active components（liquiritin, baicalin, wogonoside, baicalein, wogonin, ginsenosides Re and ginsenosides Rb1） in n-butanol effective fraction of Xiao Chai Hu Tang. A Diamonsil C18（2） column（4.6 mm × 250 mm, 5 μm） was used as the stationary phase and the mobile phase was consisted of acetonitrile and aqueous phosphate acid（0.05%, v/v）. Gradient elution was carried out at the flow rate of 1 m L/min. The detection wavelength was set at 276 nm and an evaporative light scattering detector was also used. Good linearity for all the seven active components was observed. The established method is simple, fast, reliable, and suitable for the quality control of n-butanol effective fraction of Xiao Chai Hu Tang.
基金supported by the National Natural Science Foundation of China(No.81001630)Natural Science Foundation of Shanghai(No.10ZR1436400)+1 种基金Major Projects of Knowledge Innovation Program of the Chinese Academy of Sciences(No.KSCX2-YW-R-166)the Twelfth Five-Year National Science&Technology Support Program(No.2012BAI29B06)
文摘To determine 13 flavonoids and glycyrrhizic acid in licorice （Glycyrrhiza spp.）, several samples from different areas were examined by HPLC-DAD analysisThe analysis was performed on a Zorbax Extend-C18 （250 mm× 4.6 mm, 5 μm） column connected with a Zorbax Extend guard column （20 mm × 4.6 mm, 5 μm）. The mobile phase consisted of （A） acetonitrile and （B） 0.026% aqueous H3PO4 （V/V） using a gradient elution of 20%-25% A at 0-20 min, 25%-33% A at 20-30 min, 33%-50% A at 30-55 min, 50%-60% A at 55-65 min, and 60% A between 65 min and 80 min, and peaks were detected at 280 rim. The fourteen compounds were assigned by HPLC-Orbitrap MS methods. The regression coefficient for the linear equations for the 14 compounds ranged between 0.9998 and 1. The limits of detection and quantification lay in the range of 0.032-2.461 and 0.154-8.202 μg·mL^-1, respectively. The relative recovery rates for the 14 compounds were in the range of 93.90%-106.73% with RSDs being less than 5%. Coefficient variations for intra-day and inter-day precisions were in the range of 0.27%-2.38% and 0.31%-3.51%, respectively. In summary, the validated method was applied to the simultaneous determination of the 14 components in 29 different licorice samples and was proven to be suitable for quality evaluation of licorices and their active fractions.
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.
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）.
文摘A new analytical method using Back-Propagation （BP） artificial neural networks and spectrophotometry for simultaneous determination of calcium and magnesium in tap water, the Yellow River water and seawater is established. By condition experiment, the optimum analytical conditions for calcium, magnesium and Arsenazo （Ⅲ） color reactions are obtained. Levenberg- Marquart （L-M） algorithm is used for calculation in BP neural network. The topological structure of three-layer BP ANN network architecture is chosen as 11-10-2 （nodes）. The initial value of gradient coefficient μ is fixed at 0.001 and the increase factor and reduction factor of kt take the default values of the system. The data are processed by computers with our own programs written in MATLAB 7.0. The relative standard deviations of the calculated results for calcium and magnesium are 2.31% and 2.14%, respectively. The results of standard addition method show that the recoveries of calcium and magnesium are 103.6% and 100.8% in the tap water, 103.2% and 96.6% in the Yellow River water （Lijin district of Shandong Province）, and 98.8%-103.3% and 98.43%-103.4% in seawater from Jiaozhou Bay of Qingdao. It is found that 14 common cations and anions do not interfere with the determination of calcium and magnesium under the optimum experimental conditions. The comparative experiments do not show any obvious differ- ence between the results obtained by this new method and those obtained by the classical complexometric titration method in seawater medium. This method exhibits good reproducibility and high accuracy in the determination of calcium and magnesium and can be used for the simultaneous determination of Ca^2＋ and Mg^2＋ in tap water and natural water.
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%.
基金supported from the National Natural Science Foundation of China(Nos.42020104001 and 41805103)Local Innovative and Research Team Project of Guangdong Pearl River Talents Program(No.2017BT01Z032)the Fund from Chemistry and Chemical Engineering Guangdong Laboratory(No.1922009)
文摘As more attention is being paid to the characteristics of atmospheric amines,there is also an increasing demand for reliable detection technologies.Herein,a method was developed for simultaneous detection of atmospheric amines in both gaseous and particulate phases using gas chromatography-mass spectrometry(GC-MS).The amine samples were collected with and without phosphoric acid filters,followed by derivatization with benzenesulfonyl chloride under alkaline condition prior to GC-MS analysis.Furthermore,the method was optimized and validated for determining 14 standard amines.The detection limits ranged from0.0408-0.421μg/mL(for gaseous samples)and 0.163-1.69μg/mL(for particulate samples),respectively.The obtained recoveries ranged from 68.8%-180%and the relative standard deviation was less than 30%,indicating high precision and good reliability of the method.Seven amines were simultaneously detected in gaseous and particulate samples in an industrial park using the developed method successfully.Methylamine,dimethylamine and diethylamine together accounted for 76.7%and 75.6%of particulate and gaseous samples,respectively.By comparing the measured and predicted values of gas-particle partition fractions,it was found that absorption process of aqueous phase played a more important role in the gas-partition of amines than physical adsorption.Moreover,the reaction between unprotonated amines and acid(aq.)in water phase likely promoted water absorption.Higher measured partition fraction of dibutylamine was likely due to the reaction with gaseous HCl.The developed method would help provide a deeper understanding of gas-particle partitioning as well as atmospheric evolution of amines.
文摘A new analytical method using Back-Propagation (BP) artificial neural network and kinetic spectrophotometry for simultaneous determination of iron and magnesium in tap water, the Yellow River water and seawater is established. By conditional experiments, the optimum analytical conditions and parameters are obtained. Levenberg-Marquart (L-M) algorithm is used for calculation in BP neural network. The topological structure of three-layer BP ANN network architecture is chosen as 15-16-2 (nodes). The initial value of gradient coefficient μ is fixed at 0.001 and the increase factor and reduction factor of μ take the default values of the system. The data are processed by computers with our own programs written in MATLAB 7.0. The relative standard deviation of the calculated results for iron and manganese is 2.30% and 2.67% respectively. The results of standard addition method show that for the tap water, the recoveries of iron and manganese are in the ranges of 98.0%-104.3% and 96.5%-104.5%, and the RSD is in the range of 0.23%-0.98%; for the Yellow River water (Lijin district of Shandong Province), the recoveries of iron and manganese are in the ranges of 96.0%-101.0% and 98.7%-104.2%, and the RSD is in the range of 0.13%-2.52%; for the seawater in Qingdao offshore, the recoveries of iron and manganese are in the ranges of 95.3%-104.8% and 95.3%-104.7%, and the RSD is in the range of 0.14%-2.66%. It is found that 21 common cations and anions do not interfere with the determination of iron and manganese under the optimum experimental conditions. This method exhibits good reproducibility and high accuracy in the determination of iron and manganese and can be used for the simultaneous determination of iron and manganese in tap water and natural water. By using the established ANN- catalytic spectrophotometric method, the iron and manganese concentrations of the surface seawater at 11 sites in Qingdao offshore are determined and the level distribution maps of iron and manganese are drawn.
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 method for simultaneous determination of particulate inorganic phosphorus (PIP) and particulate organic phosphorus (POP) in seawater was improved. After using cellulose acetate membrane to filter the seawater samples and washing the membrane with 1mol/L hydrochloric acid, PIP was extracted into hydrochloric acid phase and POP was left on the membrane. POP was oxygenated at 120℃, 0.12MPa with potassium persulphate. Phosphomolybdate blue spectrophotometry was used in the determination. The proper volume of seawater sample for simultaneously determining PIP and POP was 100-150ml, containing PIP≥0.27μg, POP≥0.69μg. Relative Standard Deviation (RSD) of the determination of PIP and POP was 5.8% and 4.3% respectively. This method was used to determine POP and PIP in the surface water of Huiquan Bay, Qingdao, China. PIP content there averaged at 69.0μg/L and POP at 3.3μg/L. PIP is the main form (>93%) of particulate phosphorus (PP). Maximum PIP coincided with flood tide, indicating that PIP mainly originated from disturbance of surface sediments. At the offshore area, maximum of PIP appeared at flood tide and minimum of PIP appeared at ebb-tide. The maximum of POP presented at about 10:00am, which suggests that POP is closely related to biological metabolism. The control factor of POP in seawater was concluded to be biological metabolization.
文摘dual-standard addition method was proposed and the principle of simultaneous determination for a interfering binary mixtures was discussed. The proposed procedure was applied to spectroscopic analyses for the simultaneous determination of uranium and thorium without prior separation. Various molar ratios of uranium/thorium, from 0.5∶1 to 10∶1, can be determined with satisfactory precision and accuracy. Uranium and thorium content in a phosphate ore and simulated sample were determined, the recoveries were 98.4%～102.5% for uranium and 96.8%～102.3% for thorium, the relative standard deviations (R.S.D) were 1.5%～2.3% for uranium and 2.1%～3.1% for thorium.
