Simultaneous separation and determination of four main isoflavonoids in Astragali Radix by an isocratic LC/ESI-MS method

A simple, reliable and rapid isocratic liquid chromatography(LC)-mass spectrometric detection(MS) coupled with electrospray ionization(ESI) method for simultaneous separation and determination of calycosin-7-O-β-D-glucoside, ononin, calycosin and formonometin in Astragali Radix was developed. After the samples were extracted with ethanol, the optimum separation conditions for these analytes were achieved using water and acetonitrile(70:30, v/v) containing 0.2%(v/v) acetic acid as a mobile phase and a 2.0 mm×150 mm Hypersil-Keystone C18 column. Selective ion monitoring(SIM) mode and [M+H]+ ions at m/z 447, 431, 285 and 269 were used for quantitative analysis of four main active components above mentioned. The calibration curves were linear in the range of 0.4-175.0 μg/mL for calycosin-7-O-β-D-glucoside, 0.2-146.0 μg/m L for ononin, 0.4-210.0 μg/mL for calycosin and 0.5-217.0 μg/mL for formonetion, respectively. The limits of quantification(LOQ) and detection(LOD) were 0.4 μg/mL and 0.08 μg/m L for calycosin-7-O-β-D-glucoside, 0.2 μg/mL and 0.06 μg/m L for ononin, 0.4 μg/mL and 0.1 μg/mL for calycosin, 0.5 μg/m L and 0.1 μg/m L formonetion, respectively. The standard recoveries were in the range of 96.5%-104.7%. The developed method has successfully been used for the determination of four main flavonoids in Astragali Radix from various sources and can be used for identification, differentiation and quality evaluation of Astragali Radix.     

Organic acids and inorganic anions in Bayer liquors by ion chromatography after solid-phase extraction

A method for the simultaneous separation and determination of organic acids and inorganic anions in Bayer liquors was developed by gradient ion chromatography with suppressed conductivity detection. Formate, acetate, propionate, oxalate, succinate, glutarate, fluoride, chloride and sulfate were separated and determined in 33 min. The samples were pretreated with solid-phase extraction, which has high selectivity for removing a large number of metallic ions in the Bayer liquors, and filtered with a 0.45 μm filter membrane before being injected into the ion chromatographic system. The separation of six organic acids and three inorganic anions was achieved on an IonPac AS 11-HC column with KOH as the eluent, and the detection was performed by a conductivity detection mode. No interference is found in the presence of fluorate, chlorate and sulphate when organic acids are determined. The calibration graphs of peak area for all the analytes are linear over a wide range. The relative standard derivation of the peak area of analytes is less than 2.14%. Under optimum conditions the detection ranges from 0.2 to 100.0 mg/L. The average recoveries of the added standards are between 94.3% and 102.8%.     

Determination of Stereoisomers of Epalrestat by Liquid Chromatography

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).     

Dynamic experiment and numerical simulation of solute transmission in heap leaching processing

Solute transmission in saturated ore heap was studied numerically and experimentally. The convection-diffusion equation (CDE) used to describe the mass transportation in porous media was solved by characteristic difference method to give the distribution of the concentration of ferrous ion in the ore column. To calibrate the computational model, a column test was performed using infiltration of sulfide ferrous solution (the initial concentration is c0=0.04 mol/L) on a 100 cm high column composed of ore particles smaller than 10 mm for 2.5 h. The numerical analysis shows that the results obtained from numerical modeling under the same operating conditions as used for column test are in good agreement with those from experimental procedure on the whole trend, which indicates that the model, the numerical method, and the parameters chosen can reflect the rule of ferrous ion transmission in ore heap.     

Simultaneous determination of geniposidic acid. chlorogenic acid and geniposide in eucommia by HPLC

A high performance liquid chromatography ( HPLC) method was established for simultaneous determination of geniposidic acid, chlorogenic acid and geniposide in eucommia. Detection at 240 nm with a reversed-phase column, CH3OH volume fraction, acidic additive and pH value of mobile phase were studied for their effects on the separability of the compounds. The most suitable separation was obtained with isocratic gradient elution system using CH3OH-H2O-H3PO4(12. 00 : 87. 96 : 0. 04, volume ratio) at a flow-rate of 1. 0 mL/min. Under the experimental conditions, the capacity factors of three compounds are in 3-13. The sample is separated rightly. The analysis time is 30 min and the retention time of geniposidic acid, chlorogenic acid and geniposide are 6. 7 min, 10. 5 min and 21 min, respectively.     

Sensitive determination of DNA based on resonance light scattering enhancement of azocarmine G and CTAB

A new method for the determination of DNA was developed with azocarmine G（AG） in the presence of cetyltrimethylammonium bromide（CTAB） by the resonance light scattering （RLS） technique. The synthetic samples were determined with satisfactory results, and the reaction mechanism was also studied. The results show that under the optimum conditions, the weak RLS signal of AG can be enhanced by DNA, which results from the formation of a new ternary complex AG-CTAB-DNA with large size. Moreover, the enhanced RLS intensity at 552 nm is directly proportional to the concentration of DNA in the range of 0 - 1.0 μg/mL for fish sperm DNA （fsDNA） and 0 - 1.5μg/mL for calf thymus DNA （ctDNA）. Based on this, a new assay of DNA can be established. The detection limits （3σ） are 2. 1 ng/mL for fsDNA and 2.2 ng/mL for ctDNA, respectively.     

Determination of paclitaxel in southern yew tree by HPLC

Paclitaxel in southern yew tree was quantitatively determined by high performance liquid chromatography (HPLC) with ODS-C18 column. A mixture of CH3OH-H2O-CH3COOH(volume ratio: 55 :44 :1) is used as mobile phase and UV detection is carried out at 227 nm, and the column temperature is 20℃. The results show that there is a good linear felationship between the area of paclitaxel and the concentration of the sample in the range 50-500 mg/L for paclitaxel. The corresponding regression equation is Y= 13 021. 7 + 1. 01 × 106X, r=0. 9990. The average recovery is 95. 3% and the relative standard deviation is 2. 08%.     

Structural safety monitoring for Nanjing Yangtze River Bridge

In order to evaluate objectively and accurately the integrity, safety and operating conditions in real time for the Nanjing Yangtze River Bridge, a large structural safety monitoring system was described. The monitoring system is composed of three parts: sensor system, signal sampling and processing system, and safety monitoring and assessment system. Combining theoretical analysis with measured data analysis, main monitoring contents and layout of measuring points were determined. The vibration response monitoring was significantly investigated. The main contents of safety monitoring on vibration response monitoring are vibration of the main body of the Nanjing Yangtze river bridge, collision avoidance of the bridge piers, vibration of girders on high piers for the bridge approach and earthquake. As a field laboratory, the safety monitorying system also provides information to investigate the unknown and indeterminate problems on bridge structures and specific environment around bridges.     

A Communication Protocol and Monitoring Policy for Input/Output Vehicles in an Automatic Storage and Retrieval System

The acquisition and processing of equipment information is pivotol to control and management of the automated storage and retrieval system.The work of this paper is based on the automatic storage and retrieval experimental system of Wuhan University of Technology.First,the output/input flow and the control information of storage/retrieval vehicle are studied and the plotting finite state machine model of the stacking crane is established.Then,the communication protocol between the center con- trol management computer and the PLC of stacking crane is designed.Finally,the stacking crane' s monitoring data,which in- clude operating time,running states and real-time position status,are gained by analyzing the communication protocol.The de- tailed program for the acquisition and processing of monitoring information is developed.This method is suitable for the equipment monitoring of the whole system,and provides a platform for studying the intelligent control and optimal scheduling strategies of AS/RS.     

Development and Validation of a HPLC Method for Determination of Flavone Glycoside-Camellianin B in Cephalotaxus Sinensis

A simple,rapid and sensitive method for the quantification of camellianin B in Cephalotaxus sinensis(C.sinensis)a natural plant with anti-hyperglycemic effect,was developed and validated by reversed phase liquid chromatography.Chromatographic separation was achieved on a C18 column and an isocratic elution was carried out at a flow-rate of 1.0 mL·min~(-1) with the acetonitrile-water containing0.1%formic acid(19∶81,v/v).The detection wavelength was set at 330 nm.The calibration curve was linear over the concentration range of 0.25-50μg·mL~(-1) with correlation coefficients larger than0.999 5.The limit of detection and limit of quantification were 0.09μg·mL~(-1)and 0.25μg·mL~(-1),respectively.The precisions and accuracy for all samples were acceptable.The validated method has been successfully applied for the quantification of camellianin B in C.sinensis harvested in different months and may also be used as the quality evaluation of this herb medicine.     

Direct rapid determination of traces of sulfide in environment samples

An improved ethylene blue method for determination of sulfide is developed. It has been adapted to a direct determination of sulfide by both common spectrophotometric method and total differential spectrophotometric method. In common spectrophotometric method, the calibration curve is A=1.69ρ+0.006 and the correlation coefficient is 0.9994.The apparent molar absorptivity is 5.42×104 L*mol-1*cm-1 and calibration curve is liner when ρ is in the range of 0-0.9 mg*L-1. In total differential spectrophotometric method, the calibration curve is A=9.25ρ+0.004 and the correlation coefficient is 0.9996. The apparent molar absorptivity is 2.96×105 L*mol-1*cm-1and calibration curve is liner when ρ is in the range of 0-0.10 mg*L-1. The sensitivity of this method is increased significantly compared with the former ethylene blue method. The speed of reaction is also faster than the former one. The limit of detection is found to be 1.0 ng*mL-1 by both common spectrophotometric method and total differential spectrophotometric method. Ten replicate analyses of a sample solution containing 100 ng*mL-1sulfide give a relative standard deviation of 1.8%. The effects of various cations and anions on the determination of sulfide are studied and procedures for removal of interference is described. The method is used for the determination of sulfide in environment samples with satisfactory results.     

Catalytic wave of cobalt and its analytical application in rapid determination of trace cobalt in complex zinc electrolyte solution

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Adsorption of D113 resin for dysprosium(III)

The adsorption behavior and mechanism of D113 resin for Dy(III) was investigated by using the method of resin adsorption. Experimental results show that the optimum medium pH of adsorption of D113 resin for Dy³⁺ is pH=6.00 in the HAc-NaAc medium. The static adsorption capacity of D113 resin for Dy³⁺ is 292.7 mg·g⁻¹. The optimum eluant is 0.5 mol·L⁻¹ HCl. The adsorption rate constant is k ₂₉₈=6.8×10⁻⁶s⁻¹. The apparent activation energy of D113 resin for Dy(III) is 14.79 kJ·mol⁻¹. The adsorption behavior of D113 resin for Dy(III) obeys the Freundlich isotherm. The adsorption parameters of thermodynamic are ΔH=14.48 kJ·mol⁻¹, ΔS=54.69 J·mol⁻¹·K⁻¹, ΔG=−1.82 kJ·mol⁻¹.The adsorption mechanism of D113 resin for Dy³⁺ was confirmed by chemical analysis and IR spectra. Funded by the Natural Science Foundation of Zhejiang Province (No.201027), Foundation of Zhejiang Provincial Education Bureau (No.20040551) and Zhoushan Science Technology Bureau (No.04114)     

Influence of formate on bioactivity material-thuringiensin synthesized by <Emphasis Type="Italic">Bacillus thuringiensis</Emphasis> YBT-032

The biological method to synthesize thuringiensin and the influence of formate on thuringiensin biosynthesis were investigated. Addition of 1.00 g/L formate to growth medium of bacillus thuringiensis YBT-032 resulted in significant enhancements in productions of citrate, α -ketoglutarate, intracellular adenine and thuringiensin. These results demonstrate that added formate attends metabolism of cell, facilitates carbon metabolic flux in tricarboxylic acid cycle and hexose monophosphate pathway. As a carbon source, formate facilitates cell growth, increases glucose consumption and enhances the ability of cell to synthesis adenine analogues, and subsequently thuringiensin. Thuringiensin production rate significantly enhanced from 6.44 to 8.46 mg·g^-1 · h and transformation ratio from glucose to thuringiensin increased by 43.30%.     

Synthesis and characterization of arsenate antimonic acid AAAc(1 : 1)

The AAAc(1 : 1) was synthesized in water by As₂O₃ and Sb₂O₃ with molar ratio of 1 : 1. AAAc(1 : 1) was characterized by Raman, IR, TG/DTG, DSC, XPS and XRD. The results show that there are four peaks to v _s of As-OH, As-O-Sb, Sb-OH and Sb-O-Sb in Raman spectra of AAAc(1 : 1) at 100 – 1 000 cm⁻¹. The solution of AAAc(1 : 1) was also titrated with KOH solution. The titration results show that AAAc(1 : 1) is a hexabasic acid with dissociation constants of k ₁=3.62 × 10⁻², k ₂=3.05 × 10⁻³, k ₃=6.43 × 10⁻⁶, k ₄ =9.78 × 10⁻⁸, k ₅=1.32 × 10⁻¹¹, k ₆=3.87 × 10⁻¹². AAAc(1 : 1) has a good solubility and stability in water, its solid obtained by free volatilizing water from its solution under air at ambient temperature is amorphous. Chemical and thermal analysis show that the composition of AAAc(1 : 1) is As₂O₅ · Sb₂O₅ · 8H₂O in air at 25 °C. AAAc(1 : 1) has the structure of AsO(OH)₂-OH-Sb(OH)₄-O-Sb(OH)₄-OH-AsO(OH)₂ or As(OH)₃-O-Sb(OH)₄-O-Sb(OH)₄-O-As(OH)₃ (isomerism) through experimental determination and geometry optimization. Foundation item: Project(50274075) supported by the National Natural Science Foundation of China     

Fluorescence properties and application of doping complexes Eu1-xLx (TTA)3Phen as light conversion agents

Light conversion agents Eu1-x Lx (TTA)3 Phen (L denotes La3+ , Gd3+ , Y3+ ) complexes were prepared,and the influence of doping ions on fluorescence properties was investigated by elementary analysis, FTIR and fluorescent spectra. The results show that FTIR spectra of Eu1_x Lx (TTA)3 Phen complex system are identical with that of EuTTA3 Phen, which indicates that the complexes Eu1 xLx(TTA)3Phen are similar in structure to Eu (TTA)3Phen. For the above doping elements, co-fluorescence enhancement has the following order: Gd3+ ＞Y3+ ＞La3+ , and the optimum mole fractions of doping elements are 0.4, 0.2 and 0.5 respectively for Gd3+ , Y3+ ,La3+. Among all the complexes, Eu0.6 Gd0.4 (TTA)3 Phen complex has the strongest fluorescent intensity. Applying Eu0.6 Gd0.4 (TTA)3 Phen complex to plastic and printing inks, bright red fluorescence plastic and printing inks are obtained when the content of europium reaches 0.1% (mass fraction).     

Hyers-Ulam-Rassias stability of approximate isometries on restricted domains

Let X and Y be real Banach spaces. The stability of Hyers-Ulam-Rassias approximate isometries on restricted domains S(unbounded or bounded) for into mapping f: S→Y satisfying ‖f(x)-f(y)‖-‖x-y‖≤ε(x,y) for all x,y∈S is studied in case that the target space Y is uniformly convex Banach space of the modulus of convexity of power type q≥2 or Y is the Lq(Ω,,μ) (1＜q＜ ∞) space or Y is a Hilbert space. Furthermore, the stability of approximate isometries for the case that (x,y)=‖x‖p ‖y‖p or (x,y)=‖x-y‖p for p≠1 is investigated.     

Adsorption of Macroporous Phosphonic Acid Resin for Nickel

1Introduction Thesynthesischaracterizationandadsorptionproper tyofpolymericmaterialshavebeenresearchedinrecent years[110].Macroporousphosphonicacidresin[11](PAR)isanovelpolymericmaterialwhichcontainsafunctional groupof[PO(OH)2].Ithasalotofadvantagessuchas…     

Manufacture of high-dispersed W-Cu composite powder by mechano-thermal process

In order to improve the process of co-reduction of oxide powder, a new mechano-thermal process was designed to produce high-dispersed W-Cu composite powder by high temperature oxidation, short time high-energy milling and reduction at lower temperature. The particle size, oxygen content and their sintering abilities of W-Cu composite powder in different conditions were analyzed. The results show that after a quick milling of the oxide powder for about 3-10 h, the reduction temperature of the W-Cu oxide powder can be lowered to about 650 ℃ from 700-750 ℃ owning to the lowering of particle size of the oxide powder. The average particle size of W-Cu powder after reduction at 650 ℃ is about 0. 5μm smaller than that reduced at 750 ℃. After sintering at 1 200℃ for 1 h in hydrogen atmosphere, the relative density and thermal conductivity of final products (W-20Cu) can attain 99. 5% and 210 W ·m-1· K-1 respectively.     

Water permeability parameters of dermal fibroblast employed in tissue engineering in subzero temperatures

In the construction of the tissue engineered dermal equivalent, the dermal fibroblast plays a crucial role[1]. While the fibroblasts need time to proliferate, synthesize, and se-crete extracellular matrix in the three-dimensional scaffold postseeding, a degradablescaffold commences disintegration over time. This may lead to an unusable product, if proper preservation does not conduct. Cryopreservation could solve this problem. The possibility of the long-term banking of cells and tissues would…