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Abstract  

Four ethylenediamine-N,N,N′,N′-tetraacetate complexes with Sb(III)-M-Sb(III) polynuclear structure (M=Co(II), La(III), Nd(III), Dy(III)) are synthesized. [Sb24-(EDTA)2Co(H2O)2]·5.15H2O is characterized by single crystal X-ray diffraction. The crystal structure of [Sb24-(EDTA)2Co(H2O)2]·5.15H2O belongs to monoclinic system, space group P21/n, lattice parameters: a=6.9969(2), b=20.8705(4), c=10.8106(2) Å, β=90.031(1)°, V=1578.66(6) Å3, Z=2, M r=1007.76, D c=2.120 g cm−3, F(000)=1001, μ=2.323 mm−1, the final R=0.0235 and wR=0.0629 for 3480 observed reflections (I>2σ(I)). The powder X-ray diffraction patterns of the complexes are also measured. Elemental analyses, FTIR spectra, TG-DSC and DTA of [Sb2(EDTA)2Ln]NO3·nH2O are performed. FTIR spectra reveal that the antimony and other metallic ions were connected through the carboxylate bridges. The thermal analysis can demonstrate the complex formation of the antimony, other metallic ions and EDTA. The possible pyrolysis reactions in the thermal decomposition process of the complexes, the experimental and calculated percentage mass losses are also given.

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Abstract  

Research on extracted 90Y with di(2-ethylhexyl) orthophosphoric acid (P204) in lipiodol for liver cancer was made to evaluate the stability of extracted 90Y with P204 in lipiodol (90Y-P204-lipiodol) in serum of newly-born cattle and human’s blood. At first, P204 (extractant) was dissolved in lipiodol (organic phase). Secondly, 90Y was extracted to organic phase after adding 90Y solution into test tube with P204 and lipiodol in it. The extracting efficiency with 0.01 mol/l P204 could reach 99.4%. The stability of 90Y-P204-lipiodol has been experimented in physiological saline solution as preparation for further stability experiment. The result indicated that the extracted 90Y lost 0.02%–0.36% in physiological saline solution. The results of further stability experiment showed that loss efficiencies of extracted 90Y after adding newly-born cattle serum 1 hour, 1 day, 3 and 7 days are 3.38%, 3.12%, 4.29% and 6.62%, respectively, and loss efficiencies of extracted 90Y after adding human’s blood 1 hour, 1 day, 3 and 7 days are 2.55%, 5.91%, 7.88% and 5.63%, respectively. Our data also indicated that 90Y is the most possible radioisotope for being extracted with P204 in lipiodol to treat hepatocellular carcinoma, particularly in cases of unresectable liver tumors, since 90Y is available from several commercial sources in clinical quality. We conclude that the stability of 90Y-P204-lipiodol tested with newly-born cattle serum and human’s blood attained great results. 90Y-P204-lipiodol is a kind of potential and exciting pharmaceutical in inerventional therapy for liver cancer and we can carry on the further animal test and clinical trial.

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Journal of Thermal Analysis and Calorimetry
Authors:
J. Yao
,
F. Wang
,
L. Tian
,
Y. Zhou
,
H. Chen
,
K. Chen
,
N. Gai
,
R. Zhuang
,
T. Maskow
,
B. Ceccanti
, and
G. Zaray

Abstract  

Using TAM III multi-channel calorimetry combined with direct microorganism counting (bacteria, actinomycetes and fungi) under laboratory conditions, we determined the microbial population count, resistance and activity toward cadmium (Cd(II)) and hexavalent chromium (Cr(VI)) toxicity in soil. The thermokinetic parameters, which can represent soil microbial activity, were calculated from power-time curves of soil microbial activity obtained by microcalorimetric measurement. Simultaneous application of the two methods showed that growth rate constant (k), peak-heat output power (P max) and the number of living microorganisms decreased with increasing concentration of Cd and Cr. The accumulation of Cr on E. coli was conducted by HPLC-ICP-MS. Cr6+ accumulation by Escherichia coli was increased steadily with increasing Cr6+ concentration. The results revealed that the change in some thermo-kinetic parameters could have good corresponding relationship with metal accumulation. Our work also suggests that microcalorimetry is a fast, simple, more sensitive, on-line and in vitro method that can be easily performed to study the toxicity of different species of heavy metals on microorganism compared to other biological methods, and can combine with other analytic methods to study the interaction mechanism between environmental toxicants and microbes.

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Summary

A highly sensitive and reproducible isocratic liquid chromatographic method has been developed for the analysis of artemisinin and its three commonly used derivatives (artesunate, dihydroartemisinin, and artemether). The method involves a precolumn derivatization reaction with 4-carboxyl-2,6-dinitrobenzene diazonium ion to produce azo adducts that are UV-active. The critical parameters for the derivatization such as temperature, reaction time, and reagent concentrations were studied and optimized. The chromatographic separations were carried out on a C-18 column with mobile phase consisting of acetonitrile-0.1% acetic acid (60:40) at a flow rate of 1 mL min−1. UV detection was set at 254 nm. Dynamic linear calibration range was obtained at concentrations of artemisinins ranging from 0.26 to 1.44 μg mL−1. The low limits of detections of artemisinin, artesunate, dihydroartemisinin, and artemether were found to be 0.091, 0.0125, 0.0489, and 0.0128 ng μL−1, respectively. The developed methods were precise (RSD <3%) and accurate (% error < 5%). The developed methods may find application in dosage form analysis and pharmacokinetic studies.

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Journal of Radioanalytical and Nuclear Chemistry
Authors:
S. Ambe
,
S. Chen
,
Y. Ohkubo
,
Y. Kobayashi
,
H. Maeda
,
M. Iwamoto
,
M. Yanokura
,
N. Takematsu
, and
F. Ambe

Abstract  

We established Multitracer, a new versatile radiotracer technique, for simultaneous tracing of a number of elements in various chemical, environmental, and biological systems. Metal foil targets (typically Au, Ag, Ge, Cu and Fe) are irradiated with C, N, or O ions accelerated up to 135 MeV/nucleon by RIKEN Ring Cyclotron. Radiochemical procedures have been developed to remove the target material leaving the nuclides as Multitracer solutions containing various radionuclides of Be, Na, Mg, K, Ca, Sc, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Br, Rb, Sr, Y, Zr, Nb, Mo, Tc, Ru, Rh, Pd, Ag, Cd, In, Sn, Te, I, Ba, Ce, Pm, Eu, Gd, Tb, Tm, Yb, Lu, Hf, W, Re, Os, Ir, Pt, and Hg. Multitracers enable efficient tracing of a number of elements, and comparison of their behavior under strictly identical experimental conditions. Such features will be demonstrated by means of an example of application to a model experiment for the study of removal mechanism of various elements from the ocean.

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Abstract  

The iron contents in the hair and blood samples of 37 juvenile athletes who were supplemented with 0, 8 and 16 mg Fe/day, respectively, in the food of ferrous gluconatecontaining chocolate for 3 months were determined before and after the supplementation by INAA, SRXRF and blood analysis. The experimental results showed that after supplementation of the iron-fortified food, the normal ferritin level in the blood of the male athletes was attained and the iron content in the hair was increased with supplementation, but both are not in the positive proportion. Most of the female athletes had similar results. It is suggested that supplementation of 8 mg iron/day to juvenile athletes may be desirable.

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Abstract  

Methyl ethyl ketone peroxide (MEKPO) is an unstable material above certain limits of temperature, decomposing into chain reactions by radicals. The influence of runaway reactions on this basic characteristic was assessed by evaluating kinetic parameters, such as activation energy (E a ), frequency factor (A), etc., by thermal activity monitor III (TAM III). This was done under three isothermal conditions of 70, 80, and 90 °C, with MEKPO 31 mass% combined with nitric acid (HNO3 6 N) and sodium nitrate (NaNO3 6 N). Nitric acid mixed with MEKPO gave the maximum heat of reaction (△H d ) and also induced serious reactions in the initial stage of exothermic process under the three isothermal temperatures. The time to maximum rate (TMR) also decreased when HNO3 was mixed with MEKPO. Thus, MEKPO combined with HNO3 6 N forms a very hazardous mixture. Results of this study will be provided to relevant plants for alerting their staff on adopting best practices in emergency response or accident control.

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High-performance liquid chromatography-mass spectrometry (HPLC-MS) method coupled with radical reaction for screening active ingredients from perennial fujimoto bean whole herb was established. The active ingredients, present in perennial fujimoto bean whole herb, possess scavenging effects towards 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical, superoxide, peroxy radical, and hydroxyl radical. The radical scavenging abilities of these active ingredients were evaluated based on the relative peak areas in the HPLC chromatogram. The results indicate that potent antioxidants are present in the anhydrous methanol extract of perennial fujimoto bean whole herb. Based on HPLC-MS analysis, it was found that the scavenging ability can be mostly attributed to the presence of three compounds: cyanidin-3-o-β-d-glucopyranoside, troxerutin, and rutin. The structures were identified based on the MS and nuclear magnetic resonance (NMR) data. Free radical scavenging activity decreased in the following order: troxerutin > rutin > cyanidin-3-o-β-d-glucopyranoside.

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