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  • Author or Editor: L. Q. Zhang x
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Abstract  

Fingernails of pathologically diagnosed normal people, light esophageal epitheliosis patients, severe esophageal epitheliosis patients and esophageal cancer patients were irradiated and their elemental contents were determined by INAA. Multivariate statistical treatment of Ca, Cl, K. Mg, Se and Zn data shows that esophageal cancer patients are distinguishable from non-cancer patients. The accuracy computed by neural networks is greater than 80%.

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A reversed-phase high-performance liquid chromatographic method was developed for the first time to simultaneously determine salicin and eight flavonoids in leaves of Salix matsudana, that is salicin, luteolin-7-O-glucoside, myricetin, apigenin-3′-oxyethyl-7-O-glucoside, rutin, quercetin, luteolin, kaempferol and apigenin. The separation of these compounds was achieved on a reversed phase C18 column (250 × 4.6 mm, 5 μm), with linear gradient of methanol in 0.2% phosphoric acid solution with a flow rate of 1.0 mL/min with UV detection at 246 nm. The calibration curves for the determination of all analytes showed good linearity over the investigated ranges (r > 0.999). The % relative standard deviation (% RSD) values were less than 0.34%, and the recoveries were between 95.79% and 99.94%. The values of luteolin-7-O-glucoside, salicin, myricetin, apigenin-3′-oxyethyl-7-O-glucoside, rutin, quercetin, luteolin, kaempferol, and apigenin were 1.0 μg g−1, 20.0 μg g−1, 32.9 μg g−1, 2.0 μg g−1, 29.5 μg g−1, 6.0 μg g−1, 1.0 μg g−1, 3.5 μg g−1, and apigenin was not found in the sample. This developed method can be used for evaluating the quality of different plant materials.

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Abstract  

Soybean oil based polyols (5-OH polyol, 10-OH polyol and 15-OH polyol) were synthetised from epoxidized soybean oil. The melting peak of polyols and the relationship between melting peak and the number-average functionality of hydroxyl in polyols were investigated by differential scanning calorimetry (DSC). The thermal decomposition of polyols and some of their thermal properties by thermogravimetry (TG) and derivative thermogravimetry (DTG) were also studied. The thermal stability of polyols in a nitrogen atmosphere was very close hence they had a same baseplate of triglyceride for polyols. The extrapolated onset temperature of polyols in their thermal mass loss, first step had a decreasing order: 5-OH polyol>10-OH polyol>15-OH polyol due to the difficulty in forming multiple elements ring of them had the same order. The thermal behavior of polyols under non-isothermal conditions using Friedman’s differential isoconversional method with different heating rates indicated that the 5-OH polyol had the lowest activation energy in thermal decomposition amongst these polyols according to the same fractional mass loss because of the weakest intramolecular oligomerization. The 15-OH polyol was prior to reach the mass loss region because the six-member ring is more stable than the three-member ring from 10-OH polyol and more easily formed.

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A simple hydrolysis method has been developed for determination of phenylethanoid glycosides in Lamiophlomis rotata (L.R.). Different kinds of phenylethanoid glycosides were hydrolyzed in hydrochloric acid solution to produce corresponding phenethyl alcohols and cinnamic acids, mainly containing hydroxytyrosol, homovanillyl alcohol, 3,4-dimethoxyphenethyl alcohol, caffeic acid, fumalic acid and 3,4-dimethoxycinnamic acid. The six analytes could be determined simultaneously by high-performance liquid chromatography (HPLC). The effects of mobile phase, pH and concentration of running buffer, detection wavelength, flow rate and injection volume were also investigated. Under the optimum conditions, the six hydrolyzates could be perfectly separated within 45 min. The response was linear over four orders of magnitude with detection limits (S/N = 3) ranging from 1 × 10−8 to 1.5 × 10−4 mol L−1 for the analytes. The method has been successfully applied to the analysis of real sample Du-Yi-Wei capsule and Qi-Zheng-Yan-Tong patch, with satisfactory results.

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Summary  

Electronic stopping power of 19F in Ni, Pd and Gd was measured and compared to Mstar and SRIM calculation as well as experimental results published in literature. It turns out that the present electronic stopping power agrees reasonably well with them.

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Cleavage of glucosinolates with myrosinase yields thioglycosidic compounds which have cancer chemoprevention activity. In this paper, glucosinolates in an extract (2.0 g) of broccoli seeds (Brassica oleracea var. italica) were separated by high-speed countercurrent chromatography (HSCCC) with the solvent system n-butanol-acetonitrile-10% ammonium sulfate solution 1:0.5:2.2 (v/v) to yield five glucosinolate compounds after desalting and decolorizing by MCI column chromatography. The five compounds, 7-methylsulfinylheptyl glucosinolate (22.4 mg), 4-pentenyl glucosinolate (33.6 mg), 3-butenyl glucosinolate (24.0 mg), 4-methylsulfinylbutyl glucosinolate (161.4 mg), and 3-methylsulfinylpropyl glucosinolate (29.6 mg), were identified by ESI-MS, 1H NMR and 13C NMR. The purity of the products was >98%, and 7-methylsulfinylheptyl glucosinolate was obtained from broccoli seeds for the first time.

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Abstract  

The molar heat capacity, C p,m, of a complex of holmium chloride coordinated with L-aspartic acid, Ho(Asp)Cl2·6H2O, was measured from 80 to 397 K with an automated adiabatic calorimeter. The thermodynamic functions H T-H 298.15 and S T-S 298.15 were derived from 80 to 395 K with temperature interval of 5 K. The thermal stability of the complex was investigated by differential scanning calorimeter (DSC) and thermogravimetric (TG) technique, and the mechanism of thermal decomposing of the complex was determined based on the structure and the thermal analysis experiment.

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Abstract  

The heat capacities of 2-benzoylpyridine were measured with an automated adiabatic calorimeter over the temperature range from 80 to 340 K. The melting point, molar enthalpy, Δfus H m, and entropy, Δfus S m, of fusion of this compound were determined to be 316.49±0.04 K, 20.91±0.03 kJ mol–1 and 66.07±0.05 J mol–1 K–1, respectively. The purity of the compound was calculated to be 99.60 mol% by using the fractional melting technique. The thermodynamic functions (H TH 298.15) and (S TS 298.15) were calculated based on the heat capacity measurements in the temperature range of 80–340 K with an interval of 5 K. The thermal properties of the compound were further investigated by differential scanning calorimetry (DSC). From the DSC curve, the temperature corresponding to the maximum evaporation rate, the molar enthalpy and entropy of evaporation were determined to be 556.3±0.1 K, 51.3±0.2 kJ mol–1 and 92.2±0.4 J K–1 mol–1, respectively, under the experimental conditions.

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Summary

Rapid high-performance liquid chromatographic methods with evaporative light scattering detection (HPLC-ELSD) and electrospray ionization multistage mass spectrometry (HPLC-ESI-MSn) have been established and validated for simultaneous qualitative and quantitative analysis of eight steroidal saponins in ten batches of Gongxuening capsule (GXN), a widely commercially available traditional Chinese preparation. The optimum chromatographic conditions entailed use of a Kromasil C18 column with acetonitrile-water (30:70 to 62:38, υ/υ) as mobile phase at a flow rate of 1.0 mL min−1. The drift tube temperature of the ELSD was 102°C and the nebulizing gas flow rate was 2.8 L min−1. Separation was successfully achieved within 25 min. LC-ESI-MSn was used for unequivocal identification of the constituents of the samples by comparison with reference compounds. The assay was fully validated for precision, repeatability, accuracy, and stability, then successfully applied to quantification of the eight compounds in samples. The method could be effective for evaluation of the clinical safety and efficacy of GXN.

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