A simple and sensitive method of high-performance liquid chromatography with fluorescence detection (HPLC-FLD) was developed for the determination of icariin in capsules by precolumn chelation with aluminum. In order to obtain a stable fluorescence signal, the reaction conditions of the fluorescent chelation complex between icariin and aluminum were investigated in detail. Chromatography was carried out on an Agilent Zorbax Extend C18 column (150 mm × 4.6 mm, 5.0 μm) using methanol as mobile phase at a flow rate of 1.0 mL min−1. The excitation and emission wavelengths were set at 430 and 480 nm, respectively. At optimum conditions, the calibration curve was linear in the concentration range from 0.010 to 100.0 μg mL−1 with the limit of detection of 3.5 ng mL−1 (S/N = 3). A comprehensive method was validated for precision and accuracy. The method described here has been successfully applied for the determination of the icariin content in a capsule with satisfactory results.
Authors:L. Chen, W. Song, J. Lv, L. Wang, and C. Xie
Aluminum (Al) nanopowders with mean diameter of about 50 nm and passivated by alumina (Al2O3) coatings were prepared by an evaporation route: laser heating evaporation. Thermal properties of the nanopowders were investigated
by simultaneous thermogravimetric-differential thermal analysis (TG-DTA) in dry oxygen environment, using a series of heating
rates (5, 10, 20, 30, 50 and 90°C min−1) from room temperature to 1200°C. With the heating rates rise, the onset and peak temperatures of the oxidation rise, and
the conversion degree of Al to Al2O3 varies. However, the specific heat release keeps relatively invariant and has an average value of 18.1 kJ g−1. So the specific heat release is the intrinsic characteristic of Al nanopowders, which can represent the ability of energy
Authors:Z. Zhang, L. Sun, Z. Tan, F. Xu, X. Lv, J. Zeng, and Y. Sawada
The molar heat capacities of the room temperature ionic liquid 1-butylpyridinium tetrafluoroborate (BPBF4) were measured by an adiabatic calorimeter in temperature range from 80 to 390 K. The dependence of the molar heat capacity
on temperature is given as a function of the reduced temperature X by polynomial equations, Cp,m [J K−1 mol−1]=181.43+51.297X −4.7816X2−1.9734X3+8.1048X4+11.108X5 [X=(T−135)/55] for the solid phase (80–190 K), Cp,m [J K−1 mol−1]= 349.96+25.106X+9.1320X2+19.368X3+2.23X4−8.8201X5 [X=(T−225)/27] for the glass state (198–252 K), and Cp,m[J K−1 mol−1]= 402.40+21.982X−3.0304X2+3.6514X3+3.4585X4 [X=(T−338)/52] for the liquid phase (286–390 K), respectively. According to the polynomial equations and thermodynamic relationship,
the values of thermodynamic function of the BPBF4 relative to 298.15 K were calculated in temperature range from 80 to 390 K with an interval of 5 K. The glass transition
of BPBF4 was observed at 194.09 K, the enthalpy and entropy of the glass transition were determined to be ΔHg=2.157 kJ mol−1 and ΔSg=11.12 J K−1 mol−1, respectively. The result showed that the melting point of the BPBF4 is 279.79 K, the enthalpy and entropy of phase transition were calculated to be ΔHm = 8.453 kJ mol−1 and ΔSm=30.21 J K−1 mol−1. Using oxygen-bomb combustion calorimeter, the molar enthalpy of combustion of BPBF4 was determined to be ΔcHm0 = −5451±3 kJ mol−1. The standard molar enthalpy of formation of BPBF4 was evaluated to be ΔfHm0 = −1356.3±0.8 kJ mol−1 at T=298.150±0.001 K.
Authors:Y. Wang, L. Yin, G. Lv, Y. Xu, L. Xu, Y. Qi, L. Zheng, and J. Peng
In the present paper, a simple and reliable high-performance liquid chromatography-diode array detection (HPLC-DAD) method was developed both for quantitative determination and fingerprint analysis of Agrimonia pilosa Ledeb for quality control. Under the optimized HPLC conditions, seven bioactive compounds including rutin, quercetin-3-rhamnoside, luteoloside, tiliroside, apigenin, kaempferol, and agrimonolide were determined simultaneously. For fingerprint analysis, 11 common peaks were selected as the characteristic peaks to evaluate the similarities of 16 different samples collected from different origins in China. Besides, hierarchical cluster analysis (HCA) was also performed to evaluate the variation of the raw materials. This is the first report of using a simple method for quality control of A. pilosa Ledeb through multi-component determination and chromatographic fingerprint analysis to the best of our knowledge.
Authors:B. Liu, X. Lv, Z. Tan, Z. Zhang, Q. Shi, L. Yang, J. Xing, L. Sun, and T. Zhang
The molar heat capacity, Cp,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 HT-H298.15 and ST-S298.15 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.
Authors:J. Zhang, Y. Liu, Z. Zhang, X. Lv, L. Sun, F. Xu, Z. Tan, T. Zhang, and Y. Sawada
As one 3-D coordination polymer, lead formate was synthesized; calorimetric study and thermal analysis for this compound were
performed. The low-temperature heat capacity of lead formate was measured by a precise automated adiabatic calorimeter over
the temperature range from 80 to 380 K. No thermal anomaly or phase transition was observed in this temperature range. A four-step
sequential thermal decomposition mechanism for the lead formate was found through the DSC and TG-DTG techniques at the temperature
range from 500 to 635 K.
Authors:X.-C. Lv, Z.-C. Tan, Z.-A. Li, Y.-S. Li, J. Xing, Q. Shi, and L.-X. Sun
The (R)-BINOL-menthyl dicarbonates,
one of the most important compounds in catalytic asymmetric synthesis, was
synthesized by a convenient method. The molar heat capacities Cp,m
of the compound were measured over the temperature range from 80 to 378 K
with a small sample automated adiabatic calorimeter. Thermodynamic functions
[HT–H298.15] and [ST–S298.15] were derived in the
above temperature range with a temperature interval of 5 K. The thermal stability
of the substance was investigated by differential scanning calorimeter (DSC)
and a thermogravimetric (TG) technique.
Two lines, L-19-613 and L-19-626, were produced from the common wheat cultivar Longmai 19 (L-19) by six consecutive backcrosses using biochemical marker-assisted selection. L-19 (Glu-D1a, Glu-A3c/Gli-A1?; Gli-A1? is a gene coding for unnamed gliadin) and L-19-613 (Glu-D1d, Glu-A3c/Gli-A1?) formed a set of near-isogenic lines (NILs) for HMW-GS, while L-19-613 and L-19-626 (Glu-D1d, Glu-A3e/Gli-A1m) constituted another set of NILs for the LMW-GS/gliadins. The three L-19 NILs were grown in the wheat breeding nursery in 2007 and 2008. The field experiments were designed using the three-column contrast arrangement method with four replicates. The three lines were ranked as follows for measurements of gluten strength, which was determined by the gluten index, Zeleny sedimentation, the stability and breakdown time of the farinogram, the maximum resistance and area of the extensogram, and the P andWvalues of the alveogram: L-19-613 > L-19-626 > L-19. The parameters listed above were significantly different between lines at the 0.05 or 0.01 level. The Glu-D1 and Glu-A3/Gli-A1 loci had additive effects on the gluten index, Zeleny sedimentation, stability, breakdown time, maximum resistance, area, P and W values. Although genetic variation at the Glu-A3/Gli-A1 locus had a great influence on wheat quality, the genetic difference between Glu-D1d and Glu-D1a at the Glu-D1 locus was much larger than that of Glu-A3c/Gli-A1? and Glu-A3e/Gli-A1m at the Glu-A3/Gli-A1 locus. Glu-D1d had negative effects on the extensibility and the L value compared with Glu-D1a. In contrast, Glu-A3c/Gli-A1? had a positive effect on these traits compared with Glu-A3e/Gli-A1m.