Authors:X. X. Liu, L. Wang, J. Yang, T. T. Zhang, X. D. Deng and Q. Wang
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.
Authors:S. Wang, Z. Tan, Y. Di, F. Xu, M. Wang, L. Sun and T. Zhang
As one primary component of Vitamin B3, nicotinic acid [pyridine 3-carboxylic acid] was synthesized, and calorimetric study and thermal analysis for this compound
were performed. The low-temperature heat capacity of nicotinic acid was measured with a precise automated adiabatic calorimeter
over the temperature rang from 79 to 368 K. No thermal anomaly or phase transition was observed in this temperature range.
A solid-to-solid transition at Ttrs=451.4 K, a solid-to-liquid transition at Tfus=509.1 K and a thermal decomposition at Td=538.8 K were found through the DSC and TG-DTG techniques. The molar enthalpies of these transitions were determined to be
ΔtrsHm=0.81 kJ mol-1, ΔfusHm=27.57 kJ mol-1 and ΔdHm=62.38 kJ mol-1, respectively, by the integrals of the peak areas of the DSC curves.
Thioacetamide (TAA) is a potent hepatotoxicant in acute and chronic hepatic injury. The study examined the protective effect of sesame oil against TAA-induced hepatic injury in rats. Hepatic injury was induced by intraperitoneal injection of 100 mg/kg of TAA for 24 h. Triple doses of sesame oil (1, 2, or 4 mL/kg) was given orally 0, 6, and 12 h after TAA treatment. TAA significantly increased serum aspartate aminotransferase (AST) and alanine aminotransferase (ALT) levels. Sesame oil decreased serum AST and ALT levels and significantly inhibited hepatic lipid peroxidation and nitric oxide levels compared with TAA-alone group. Further, sesame oil significantly inhibited TAA-induced hepatic neutrophil activation marker myeloperoxidase activity. However, sesame oil did not affect hepatic tumor necrosis factor, IL-1β and IL-10 generation in TAA-treated group. In conclusion, sesame oil protects against TAA-induced hepatic injury and oxidative stress via the inhibition of neutrophil activation. However, inflammatory cytokines may not be involved in sesame-oil-associated hepatic protection against TAA in rats.
Authors:L. Xiao, Y. Li, S. Wang, Z. Fang and G. Qiu
The principle for the electro-generative simultaneous leaching (EGSL) is applied to simultaneous leaching of pyrite-MnO2 in this paper. A galvanic system for the bio-electro-generative simultaneous leaching (BEGSL) has been set up. The equation
of electric quantity vs. time is used to study the effect of produced sulfur on electro-generative efficiency and quantity. It has been shown that
the resistance decreased in the presence of Acidithiobacillus thiooxidans (A. thiooxidans) with the increase of electro-generative efficiency. The effects of temperature and grain size on rate of ferrous extraction
from pyrite under the conditions of presence and absence of A. thiooxidans were studied, respectively. The changes in the extraction rate of Fe2+ as particle size in presence of A. thiooxidans were more evident than that in the absence, which indicated that the extraction in bio-electro-generative leaching was affected
by particle size remarkably. Around the optimum culture temperature for A. thiooxidans, the bigger change in the conversion rate of Fe2+ was depending on temperature. The transferred charge in BEGSL including part of S0 to sulfate group in the presence of (A. thiooxidans) which is called as biologic electric quantity, and the ratio of biologic electric quantity reached to 58.10% in 72 h among
the all-transferred charge.
In our invention, FCC (fluid catalytic cracking) dry gas could be used to react with benzene without any special purification, and more than 90% ethylene was converted to ethylbenzene. The phenomenon of carbon deposition over catalyst surface was obvious and leads to a deactivation of catalyst, so it is important to study the behavior of carbon deposition of catalyst during alkylation of benzene. The influence of several factors such as temperature, reaction time, reactant concentration of the amount and the kinetics of carbon deposition were investigated, during which carbon depositing rate equations were obtained for different reactant.
The combustion behavior of Shuangya Mountain (SYM) coal dust has been investigated by means of TG in this paper. The reaction fraction can be obtained from isothermal TG data. The regressions of g(), an integral function of
vs. t for different reaction mechanisms were performed. The mechanism of nucleation and nuclei growth is determined as the controlling step of the coal dust combustion reaction by the correlation coefficient of the regression, and the kinetic equation of the SYM coal dust combustion reaction has been established.
The effect of itaconic acid (IA) content and heating rate on the stabilization reactions in poly(acrylonitrile-co-itaconic
acid) (P(AN-co-IA)) was investigated by differential scanning calorimetry (DSC) with peak-resolving method. Increasing IA
content was effective in decreasing the initial temperature and the heat evolved, and found to enhance oxidative reactions
to some extent. While, promoting heating rate resulted in a shift of the exotherm to a higher temperature and a more rapid
liberation of heat. The percentage of area of the first exothermic peak increased with increasing heating rate, which would
be attributed to the enhancement of the free radical cyclization reactions.
Authors:W. Guan, L. Li, H. Wang, J. Tong and J. Yang
A brown and transparent ionic liquid (IL), [C4mim][FeCl4], was prepared by mixing anhydrous FeCl3 with 1-butyl-3-methylimidazolium chloride ([C4mim][Cl]), with molar ratio 1/1 under stirring in a glove box filled with dry argon. The molar enthalpies of solution, ΔsHm, of [C4mim][FeCl4], in water with various molalities were determined by a solution-reaction isoperibol calorimeter at 298.15 K. Considering
the hydrolyzation of anion [FeCl4]− in dissolution process of the IL, a new method of determining the standard molar enthalpy of solution, ΔsHm0, was put forward on the bases of Pitzer solution theory of mixed electrolytes. The values of ΔsHm0 and the sum of Pitzer parameters:
were obtained, respectively. In terms of thermodynamic cycle and the lattice energy of IL calculated by Glasser’s lattice
energy theory of ILs, the dissociation enthalpy of anion [FeCl4]−, ΔHdis≈5650 kJ mol−1, for the reaction: [FeCl4]−(g)→Fe3+(g)+4Cl−(g), was estimated. It is shown that large hydration enthalpies of ions have been compensated by large the dissociation enthalpy
of [FeCl4]− anion, ΔdHm, in dissolution process of the IL.
Synthesis, characterization and thermal analysis of polyaniline (PANI)/ZrO2 composite and PANI was reported in our early work. In this present, the kinetic analysis of decomposition process for these
two materials was performed under non-isothermal conditions. The activation energies were calculated through Friedman and
Ozawa-Flynn-Wall methods, and the possible kinetic model functions have been estimated through the multiple linear regression
method. The results show that the kinetic models for the decomposition process of PANI/ZrO2 composite and PANI are all D3, and the corresponding function is ƒ(α)=1.5(1−α)2/3[1−(1-α)1/3]−1. The correlated kinetic parameters are Ea=112.7±9.2 kJ mol−1, lnA=13.9 and Ea=81.8±5.6 kJ mol−1, lnA=8.8 for PANI/ZrO2 composite and PANI, respectively.
A simple and rapid method, using online ultraperformance liquid chromatography with photodiode array detection and electrospray ionization mass spectrometry (UPLC-PDA-eλ-ESI-MS/MS), was developed for the in-depth analysis of 50 batches Radix et Rhizoma Rhei. The analysis was performed on a UPLC BEH C18 column using a gradient elution system. Baseline separation could be achieved in less than 7.5 min. At the same time, on the basis of the 50 batches of samples collected from representative cultivated regions, a novel chromatographic fingerprint was devised by UPLC-PDA, in which 27 common peaks were detected and identified by the developed UPLC-MS/MS method step by step according to fragmentation mechanisms, MS/MS data, standards, and relevant literature. Many active components gave prominent [M - H]− ions in the ESI mass spectra. These components include anthraquinones, sennosides, stilbenes, glucose gallates, naphthalenes, and catechins. Furthermore, based on the information of these Radix et Rhizoma Rhei components, and further combined with discriminant analysis, a novel discriminant analysis equation (DAE) was established for the quality control of Radix et Rhizoma Rhei for the first time.