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Studies of thermokinetics in an adiabatic calorimeter

I. Design and testing of an adiabatic automatic calorimeter

Journal of Thermal Analysis and Calorimetry
Authors: S. Zhan, J. Liu, Z. Qin, and Y. Deng

Abstract  

An adiabatic calorimeter in which automation of the control of the adiabatic condition and the thermogram recording is achieved in a simple way has been designed for studies of both thermochemistry and thermokinetics. A new method for specific heat measurements has been proposed and specific heats ofn-heptane were measured to test the reliability of this calorimeter.

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Abstract  

The transformation equation for the thermokinetics of consecutive first-order reactions has been deduced, and a thermokinetic research method of irreversible consecutive first-order reactions, which can be used to determine the rate constants of two steps simultaneously, is proposed. The method was validated and its theoretical basis was verified by the experimental results.

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Studies of thermokinetics in an adiabatic calorimeter

II. Calorimetric curve analysis methods for irreversible and reversible reactions

Journal of Thermal Analysis and Calorimetry
Authors: S. Zhan, J. Liu, Z. Qin, and Y. Deng
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Abstract  

Samarium-153-EDTMP (ethylene diamine tetramethylene phosphonate), for its promising biological properties, has been proved as a palliating therapeutic agent for boné cancer in human beings. In this article, we present the results on synthesis and structure analysis of Samarium-153-EDTMP. In a basic medium,153Sm-EDTMP can be readily prepared with a complexing yield not less than 98%, and it is confirmed that the ratio of the ligand to Sm is 11, and the charge of153Sm-EDTMP is negative two.

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Abstract  

The characterization of different sized TiO2 (25 nm, 80 nm, and 155 nm) was carried out by transmission electron microscopy (TEM) and the micro-distributions of TiO2 in the olfactory bulb of mice after nasal inhalation were investigated by microbeam SRXRF mapping techniques. The results show that TiO2 particles can be translocated to the olfactory bulb through the olfactory nerve system after inhalation. The distributions of Fe, Cu, and Zn in the olfactory bulb were also studied.

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A sensitive and simple liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS) method for determination of dasatinib in rat plasma using one-step protein precipitation was developed. After addition of carbamazepine as internal standard (IS), protein precipitation by acetonitrile was used as sample preparation. Chromatographic separation was achieved on an SB-C18 (2.1 mm × 150 mm, 5 μm) column with methanol-0.1% formic acid as mobile phase with gradient elution. Electrospray ionization (ESI) source was applied and operated in positive ion mode; selective ion monitoring (SIM) mode was used to quantification using target fragment ions m/z 488.2 for dasatinib and m/z 338.7 for the IS. Calibration plots were linear over the range of 10–1000 ng mL−1 for dasatinib in rat plasma. Lower limit of quantification (LLOQ) for dasatinib was 10 ng mL−1. Mean recovery of dasatinib from plasma was in the range 82.2%–93.6%. Relative standard deviation (RSD) of intra-day and inter-day precision were both less than 8%. This developed method is successfully used in pharmacokinetic study of dasatinib in rats.

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A rapid and sensitive ultraperformance liquid chromatography-multiple reaction monitoring-multi-stage/mass spectrometry (UPLC-MRM-MS/MS) method has been developed for simultaneous quantification of salvianolic acid B and tanshinone IIA of salvia tropolone tablets in dog plasma. This was achieved by performing quantification using the MRM acquisition with two channels of MRM-MS/MS and MS full scan for more accuracy qualitative results, and the fragmentation transitions of m/z 295→249, 191 for tanshinone IIA and m/z 297→279, 251 for IS in positive mode, m/z 717→519, 321 for salvianolic acid B and m/z 295→267, 239 for IS in negative mode were selected. The UPLC separation was achieved within 3 min in a single UPLC run. Linear calibration curves were obtained over the concentration range of 10 pg/mL−1 ng/mL for tanshinone IIA and 100 pg/mL−1 for salvianolic acid B. Lower limit of quantitation (LLOQ) was 10 pg/mL and 100 pg/mL for tanshinone IIA and salvianolic acid B, respectively. The inter-day and intra-day precision (relative standard deviation, RSD) in all samples were less than 8.21%, and the recoveries were over 85.9% for both tanshinone IIA and salvianolic acid B. The two channels of MRM with MS full scan approach could provide both qualitative and quantitative results without the need for repetitive analyses and resulted in the reduction of further confirmation experiments and analytical time. The pharmacokinetic study of the two active components of salvia tropolone tablets following oral gavage administration of dogs was thus explored with this method.

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