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Journal of Thermal Analysis and Calorimetry
Authors: L. Xu, Y. De-Jun, L. Qiang-Guo, L. Ai-Tao, Y. Li-Juan, J. Qian-Hong, and L. Yi

Abstract  

The product from reaction of samarium chloride hexahydrate with salicylic acid and Thioproline, [Sm(C7H5O3)2·(C4H6NO2S)]·2H2O, was synthesized and characterized by IR, elemental analysis, molar conductance, and thermogravimetric analysis. The standard molar enthalpies of solution of [SmCl3·6H2O(s)], [2C7H6O3(s)], [C4H7NO2S(s)] and [Sm(C7H5O3)2·(C4H7NO2S)·H2O(s)] in a mixed solvent of absolute ethyl alcohol, dimethyl sulfoxide(DMSO) and 3 mol L−1 HCl were determined by calorimetry to be Δs H m Φ[SmCl3 δ6H2O (s), 298.15 K]= −46.68±0.15 kJ mol−1 Δs H m Φ[2C7H6O3 (s), 298.15 K]= 25.19±0.02 kJ mol−1, Δs H m Φ[C4H7NO2S (s), 298.15 K]=16.20±0.17 kJ mol−1 and Δs H m Φ[Sm(C7H5O3)2·(C4H6NO2S)]·2H2O (s), 298.15 K]= −81.24±0.67 kJ mol−1. The enthalpy change of the reaction

\documentclass{aastex} \usepackage{amsbsy} \usepackage{amsfonts} \usepackage{amssymb} \usepackage{bm} \usepackage{mathrsfs} \usepackage{pifont} \usepackage{stmaryrd} \usepackage{textcomp} \usepackage{upgreek} \usepackage{portland,xspace} \usepackage{amsmath,amsxtra} \pagestyle{empty} \DeclareMathSizes{10}{9}{7}{6} \begin{document} $$SmCl_3 \cdot 6H_2 O(s) + 2C_7 H_6 O_3 (s) + C_4 H_7 NO_2 S(s) = Sm(C_7 H_5 O_3 )_2 \cdot (C_4 H_6 NO_2 S) \cdot 2H_2 O(s) + 3HCl(g) + 4H_2 O(1)$$ \end{document}
((1)) was determined to be Δs H m Φ =123.45±0.71 kJ mol−1. From date in the literature, through Hess’ law, the standard molar enthalpy of formation of Sm(C7H5O3)2(C4H6NO2S)δ2H2O(s) was estimated to be Δs H m Φ[Sm(C7H5O3)2·(C4H6NO2S)]·2H2O(s), 298.15 K]= −2912.03±3.10 kJ mol−1.

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Acta Chromatographica
Authors: Hao-ran Dai, Ya-hui Hu, Jia-yi Long, Ying Xia, Hong-li Guo, Jing Xu, Xuan-sheng Ding, Jing Chen, Xiao-peng Lu, and Feng Chen

Abstract

Perampanel (PER) is the first clinically available selective antagonist of α-amino-3-hydroxy-5-methylisoxazole-4-propionic acid (AMPA) receptor approved globally for the treatment of epilepsy. Studies have recently underlined the significant association between dose-exposure-effect-adverse events of PER in patients with epilepsy, so the therapeutic drug monitoring (TDM) of PER is critical in clinical practices, especially for pediatric patients with drug-resistant epilepsy. Due to several limits in previous published analytical methods, herein, we describe the development and validation of a novel liquid chromatography tandem mass spectrometry (LC-MS/MS) method for monitoring PER in human plasma samples. Protein precipitation method by acetonitrile containing PER-d5 as internal standard was applied for the sample clean-up. Formic acid (FA, 0.2 mM) in both aqueous water and acetonitrile were used as the mobile phases and the analyte was separated by an isocratic elution. Qualification and quantification were performed under positive electrospray ionization (ESI) mode using the m/z 350.3 → 219.1 and 355.3 → 220.0 ions pairs transitions for PER and PER-d5, respectively. Potential co-medicated anti-seizure medications (ASMs) have no interference to the analysis. Calibration curves were linear in the concentration range of 1.00–2,000 ng mL−1 for PER. The intra- and inter-batch precision, accuracy, recovery, dilution integrity, and stability of the method were all within the acceptable criteria and no matrix effect or carryover was found. This method was then successfully implemented on the TDM of PER in Chinese children with drug-resistant epilepsy. We firstly confirmed the apparent inter- and intra-individual PER concentration variabilities and potential drug-drug interactions between PER and several concomitant ASMs occurred in Chinese pediatric patients, which were also in line with previous studies in patients of other race.

Open access