Development and validation of UPLC‐MS/MS method for determination of domperidone in human plasma and its pharmacokinetic application

A sensitive, rapid and selective ultra‐performance liquid chromatography–tandem mass spectrometric (UPLC‐MS/MS) method was developed for the determination and pharmacokinetic study of domperidone in human plasma. Diphenhydramine was used as the internal standard. Plasma sample pretreatment involved a one‐step liquid–liquid extraction with a mixture of diethyl ether–dichloromethane (3:2, v/v). The analysis was carried out on an Acquity UPLC^TM BEH C₁₈ column. The mobile phase consisted of methanol–water containing 10 mmol/L ammonium acetate and 0.5% (v/v) formic acid (60:40, v/v). The detection was performed on a triple quadrupole tandem mass spectrometer in multiple reaction monitoring mode via electrospray ionizationsource with positive mode. Each plasma sample was chromatographed within 2.1 min. The standard curves for domperidone were linear (r² ≥ 0.99) over the concentration range of 0.030–31.5 ng/mL with a lower limit of quantification of 0.030 ng/mL. The intra‐ and inter‐day precision (relative standard deviation) values were not higher than 13% and accuracy (relative error) was from ?7.6 to 1.2% at three quality control levels. The method herein described was superior to previous methods and was successfully applied to the pharmacokinetic study of domperidone in healthy Chinese volunteers after oral administration. Copyright © 2012 John Wiley & Sons, Ltd.     

1,3-二羟基呫吨酮类化合物的简洁合成及清除亚硝酸根作用研究

以间苯三酚为起始原料,在伊顿试剂的催化作用下,与不同取代水杨酸反应合成1,3-二羟基呫吨酮类化合物3a~3l 12个,收率63%~87%,并探讨了反应机理及结构-反应活性关系.利用紫外分光光度法测定了所合成化合物对亚硝酸盐的清除作用,结果表明,在37℃、pH 3及反应时间为30 min条件下,1,3-呫吨酮类化合物对亚硝酸根均有较好的清除作用,其中化合物3f和3b的清除作用最强,清除率达34%.同时对1,3-二羟基呫吨酮类化合物清除亚硝酸盐的作用机制及构效关系进行了探讨.     

The removal of H2S derived from livestock farm on activated carbon modified by combinatory method of high-pressure hydrothermal method and impregnation method

H₂S is considered as the main gas pollutant from livestock farm and activated carbon (AC) is widely used as adsorbent for H₂S. This paper focuses on the influence of modification conditions and operation conditions on the H₂S adsorption performance on AC samples. The H₂S adsorption performance on modified AC (MAC) samples by single and combinatory method has been investigated. It is concluded that the MAC by combinatory method of high-pressure hydrothermal method followed by alkaline solution impregnation method could promote the H₂S adsorption performance remarkably. The H₂S adsorption performance differs with different operation conditions. Meanwhile the samples of fresh AC and exhausted AC have been characterized using BET, FTIR, TPD and Boehm titration method. The experimental results are confirmed that the characteristics of AC have significant influence on the adsorption ability for H₂S.