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在水相和二甲基亚砜/水溶液中使用阳极溶出伏安法直接测定药物成分中的镉和铅。

Direct determination of cadmium and lead in pharmaceutical ingredients using anodic stripping voltammetry in aqueous and DMSO/water solutions.

作者信息

Rosolina Samuel M, Chambers James Q, Lee Carlos W, Xue Zi-Ling

机构信息

Department of Chemistry, University of Tennessee, Knoxville, TN 37996, USA.

Pfizer, Inc., Analytical Research and Development, PharmaTherapeutics Pharmaceutical Sciences, Groton, CT 06340, USA.

出版信息

Anal Chim Acta. 2015 Sep 17;893:25-33. doi: 10.1016/j.aca.2015.07.010. Epub 2015 Aug 8.

Abstract

A new electrochemical method has been developed to detect and quantify the elemental impurities, cadmium(II) (Cd(2+)) and lead(II) (Pb(2+)), either simultaneously or individually in pharmaceutical matrices. The electro-analytical approach, involving the use of anodic stripping voltammetry (ASV) on an unmodified glassy carbon electrode, was performed in both aqueous and in a 95/5 dimethyl sulfoxide (DMSO)/water solutions, without acid digestion or dry ashing to remove organic matrices. Limits of detection (LODs) in the μg L(-1) [or parts per billion (ppb), mass/volume] range were obtained for both heavy metals - in the presence and absence of representative pharmaceutical components. To the best of our knowledge, the work demonstrates the first analysis of heavy metals in DMSO/water solutions through ASV. The strong reproducibility and stability of the sensing platform, as well as obviation of sample pretreatment show the promise of utilizing ASV as a sensitive, robust, and inexpensive alternative to inductively-coupled-plasma (ICP)-based approaches for the analysis of elemental impurities in, e.g., pharmaceutical-related matrices.

摘要

一种新的电化学方法已被开发出来,用于检测和定量药物基质中镉(II)(Cd(2+))和铅(II)(Pb(2+))这两种元素杂质,可同时或单独检测。该电分析方法采用未修饰的玻碳电极上的阳极溶出伏安法(ASV),在水溶液以及95/5的二甲基亚砜(DMSO)/水溶液中进行,无需酸消解或干法灰化来去除有机基质。在有代表性药物成分存在和不存在的情况下,两种重金属均获得了微克每升[或十亿分之一(ppb),质量/体积]范围内的检测限(LOD)。据我们所知,这项工作首次通过ASV对DMSO/水溶液中的重金属进行了分析。传感平台的强重现性和稳定性,以及无需样品预处理,表明利用ASV作为一种灵敏、稳健且廉价的替代方法,可用于分析例如药物相关基质中的元素杂质,以替代基于电感耦合等离子体(ICP)的方法。

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