使用基于表面活性剂的原位固相萃取法测定药用植物输液中的低浓度 CrIII

Alêssa Gomes Siqueira, Bruno Elias dos Santos Costa, Lincoln Lucílio Romualdo, Vanessa Nunes Alves
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摘要

摘要 有人提出了一种新的固相萃取方法,即基于表面活性剂的原位固相萃取,用于检测药用植物输液中是否含有 CrIII。在这项工作中,将少量十六烷基三甲基溴化铵注入含有 1-(2-吡啶偶氮)-2-萘酚络合物的 CrIII 样品中。摇匀后,向溶液中加入少量 NaClO 作为离子配对剂。预浓缩后,将沉淀相溶解在一定体积的盐酸中,然后用火焰原子吸收光谱法进行分析。采用 Doehlert 矩阵优化 CrIII 复合物的形成条件,如螯合剂浓度(0.18 mmol L-1)和反应介质的 pH 值 9.5。采用 23 因子设计筛选影响萃取络合物的变量。离子配对剂的浓度(0.26 mol L-1)和涡旋搅拌器的搅拌时间(7.51 分钟)对萃取有显著影响,并采用响应面方法进行了优化。检出限、定量限和预浓缩因子分别为 1.66 μg L-1、5.5 μg L-1 和 12。线性范围为 5.5-5000 μg L-1。该方法与标准物质APS-1071比较(P>0.05),结果表明,该方法准确度高,优化后的条件成功地应用于药用植物输液样品中CrIII的测定。图表摘要
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Use of in-situ surfactant-based solid phase extraction for determination of low concentrations of CrIII in infusions of medicinal plants
Abstract A new solid phase extraction procedure, known as in situ surfactant-based solid phase extraction, has been proposed to detect the presence of CrIII in infusions of medicinal plants. In this work, a small amount of cetyltrimethylammonium bromide was injected into a sample containing CrIII, which was complexed by 1-(2-pyridylazo)-2-naphthol. After shaking, a small volume of NaClO Was added to the solution as an ion-pairing agent. After preconcentration, the settled phase was dissolved in a specific volume of HCl and then analyzed by Flame Atomic Absorption Spectrometry. A Doehlert matrix was used to optimize the CrIII complex formation conditions, such as the chelating agent concentration (0.18 mmol L-1) and pH of 9.5 in the reaction medium. A 23 factorial design was used to screen the variables that influence the extraction of the complex. The concentration of ionic-pairing agent (0.26 mol L-1) and the vortex mixer agitation time (7.51 minutes) were significant and optimized using response surface methodology. The limit of detection, limit of quantification, and preconcentration factor were 1.66 μg L-1, 5.5 μg L-1 and 12, respectively. The linear range was 5.5-5000 μg L-1. The method proved accuracy by the comparison with certified reference material APS-1071 (p>0.05), and the optimized conditions were successfully applied for the determination of CrIII in samples of medicinal plant infusions. GRAPHICAL ABSTRACT
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