Jasna Jablan, Maja Bival Štefan, Dario Paler, Emma Kamenski
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Based on the results obtained, sample suspensions were prepared by weighing 10 mg of the sample and adding 1 mL of 5 % Triton X-100 with 10 mL Ga as internal standard and deposition volume was set at 10 mL. The results obtained with TXRF were comparable with those obtained with the FAAS method, indicating that this technique can be used instead of the conventional methods. Using the best analytical conditions, the limits of detection for trace elements were in the range of 0.2-0.6 mg kg<sup>-1</sup>. Trueness and precision of the results, evaluated by CRM sample analysis, were in most cases acceptable with recoveries values in the range of 104.9-111.4 % and relative standard deviations of 2-10 % (. = 6). 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引用次数: 0
摘要
沸石是一大类矿物,研究最多的是自然产生的斜沸石。它们具有抗炎、抗氧化和排毒的特性,这使它们具有药用价值。对沸石的组成进行元素分析是其精确化学表征的必要条件,本文提出了用全反射x射线荧光光谱法(TXRF)悬浮法测定锰、铁和锌的方法。采用基于响应面法的Box-Behnken设计确定最佳制样条件。选取样品数量、体积沉积和分散剂等重要变量作为关键变量。在此基础上,取10 mg样品称重,加入1 mL 5% Triton X-100,以10 mL Ga为内标,沉积体积为10 mL,制备样品悬浮液。TXRF法与火焰原子吸收光谱法所得结果相当,表明该技术可替代传统方法。在最佳分析条件下,样品中微量元素的检出限为0.2 ~ 0.6 mg kg-1。结果的准确性和精密度,通过CRM样品分析评估,在大多数情况下,回收率在104.9- 114%范围内,相对标准偏差为2- 10%()。= 6)。沸石对自由基没有抑制作用,对膳食抗氧化剂也没有影响。
Optimization of the suspension procedure by Box-Behnken design for the determination of manganese, iron, and zinc in zeolite clinoptilolite with the TXRF system and insight into its antioxidant properties.
Zeolites are a large family of minerals and the most studied is the naturally occurring clinoptilolite. They possess anti-inflammatory, antioxidant, and detoxifying properties which makes them valuable for medicinal use. Element analysis of zeolite's composition is necessary for its precise chemical characterization, and within this work development of a suspension method for the determination of manga nese, iron, and zinc by total reflection X-ray fluorescence spec-trometry (TXRF) was presented. The Box-Behnken design based on the response surface methodology was applied to determine the optimal sample preparation conditions. The significant variables such as sample amount, volume deposition, and dispersant were selected as critical variables. Based on the results obtained, sample suspensions were prepared by weighing 10 mg of the sample and adding 1 mL of 5 % Triton X-100 with 10 mL Ga as internal standard and deposition volume was set at 10 mL. The results obtained with TXRF were comparable with those obtained with the FAAS method, indicating that this technique can be used instead of the conventional methods. Using the best analytical conditions, the limits of detection for trace elements were in the range of 0.2-0.6 mg kg-1. Trueness and precision of the results, evaluated by CRM sample analysis, were in most cases acceptable with recoveries values in the range of 104.9-111.4 % and relative standard deviations of 2-10 % (. = 6). Zeolites showed no ability to quench free radicals nor the ability to influence dietary antioxidants.
期刊介绍:
AP is an international, multidisciplinary journal devoted to pharmaceutical and allied sciences and contains articles predominantly on core biomedical and health subjects. The aim of AP is to increase the impact of pharmaceutical research in academia, industry and laboratories. With strong emphasis on quality and originality, AP publishes reports from the discovery of a drug up to clinical practice. Topics covered are: analytics, biochemistry, biopharmaceutics, biotechnology, cell biology, cell cultures, clinical pharmacy, drug design, drug delivery, drug disposition, drug stability, gene technology, medicine (including diagnostics and therapy), medicinal chemistry, metabolism, molecular modeling, pharmacology (clinical and animal), peptide and protein chemistry, pharmacognosy, pharmacoepidemiology, pharmacoeconomics, pharmacodynamics and pharmacokinetics, protein design, radiopharmaceuticals, and toxicology.