Nóbrega J A, Lopes G S
Grupo de Química Analítica, Departamento de Química, Universidade Federal de São Carlos, São Carlos. SP, Brazil.
Talanta. 1996 Jun;43(6):971-6. doi: 10.1016/0039-9140(95)01830-1.
A lot of modern analytical strategies for exploiting chemistries have been developed by using flow-injection analysis. However, even after 20 years of flow-injection evolution, there still are new quantitative procedures being established using old qualitative assays. The formation of Prussian Blue is a classical test to detect Fe(2+) using hexacyanoferrate(III) as a precipitating reagent. This reaction was evaluated for spectrophotometric determination of ascorbic acid employing Fe(3+) and hexacyanoferrate(III) as chromogenic reagents. An excess of the complexing anion avoids the formation of precipitate and forms a deep blue solution when Fe(3+) is reduced to Fe(2+) by ascorbic acid. The maximum absorbance of the colored complex occurs at 700 nm and the molar absorptivity is 3.0 x 10(4) 1 mol(-1) cm(-1). Under flow-injection conditions the Prussian Blue reaction was employed with an intermittent flow of an oxalate alkaline solution for removing the colored product adsorbed on tube and flow-cell walls. Reference solutions containing 5.0 x 10(-6)-1.0 x 10(-4) M of ascorbic acid were employed to obtain the analytical curve (r = 0.9999). For all solutions the relative standard deviation was lower than 1.0% (n=10). Results obtained for ascorbic acid determination in pharmaceutical products (Cewin, Redoxon and Cebion) are in good agreement with those obtained by using a flow-injection procedure involving the reaction between triiodide and ascorbic acid. The sampling frequency is 140 h(-1) and only 430 microl of reagents is consumed in each determination.
许多利用化学原理的现代分析策略是通过流动注射分析开发出来的。然而,即使经过20年的流动注射技术发展,仍有新的定量方法是基于旧的定性分析建立的。普鲁士蓝的形成是一种经典测试,使用铁氰酸盐(III)作为沉淀剂来检测Fe(2+)。该反应被评估用于以Fe(3+)和铁氰酸盐(III)作为显色剂分光光度法测定抗坏血酸。过量的络合阴离子可避免沉淀的形成,当Fe(3+)被抗坏血酸还原为Fe(2+)时会形成深蓝色溶液。有色络合物的最大吸收波长在700 nm处,摩尔吸光系数为3.0×10(4) 1 mol(-1) cm(-1)。在流动注射条件下,普鲁士蓝反应与草酸碱溶液的间歇流动一起使用,以去除吸附在管道和流通池壁上的有色产物。使用含有5.0×10(-6)-1.0×10(-4) M抗坏血酸的参考溶液来获得分析曲线(r = 0.9999)。对于所有溶液,相对标准偏差低于1.0%(n = 10)。在药品(Cewin、Redoxon和Cebion)中抗坏血酸测定的结果与使用涉及碘化物和抗坏血酸反应的流动注射程序获得的结果高度一致。采样频率为140 h(-1),每次测定仅消耗430微升试剂。