Tokay Feyzullah, Bağdat Sema
Department of Chemistry, Faculty of Science and Arts, Balıkesir University, Balıkesir, Turkey.
Turk J Chem. 2021 Dec 6;46(2):459-474. doi: 10.3906/kim-2109-11. eCollection 2022.
A method for separation and preconcentration of Cu(II), Ni(II), and Cd(II) using N-N'-bis(5-methoxsalicylidene)-2-hydroxy-1,3-propanediamine modified silica gel was improved for aqueous samples and pharmaceuticals. Determination of the analytes was achieved by inductively coupled plasma optic emission spectrometry. The experimental conditions including pH value, sample volume, eluent type and volume, sorbent mass, sample, and eluent flow rates were optimized with univariate and multivariate optimization tools. The relative standard deviations of the method were 2.9% for Cu(II), 3.0% for Ni(II), and 3.3% for Cd(II) with recovery values between 98.8 ± 3.2-101.5 ± 3.0%. The limits of detection were found to be 62.4, 39.5, and 28.2 ng L for Cu(II), Ni(II), and Cd(II), respectively. The accuracy of the suggested procedure was tested with the certified reference material (Certipur ICP multi-element standard solution IV) and addition-recovery experiments. The method was successfully applied to eye drop, anesthetic, serum, tap water, mineral water, and spring water samples.
一种使用N - N'-双(5 - 甲氧基水杨醛)-2 - 羟基-1,3 - 丙二胺修饰硅胶对水样和药物中铜(II)、镍(II)和镉(II)进行分离和预富集的方法得到了改进。通过电感耦合等离子体光发射光谱法测定分析物。利用单变量和多变量优化工具对包括pH值、样品体积、洗脱剂类型和体积、吸附剂质量、样品及洗脱剂流速在内的实验条件进行了优化。该方法的相对标准偏差分别为:铜(II)为2.9%,镍(II)为3.0%,镉(II)为3.3%,回收率在98.8 ± 3.2 - 101.5 ± 3.0%之间。发现铜(II)、镍(II)和镉(II)的检测限分别为62.4、39.5和28.2 ng/L。使用有证标准物质(Certipur ICP多元素标准溶液IV)和加标回收实验对所建议方法的准确性进行了测试。该方法成功应用于眼药水、麻醉剂、血清、自来水、矿泉水和泉水样品的分析。