Universidade Federal de Alfenas (UNIFAL-MG), Instituto de Química, Rua Gabriel Monteiro da Silva, 714, CEP 37130-000 Alfenas, MG, Brazil.
Spectrochim Acta A Mol Biomol Spectrosc. 2014 Jan 3;117:304-8. doi: 10.1016/j.saa.2013.08.008. Epub 2013 Aug 11.
In this work a spectrophotometric flow injection analysis system for streptomycin determination in veterinary samples, is being proposed. The method is based on streptomycin alkaline hydrolysis that forms guanidine, followed by the reaction with Fe(II). The colored product has absorption peak at 520 nm. To evaluate and optimize the system parameters, chemometrics tools, such as factorial design, Pareto chart and Doelhert design, were used. The veterinary samples are diluted in water and introduced in the FIA system, therefore no sample preparation is required. The optimized system presented: linear range of 60 up to 1000 mg L(-1), limit of detection of 18 mg L(-1) and sampling rate of 36 readings per hour. The precision was checked and the CV for veterinary sample readings were always less than 6.5%. The accuracy was studied by comparison with chromatographic method, thus, five samples of pharmaceutical veterinary were determined by HPLC and by the proposed method, and the results are in agreement (t-test, p=0.05).
本工作提出了一种分光光度流动注射分析系统，用于兽医样品中链霉素的测定。该方法基于链霉素的碱性水解，生成胍，然后与 Fe(II)反应。生成的有色产物在 520nm 处有吸收峰。为了评估和优化系统参数，使用了化学计量学工具，如析因设计、Pareto 图和 Doelhert 设计。兽医样品在水中稀释后直接引入 FIA 系统，因此无需样品制备。优化后的系统具有以下特点：线性范围为 60 至 1000mg/L(-1)，检测限为 18mg/L(-1)，采样速率为 36 次/小时。对兽医样品读数的精密度进行了检查，CV 始终小于 6.5%。通过与色谱法进行比较研究了准确性，因此，用 HPLC 和所提出的方法测定了 5 个兽药样品，结果一致（t 检验，p=0.05）。
