Gallignani M, Ayala C, Brunetto M R, Burguera M, Burguera J L
Venezuelan Andean Institute for Chemical Research, Faculty of Science, University of Los Andes, Merida, Venezuela.
Talanta. 2003 Apr 10;59(5):923-34. doi: 10.1016/S0039-9140(02)00648-3.
In this work, a flow analysis system with hydride generation and Fourier transform infrared (FTIR) spectrometric detection has been developed for the determination of antimony in pharmaceuticals. The method is based on the on-line mineralization/oxidation of the organic antimonials present in the sample and pre-reduction of Sb(V) to Sb(III) with K(2)S(2)O(8) and KI, respectively; prior to the stibine generation. The gaseous SbH(3) is separated from the solution in a gas phase separator, and transported by means of a nitrogen carrier into a short pathway (10 cm) IR gas cell, where the corresponding FTIR spectrum is acquired by accumulating 3 scans in a continuous mode. The 1893 cm(-1) band was used for the quantification of the antimony. The procedure is carried out in a closed system, which reduces sample handling and makes possible the complete automation of the antimony determination. The figures of merit of the proposed method (linear range: 0-600 mg l(-1), limit of detection (3sigma)=0.9 mg l(-1), limit of quantification (10sigma)=3 mg Sb l(-1), precision (R.S.D.) less than 1% and sample frequency=28 h(-1)), are appropriate for the designed application. Furthermore, precise and accurate results were found for the analysis of different antimonial pharmaceutical samples, indicating that the methodology developed represents a valid alternative for the determination of antimony in pharmaceuticals, which could be suitable for the routine control analysis.
在本研究中，开发了一种具有氢化物发生和傅里叶变换红外（FTIR）光谱检测功能的流动分析系统，用于测定药物中的锑。该方法基于样品中有机锑的在线矿化/氧化，以及分别用K₂S₂O₈和KI将Sb(V)预还原为Sb(III)；在生成锑化氢之前进行。气态SbH₃在气相分离器中与溶液分离，并通过氮气载气输送到短程（10 cm）红外气室中，在此以连续模式累积扫描3次获取相应的FTIR光谱。利用1893 cm⁻¹处的谱带对锑进行定量。该分析过程在封闭系统中进行，减少了样品处理量，并使锑的测定完全自动化成为可能。所提出方法的性能指标（线性范围：0 - 600 mg l⁻¹，检测限(3σ)=0.9 mg l⁻¹，定量限(10σ)=3 mg Sb l⁻¹，精密度（相对标准偏差）小于1%，进样频率=28 h⁻¹）适用于设计的应用。此外，对不同含锑药物样品的分析得到了精确准确的结果，表明所开发的方法是药物中锑测定的有效替代方法，适用于常规控制分析。
