建立并验证了一种通过示差脉冲极谱法选择性测定辛酸亚锡中锡形态的定量方法。

Development and validation of a quantitative method for the selective determination of tin species in tin octoate by differential pulse polarography.

机构信息

Laboratory of Analytical Chemistry, CIRM, Department of Pharmacy, University of Liège, Avenue de l'Hôpital 1, B36, 4000 Liège, Belgium.

出版信息

Talanta. 2010 Jan 15;80(3):1413-20. doi: 10.1016/j.talanta.2009.09.045.

DOI:10.1016/j.talanta.2009.09.045

PMID:20006107

Abstract

Tin octoate is used as a catalyst in the synthesis of polydimethylsiloxane (PDMS), a room temperature vulcanizing (RTV) silicone rubber. This rubber is largely used in the medical field due to its great biocompatibility. In this framework, a high-speed and costless analytical method for the determination of stannic ions, Sn(IV), in the presence of stannous ions, Sn(II), has been developed. The separation of these two ions was carried out using differential pulse polarography (DPP). For this purpose, the tin species contents in the catalyst is quantitatively extracted under inert condition to avoid any changes in the ratio Sn(IV)/Sn(II). Polarography showed well-shaped oxidation and reduction peaks respectively at -650 and -860mV for stannous ions. The peak of the stannic ion was well separated and appeared at -1210mV. Many parameters such as extraction process, extraction time, pH, chelating agents and polarographic conditions were optimized. We have also demonstrated that no oxidation of the stannous ions occurred during the sample preparation. The dosing range considered in this study extends between 10 and 40mug/mL, corresponding to 6.8% and 27.2% of the degradation product (Sn(IV)) in the catalyst, regarding to the sampling. Finally this method was successfully validated using the total error concept.

摘要

辛酸亚锡被用作合成聚二甲基硅氧烷（PDMS）的催化剂，PDMS 是一种室温硫化（RTV）硅橡胶。由于其良好的生物相容性，这种橡胶在医学领域得到了广泛应用。在这种情况下，开发了一种在存在亚锡离子（Sn(II)）的情况下测定四价锡离子（Sn(IV)）的高速、无成本分析方法。使用差分脉冲极谱法（DPP）对这两种离子进行分离。为此，在惰性条件下定量提取催化剂中的锡物质含量，以避免 Sn(IV)/Sn(II) 比例发生任何变化。极谱法分别在-650 和-860mV 处对亚锡离子显示出良好的氧化和还原峰。锡离子的峰得到了很好的分离，出现在-1210mV。优化了许多参数，如萃取过程、萃取时间、pH 值、螯合剂和极谱条件。我们还证明了在样品制备过程中不会发生亚锡离子的氧化。本研究考虑的剂量范围在 10 至 40μg/mL 之间，对应于催化剂中降解产物（Sn(IV)）的 6.8%至 27.2%，采样量为 6.8%至 27.2%。最后，使用总误差概念成功验证了该方法。