高效液相色谱-电感耦合等离子质谱分析烟草中硒形态

Speciation Analysis of Selenium in Tobacco by HPLC-ICP-MS

采用高效液相色谱-电感耦合等离子体质谱（HPLC-ICP-MS）联用技术建立了烟草中硒的形态分析方法。烟草样品采用0.10mol/L HCl超声提取30min,经离心、过膜后引入HPLC-ICP-MS进行分析。使用Hamilton PRP X-100阴离子交换柱,以20mmol/L柠檬酸水溶液为流动相（pH=7.0）,流速1.2mL/min,优化条件下实现了6种硒形态的分离。质谱采用He碰撞模式,硒代胱氨酸、亚硒酸根、甲基硒代半胱氨酸、硒酸根、硒脲、硒代蛋氨酸检出限分别为1.20、0.34、1.65、0.13、3.25和0.65ng/mL。该方法操作简单、快速、灵敏度高,精密度好,加标回收率在86.1%~95.8%之间,适用于烟草中硒元素形态分析。

A method of high performance liquid chromatography（HPLC） coupled with inductively coupled plasma-mass spectrometry（ICP-MS） was developed for the speciation of selenium in tobacco. By using Hamilton PRP X-100 anion-exchange column, the mobile phase composition, concentration, pH value and flow rate were optimized for the separation of target Se species. Under the optimized condition with collision cell technology, the detection limits of the proposed method for SeCys2, SeO32-, MeSeCys,SeO42-,SeUr and SeMet were 1. 20,0. 34, 1. 65,0. 13,3. 25 and 0. 65 ng/mL, respectively. Tobacco Samples were extracted by sonication with 0.10 mol/L HC1 solution for 30 min and the extracts were centrifuged and filtered before analyzed. The method was demonstrated to be a simple operation with high sensitivity and good precision for target Se species, and the recoveries were between 86.1%-95.8%, which promised a good application potential for Se speciation in tobacco.