National Institute of Science and Technology for Bioanalytics and Spectrometry, Sample Preparation and Mechanization Group (GEPAM), Institute of Chemistry - University of Campinas (UNICAMP), P.O. Box 6154, 13083-970 Campinas, SP, Brazil.
Analyst. 2012 Aug 21;137(16):3841-6. doi: 10.1039/c2an35598a. Epub 2012 Jul 3.
A solid-phase micro-extraction (SPME) method using an SPME fiber device and graphite furnace (GF) for extracting Se compounds was proposed. Various factors affecting the derivatization and extraction of Se(IV) by SPME-GF were evaluated, including the effect of acid (type and concentration), the concentration of the derivatizing agent, the derivatization temperature, the extraction and derivatization times and the extraction temperature. After optimizing these conditions, the quantification of Se(IV) was performed by Gas Chromatography-Mass Spectrometry (GC-MS). The limit of detection was 0.37 μg L(-1) for Se(IV). The method was successfully applied to the total Se determination in certified reference materials (BCR-414 and SRM 1643e). A recovery of 97% was obtained for water (SRM 1643e). After microwave oven decomposition and the reduction of selenium using a mixture of 2 mol L(-1) HCl and 1% (w/v) KBr, a recovery of 101% and a relative standard deviation of 3.5% were attained for plankton (BCR-414). The SPME-GF method combined with GC-MS was also applied to the determination of the total selenium in a drug sample (selenium chelate).
提出了一种使用固相微萃取（SPME）纤维装置和石墨炉（GF）萃取硒化合物的 SPME-GF 方法。评估了各种因素对 SPME-GF 中硒（IV）衍生和萃取的影响，包括酸的类型和浓度、衍生剂浓度、衍生化温度、萃取和衍生化时间以及萃取温度的影响。优化这些条件后，通过气相色谱-质谱法（GC-MS）对 Se(IV)进行定量。Se(IV)的检测限为 0.37 μg L(-1)。该方法成功应用于认证参考物质（BCR-414 和 SRM 1643e）中总硒的测定。对于水（SRM 1643e），回收率为 97%。在使用 2 mol L(-1) HCl 和 1%（w/v）KBr 的混合物微波消解和还原硒后，对于浮游生物（BCR-414），回收率为 101%，相对标准偏差为 3.5%。SPME-GF 方法结合 GC-MS 还应用于药物样品（硒螯合物）中总硒的测定。
