Warsaw University of Technology, Faculty of Chemistry, Department of Analytical Chemistry, ul. Noakowskiego 3, 00-664 Warsaw, Poland.
J Pharm Biomed Anal. 2013 Feb 23;74:268-72. doi: 10.1016/j.jpba.2012.11.011. Epub 2012 Nov 16.
Headspace solid phase microextraction (HSSPME) of chemically generated selenium hydride from alkaline solution followed by thermal desorption (TD) coupled directly to a microwave plasma (MWP) source has been examined for the optical emission spectrometric (OES) determination of Se. Various chemical and operating parameters including the NaBH(4) and HCl concentrations as well as the fiber exposure time and desorption temperature have been optimized. Alternatively, continuous hydride generation (HG) from alkaline medium and inductively coupled plasma (ICP) may be used for Se determination by OES. With the procedure developed, the determination of Se in dietary supplements at the tens of μgg(-1) level and an accuracy of 3-6% could be performed even in the presence of the 1000-fold excess of Fe and Cu. Additionally, Se was determined in the NIST 8418 material (Wheat gluten) with a certified concentration of Se of 2.58 ± 0.19 μgg(-1), and a value of 2.45 ± 0.25 μgg(-1) was found using HG-HSSPME-MWP-OES. The detection limit for Se (3.2 ng ml(-1)) with the proposed procedure was comparable to those obtained with HG-ICP-OES and the calibration curve was linear of about 2 orders of magnitude.
从碱性溶液中化学生成的硒化氢的顶空固相微萃取（HSSPME），随后进行热解吸（TD），直接与微波等离子体（MWP）源耦合，已被用于硒的光学发射光谱（OES）测定。已经优化了各种化学和操作参数，包括 NaBH（4）和 HCl 的浓度以及纤维暴露时间和解吸温度。或者，可以从碱性介质中连续进行氢化物生成（HG），并通过 OES 进行 Se 的测定。通过开发的程序，可以在存在 Fe 和 Cu 1000 倍过量的情况下，在数十 μg g（-1）水平上测定膳食补充剂中的 Se，准确度为 3-6%。此外，使用 HG-HSSPME-MWP-OES 在 NIST 8418 材料（小麦面筋）中测定了 Se，其 Se 的认证浓度为 2.58 ± 0.19 μg g（-1），发现值为 2.45 ± 0.25 μg g（-1）。与 HG-ICP-OES 相比，所提出的程序测定 Se 的检测限（3.2 ng ml（-1））相当，校准曲线的线性范围约为 2 个数量级。
