Department of Chemistry, Pharmaceutical Sciences Branch, Islamic Azad University, Tehran, Iran.
J Chromatogr A. 2012 Oct 5;1258:16-20. doi: 10.1016/j.chroma.2012.08.027. Epub 2012 Aug 15.
A novel and efficient speciation method based on the nano-structured lead dioxide as stationary phase of head space solid phase microextraction combined with gas chromatography mass spectrometry (GC-MS) was developed for the determination of volatile organoselenium compounds (dimethylselenide (DMSe) and dimethyldiselenide (DMDSe)) in different biological and environmental samples. PbO(2) particles with a diameter in the range of 50-70 nm have been grown on platinum wire via elechtrochemical deposition. The effect of different variables on the extraction efficiency was studied simultaneously using an experimental design. The variables of interest in the HS-SPME were condition of coating preparation, desorption time, stirring rate, desorption temperature, ionic strength, time and temperature of extraction. A Plackett-Burman design was performed for screening in order to determine the significant variables affecting the extraction efficiency. Then, the significant factors were optimized by a Box-Behnken design (BBD) and the response surface equations were derived. The detection limit and relative standard deviation (RSD) (n=5, c=50 μgL(-1)) for DMSe were 16 ngL(-1) and 4.3%, respectively. They were also obtained for DMDSe as 11ngL(-1) and 4.6%, respectively. The developed technique was found to be applicable to spiked environmental and biological samples.
一种基于纳米结构二氧化铅作为顶空固相微萃取固定相，结合气相色谱-质谱联用（GC-MS）的新型、高效形态分析方法，用于测定不同生物和环境样品中的挥发性有机硒化合物（二甲基硒（DMSe）和二甲基二硒（DMDSe））。通过电化学沉积在铂丝上生长出直径在 50-70nm 范围内的 PbO2 颗粒。同时使用实验设计研究了不同变量对萃取效率的影响。HS-SPME 中的感兴趣变量为涂层制备条件、解吸时间、搅拌速度、解吸温度、离子强度、萃取时间和温度。进行 Plackett-Burman 设计以筛选确定影响萃取效率的显著变量。然后，通过 Box-Behnken 设计（BBD）对显著因素进行优化，并得出响应面方程。DMSe 的检测限和相对标准偏差（RSD）（n=5，c=50μgL-1）分别为 16ngL-1 和 4.3%。DMDSe 的检测限和相对标准偏差（RSD）（n=5，c=50μgL-1）分别为 11ngL-1 和 4.6%。该方法适用于加标环境和生物样品。
