采用气相色谱法并结合质量选择检测、电子捕获检测和氮磷检测对牛肝中的硒进行分析。

Analysis of selenium in bovine liver by gas chromatography with mass-selective, electron-capture and nitrogen-phosphorus detection.

作者信息

Singh A K, White T, Arendt T, Jiang Y

机构信息

Minnesota Veterinary Diagnostic Laboratory, Department of Veterinary Diagnostic Medicine, College of Veterinary Medicine, University of Minnesota, St Paul 55108, USA.

出版信息

J Chromatogr B Biomed Sci Appl. 1997 Mar 7;690(1-2):327-31. doi: 10.1016/s0378-4347(96)00394-5.

DOI:10.1016/s0378-4347(96)00394-5

PMID:9106060

Abstract

The concentration of selenium (Se) in liver was determined by gas chromatography (GC) with mass-selective (GC-MS), electron capture (GC-ECD) and nitrogen-phosphorus (GC-NPD) detection. Liver samples were digested in a mixture containing HNO3 and Mg(NO3). SeVI was converted to SeIV. SeIV was derivatized with 4-nitrophenylenediamine and then extracted in toluene. A 1-microliter volume of the toluene extract was analyzed by the GC-MS, GC-ECD or GC-NPD methods. The detection limits of the GC-ECD, the GC-NPD and the GC-MS methods were 25, 50 and 800 pg, respectively. The GC-NPD method was more selective for the derivatized Se than the GC-ECD method. The GC-MS method had the advantage of using the 76Se isotope as the internal standard. Se concentrations in liver samples determined by the three methods were comparable.

摘要

采用气相色谱（GC）结合质量选择检测（GC-MS）、电子捕获检测（GC-ECD）和氮磷检测（GC-NPD）测定肝脏中硒（Se）的浓度。肝脏样品在含有硝酸（HNO₃）和硝酸镁（Mg(NO₃)）的混合液中进行消化。将硒（VI）转化为硒（IV）。硒（IV）用4-硝基苯二胺进行衍生化，然后萃取到甲苯中。取1微升甲苯萃取液，通过GC-MS、GC-ECD或GC-NPD方法进行分析。GC-ECD、GC-NPD和GC-MS方法的检测限分别为25、50和800皮克。与GC-ECD方法相比，GC-NPD方法对衍生化硒的选择性更高。GC-MS方法的优点是使用⁷⁶Se同位素作为内标。用这三种方法测定的肝脏样品中的硒浓度具有可比性。