Fuh Ming-Ren, Huang Shu-Yen, Lin Tzeun-Yean
Department of Chemistry, Soochow University, P.O. Box 86-72, Taipei, Taiwan.
Talanta. 2004 Oct 8;64(2):408-14. doi: 10.1016/j.talanta.2004.03.002.
The use of natural and synthetic anabolic steroids in animal fattening has been prohibited in Taiwan and many countries because of their potential toxic effect on public health. This paper describes a newly developed gas chromatography-ion trap-mass spectrometry (GC-IT-MS) method for the quantitative determination of various residual anabolic steroids in meat. Anabolic steroid was derivatized with N-methyl-N-trimethylsilytrifluoroacetamide prior to GC-IT-MS analysis. MS(2) was employed for quantitative measurement. In addition, 2d-estradiol was used as an internal standard. Quantitative determination was based on the ratio of peak area of steroid derivative to peak area of internal standard derivative. Good linearity of each compound, 0.03-1.0mug/ml, was determined. Solvent extraction was used to extract residual anabolic compounds in meat samples and a solid phase extraction (SPE) procedure was utilized for sample cleanup and pre-concentration. The limits of detection of anabolic compounds approximately ranged from 0.1 to 0.4mug/kg. The detection limit was comparable with or better than reported methods and was below the minimum required performance limits (MRPLs) established by the European Community (EC). The application of this newly developed method was demonstrated by analyzing various beef, pork, chicken and several animal internal organ samples from local markets.
由于天然和合成同化类固醇对公众健康具有潜在毒性作用，台湾及许多国家已禁止在动物育肥中使用此类物质。本文描述了一种新开发的气相色谱 - 离子阱 - 质谱联用（GC - IT - MS）方法，用于定量测定肉类中各种残留的同化类固醇。在进行GC - IT - MS分析之前，同化类固醇用N - 甲基 - N - 三甲基硅基三氟乙酰胺进行衍生化处理。采用MS(2)进行定量测定。此外，使用2d - 雌二醇作为内标。定量测定基于类固醇衍生物的峰面积与内标衍生物的峰面积之比。测定了各化合物在0.03 - 1.0μg/ml范围内具有良好的线性关系。采用溶剂萃取法提取肉类样品中的残留同化化合物，并利用固相萃取（SPE）程序对样品进行净化和预浓缩。同化化合物的检测限约为0.1至0.4μg/kg。该检测限与已报道的方法相当或更好，且低于欧盟（EC）制定的最低要求性能限（MRPLs）。通过分析当地市场上的各种牛肉、猪肉、鸡肉及几种动物内脏样品，证明了这种新开发方法的应用。
