动物组织中己烯雌酚残留的基体固相扩散-气相色谱-质谱分析方法研究

Matrix Solid-Phase Dispersion Coupled with Gas Chromatography-Mass Spectrometry for the Analysis of Trace Residue of Diethylstilboestrol in Animal Tissue

采用基体固相扩散和固相萃取结合的方法提取并净化动物肝脏组织中残留的己烯雌酚 ,用N 甲基 ,N 三甲基硅烷三氟乙酰胺衍生化 ,毛细管气相色谱 质谱联用 (选择离子模式 ,选择离子为 :383、397、4 12、4 13)对衍生物检测分析 ,确立了对动物肝脏组织中己烯雌酚定性、定量分析的方法。该法检出限低于 1μg/kg;不同DES加入量的回收率为 81.6 %～ 10 0 .9% ;相对标准偏差 8.7%～ 13.2 %。

The residual diethylstilboestrol (DES) in animal liver tissue was extracted and purified using matrix solid-phase dispersion combined with solid-phase extraction. DES was separated and determined. by gas chromatography mass spectrometry (selected ion mode, the selected ions are: 383, 397, 412, 413) after derivatization of the purified sample with N-methyl-N-trimethylsilyl-trifluoracetamide. A simple qualitative and quantitative analysis method has been developed for the determination of the residue of DES in animal liver sample. Its limit of detection is below 1 mug/kg for liver sample, the recoveries of different quantities of DES are between 81.6% and 100.9%, the relative standard deviations are 8.7%similar to13.2%. Dichlorophenol was selected as internal standard, and there is a good linear correlation (the calibration coefficient is above 0.9999) between the ratio of peak areas and the concentration of DES in the range of 2-1000 mug/L.